publication information and contributorspolycrystalline, x-ray topographic analysis 365 x-ray powder...

$: Publication Information and Contributorspolycrystalline, x-ray topographic analysis 365 x-ray powder diffraction analysis of ..333-343 Aging effects in iron-chromium-cobaltalloy, autocorrelograms$
29 geometry, variable, RDF analysis 3964-(2-pyridylazo)-resorcino(PAR) reagent, use

in ion chromatography 661S-hydroxyquinoline

as precipitant 170as solvent extractant. 170

S-quinolinol, as precipitant. 16914-MeV fast neutron activation analysis,

elemental concentrations in NBS fly ashdetermined using. " 239

32 point groups. See Crystal classes.

A

a-j3 alloy, SCC environment, AESanalysis 563-564

a- and j3-fibers, in rolled copper 363a-brass alloy, Auger analysis 563a-phase alloy, SCC environment, AES

analysis 563-564a. See Crystal lattice length along the a axis.A. See Absorbance.AAS. See Atomic absorption spectrometry.Abbreviations, and symbols 689-692Aberration

chromatic, defined 670defined 668spherical 682

Ablation, laser, for solid sample analysis 36Abraded ribbons, FMR study of 274Abrasion, in XPS samples 575Abrasive cutoff machine, for optical

metallography specimen preparation 300Absolute depth scale, by FIMIAP 593Absolute methanol, and bromine, to isolate

inclusions in steel. 176Absorbance

abbreviation for 689defined 668as function of wavelength 63in IR quantitative analysis 117in IR spectra 110optimum, UVNIS 68vs radiation energy 85-86UVNIS, as function of sample

concentration 62-64Absorbance-subtraction techniques

as IR qualitative analysis 116for polymer curing reactions 120

Absorbed dose, SI derived unit and symbolfor 685

Absorption. See also K-edge; X-ray absorption.characteristics, compared with neutron and

x-ray scattering .421contrast, AEM " .444-445correction, EPMA 524cross section, M6ssbauer effect. 288cross section, M6ssbauer spectroscopy 288curve, for uranium, as function of

wavelength 85

Index

defined 84, 668edges 85-86effect in AAS .43effect of low neutron .423-emission, model approximations of 97enhancement effects, interelement 97in ferromagnetic resonance 267and fluorescence spectra, N-phenyl

carbazole 75jump 85-86of light, effect of sample thickness 61lineshapes, NMR 280and Lorentz polarization, in surface stress

measurement 385-386matrix, as XRPD source of error 341measured as function of applied magnetic

field, FMR 267micro-, as XRPD source of error 341molecular, and de-excitation processes, MFS

Jablonsky diagram for 73molecular, of UVNIS radiation, as

requirement for fluorescence 73negative 98particle, as XRPD source of error. 341and photoelectric effect 97photoelectric, in EXAFS .409of a photon 61probability, fluorescence intensity as measure

of. .411spectra, ESR 260spectra, M6ssbauer spectroscopy 294spectrum, K-edge, of krypton gas .410total, above absorption edge .409x-ray, as cause of interelement effects 97x-ray, effect in AEM-EDS microanalysis . .448x-ray, in XRS 84

Absorption contrastAEM .444-445defined 668

Absorption correction (A), in EPMAanalysis 524

Absorption diffraction method, XRPDanalysis 339-340

Absorption edge, defined 668Absorption spectroscopy, defined 668Absorptivity

defined . . . . . . . . . . . . . . . . . . . . . . . . . . . . .668molar 62-63in UVNIS 62

Abundance, natural, and atomic mass, fornaturally occurring isotopes 643

ac, See Alternating current.Accelerating voltage, defined 668Acceleration

angular, SI derived unit and symbol for ...685potential, electron, effect in x-ray

emission 84SI derived unit and symbol for 685

Accelerators, combustion, use inhigh-temperature combustion 221-222

Accuracydefined 668of microanalysis, standards for 530

and precision, compared 525of radioanalysis 246-247of single-crystal analysis 352in UVNIS 70

Acetylacetone, as solvent extractant 161Achromatic, defined 668Achromatic lens, defined 668Acid attack, in qualitative classical wet

methods 168Acid-base indicators, common 172Acid-base titrations

equilibrium in 163of industrial materials 172-173

Acid digestionbomb 165oxidizing or nonoxidizing 165-166for residue isolation 176

Acid gases, as samples in gas analysis by massspectroscopy 152

Acid pickling bathsacidity-basicity measured 172wet chemical analysis of 165

Acidsanalytic methods for. 7-base indicators 172-base solutions, conductometric titration used

in 203-base titrations 172-173concentrated, analysis of solutions in 35determined 215-216equivalent weight of an unknown 216functional group analysis of. 215-216isolation, as second-phase test method .... 177mixtures, for sample dissolutions 165, 166purity of 216

ac noncapacitive are, defined 668ACO, as synchrotron radiation

source .413Acoustic electron spin resonance, as ESR

supplemental technique 258Acronyms, for analytical techniques 689Actinides

ICP-MS analysis of .40laser-induced resonance ionization mass

spectrometry for 142in periodic table 688

Activated carbonAmoco PX-21, diffraction data 399RDF analysis of 399-400

Activated charcoal, Raman analysis 132Activation analysis. See also Prompt gamma

activation analysis (PGAA).chemical elements measured by 243defined 668

Activation energyESR analysis 266RBS analysis 628

Activity (of radionuclides), SI derived unit andsymbol for 685

ADC. See Analog-to-digital converter.Addition techniques, potentiometric membrane

electrodes 183Additives, GCIMS analysis of 639

ASM Handbook, Volume 10: Materials Characterizations (#06358G)

Copyright © 1986 ASM International ® All rights reserved. www.asminternational.org

694/lndex

Add-on SIMS instrument, for qualitativeanalysis 613

Adhesion theory of friction, AESanalyses 565

Adiabatic fast passage, defined as ESRsupplemental technique 258

Admiralty alloy, SCC environment, AESanalysis of 563-564

ADONE, as synchrotron radiationsource .413

Adsorbed surfactants, IR analysis of 109Adsorption

as contamination of gravimetric samples .. 163isotherms, for surface species, Raman

analysis as probe for 134LEED analysis of 536of molecular species, IR identification of. .109pyridine, Raman studies 134surface, FIMIAP study of 583

Adsorption chromatography. See alsoLiquid-solid chromatography.

defined 668Advantage, Fellgett's or multiplex 129AEM. See Analytical electron microscopy.Aerosol samples

atmospheric, PIXE particle size analysisof. 102

collection 94AES. See Auger electron spectroscopy;

Atomic emission spectrometry.AFC. See Automatic frequency control.AFS. See Atomic fluorescence spectrometry.Aggregates

molecular, in complexometric titrations ... 164polycrystalline, x-ray topographic

analysis 365x-ray powder diffraction analysis of ..333-343

Agingeffects in iron-chromium-cobalt alloy,

autocorrelograms for 599, 600materials, FIMIAP study of nucleation,

growth, and coarsening of precipitatesin 583

over-, kinetics of 317polymer, liquid chromatography monitoring

of stability during 649precipitates, in gravimetric sample

preparation 163Agricultural materials. See also Food

products.use of ICP-AES for 31

Air. See also Oxygen.analytic methods for. 8assay, for toxic elements, NAA for 233direct sampling by AAS .43pollutants, GFAAS analysis 58UVIVIS trace analysis of 60

Air-acetylene flame atomizer .48Air filters

GFAAS atomizers as 58PIXE analysis of " 102

Air-fired fracture surface, XPS survey 577Alcohols, determined by EFG 216-217Aldehydes

functional group analysis of 217and ketones, determined 217

Alignment of silicon boule, for cutting alongcrystallographic planes 342

Aliquot, defined 668Alkali halides

ESR studied 263as sample in Raman analysis of metal

oxides 131Alkali metals

eluent suppression technique for 660flame source emissions for trace

analyses 29-30optical emission spectroscopy 21, 29-30solvent extractants for 170

Alkaline earth metalscomplexometric titrations for 164eluent suppression technique for 660extractants for. 170optical emission spectroscopy for 21

Alkaline environmentscorrosion of nickel and cobalt in

aqueous 135oxidation of silver electrodes in 135

Alkenes, determined 219Alkyl amines, as solvent extractants 170Allowed (diagram) lines, x-radiation 86Alloying elements

flame AAS analysis in steels 56partitioning of, FIMIAP analysis 583sampling trainload of metal pipe for

percentage of 15Alloys. See also Metals and alloys,

characterization of.analytic methods for .4characterized 1chemical analysis by controlled-potential

coulometry 207commercial, hydrochloric acid for sample

dissolution of 165effects of composition on mass

absorption 97FIMIAP study of point defects in 583FIM images of 589-590formation, RBS analysis 628high-purity, voltammetric analysis of 188high-temperature, dissolution mediums 166ion-implanted, AEM microstructural

analysis .484-487liquid, NMR analysis of electronic structure

of. 284metals in, quantitative determination by

electrogravimetry 197multicomponent, phase separation analysis

by SAXS/SANS/SAS .402ordered, effect of antiphase boundaries on

FIM images 589ordered, ladder diagrams of. . . . . . . .. . ..594perchloric acid as dissolution medium .... 166prompt gamma activation analysis (PGAA)

of 240spark source excitation for elemental

analysis of 29spot test kits for 168surfaces, FIM imaged 590trace impurities detected 31, 43two-phase, SEM atomic number contrast

analysis of 508verification of inorganic solids, applicable

methods .4-6Alloys and metals characterization. See Metals

and alloys. characterization of.Alphabenzoinoxime, as narrow-range

precipitant. 169Alphabet, Greek, symbols for 692Alpha-particle emission, as radioactive decay

mode 244-245Alternating current, abbreviation for 689Alumina

AES spectra with peakshifts and plasmonloss peak structures 552

background fluorescence of 205chromia catalysts, ESR analysis of 265fusion fluxes for 167sulfuric acid as dissolution medium 165transition metals as source of fluorescence

on " 130Aluminon method

analysis for aluminum inferrosiliconlferroboron by 68

analysis for beryllium in copper-berylliumalloys by 65

Aluminum. See also Aluminum alloys;Aluminum alloys. specific types.

AES spectra with peakshifts and plasmon losspeak structures 552

age-hardened, FIMIAP study of precipitatesin 583

analysis in ferrosiliconlferroboron, byaluminon method 68

crystallization and coarsening stages, x-raytopography 376

determined in plant tissues .41dominant texture orientations 359EDTA titration 173in electronic nickel, photometric method

for 65extended solubility of iron in 294-295field evaporation of 586, 587in flame atomizers .48ingot, macrograph of 302ion-induced Auger yields 550ion removal from 200in iron-base alloys, flame AAS analysis

for 56iron in, extended solubility of 294-295LEISS spectra 604molybdenum-implanted .484, 486neutron and x-ray scattering, and absorption,

compared .421nickel-implanted .485photometric analysis methods 64polycrystalline, bright-field image of

dislocations in .444polycrystalline, ring pattern from .437pure, K-M CBEDP from .441single-crystal, spot diffraction pattern

from " .437species weighed in gravimetry 172in thermite, AAS analysis for 56TNAA detection limits 237as unknown particle .457volumetric procedures for 175weighed as the phosphate 171wire connections, EPMA failure

analysis 531-532Aluminum alloys. See also Aluminum;

Aluminum alloys, specific types.analysis for boron, by Carmine method ....68diffraction techniques, elastic constants, and

bulk values for 382FIM sample preparation of 586

Aluminum alloys, specific types. See alsoAluminum; Aluminum alloys.

1100, dynamically recovered .4702014-T6, diffraction techniques, elastic

constants, and bulk values for. 3822024-T351, diffraction techniques, elastic

constants, and bulk values for 3825056-0, surface stress measurement. 3837050-T6, diffraction techniques, elastic

constants, and bulk values for 3827075-T6, diffraction techniques, elastic

constants, and bulk values for 382AI-4.7Cu, diffusion-induced grain-boundary

migration .461-464AI-4.7Cu, typical CBEDP for .464AI-I.7Cu, information from FIM image

of 589-590Aluminum/brass interface, aluminum wire

connections, EPMA and SEM imagesof 531-532

Aluminum-copper alloysCBEDP for .462Guinier-Preston zone, FIM images

of 589-590Aluminum/iron interface, aluminum wire

connections, EPMA and SEM imagesof 531-532

Aluminum-lithium alloysdouble arc contrast. .467warm-worked and annealed, recovered

subgrain structure .470



Aluminum nitrides, as particles in stainlesssteel tubing, EDSIEELS spectra .461

Aluminum oxide, in binary phosphateglasses 131

Amalgam formation, in controlled-potentialelectrolysis 208

American Society for Testing andMaterials (ASTM), photometric testsapproved" 64

Aminesdetermined 217-218as samples in gas analysis by mass

spectrometry 52simple, eluent suppression technique for ..660

Amino acids, irradiated, ESR analysis of 266Ammeter, for electrogravimetry 200Ammonia

conductometric titration of. 203eluent suppression technique for 660as sample in gas analysis by mass

spectrometry 152Ammonium dihydrogen phosphate, as

common analyzing crystal, x-rayspectroscopy 88

Ammonium hydroxide, as precipitant. 168Ammonium ion, organic precipitant for 169Ammonium nitrate, as sample modifier,

GFAAS analysis 55Ammonium phosphate, and magnesium

nitrate, as sample modifiers, GFAASanalysis 55

Ammonium phosphomolybdate, asprecipitate 173

Ammonium purpureate, as metallochromicindicator 174

Ammonium pyrrolidinedithio-carbamate, assolvent extractant 170

Amorphous carbonoxidized in high-temperature combustion

resistance furnaces 224RDF structural ordering in 393

Amorphous materialsEXAFS analysis .407, 410RDF determined interatomic distance

distributions and coordinationnumbers 393

Amorphous solid, defined 668Amount of phase, as x-ray diffraction

analysis 325Amount of substance, SI base unit and SI

symbol for 685Amperometric gas sensors, capabilities 181Amperometric titration, as electrometric 204Amperometry

capabilities, compared with voltammetry .. 188and conductometry, compared 204defined . . . . . . . . . . . . . . . . . . . . . . . . . . . . .668

Amplifiersand preamplifiers, in x-ray spectrometer

detectors 91stabilized operational, in

electrogravimetry 199amu, See Atomic mass unit.Analog dot mapping. See also Dot mapping;

Mapping; X-ray maps.and digital compositional mapping 528as elemental-distribution mapping 525-528

Analog imaging, and digital imaging, of iron inaluminum matrix 448

Analog-to-digital converterdefined 668in ICP systems 39

Analysischemical, and sampling 15defined 668general, of organic gases 11nondestructive, MOLE as 130on-line, PGAA as 239-240remote, electrometric titration as 202

Analysis of surfaces. See Surface analysis;Surface analysis and characterization;Surface.

Analytesin complexometric titrations 164concentration in sample for ICP-AES 33concentration yielded by back-titration 173defined 668in gravimetric analysis 170ion association in solvent extraction 170moieties, weighing as the, gravimetric

analysis 171separation 164submicrogram amounts determined by

electro metric titration 202titer technique for 172

Analytical chemistrycomplexometric titrations 164defined . . . . . . . . . . . . . . . . . . . . . . . . . . 668gravimetric 163ion exchange separation 164-165oxidation-reduction reactions 163-164solvent extraction 164

Analytical curve, defined 668Analytical electron microscopes

conventional transmission electron .. .430-431convergent-beam electron-diffraction

pattern .431electron microdiffraction .431electron optical column .431imaging in the .440-446modern .431-432scanning electron .430-431signal detector positioning .434x-ray microanalysis in the 446-449

Analytical electron microscopy. See alsoAnalytical transmission electronmicroscopy.

absorption contrast 444-445capabilities 516contrast mechanisms 444-445defined 668dislocation cell structure analysis by . .470-473effect of lenses in .432and energy-dispersive x-ray spectroscopy, as

electron-beam microanalyticaltechnique 446

imaging in TEM mode .440-442phase contrast. .445special techniques .445-446in the STEM mode .442TEM and STEM images, relationship

between 442-444Analytical gap, defined 668Analytical line, defined 668Analytical transmission electron

microscopy .429-489analytical electron microscope .430-432applications .429, 453, 473-487applications, techniques and procedures

for .429, 453-473Bragg's law .436bright-field imaging 441-446capabilities 365, 402, 490, 516, 536capabilities, compared with optical

metallography 299capabilities, compared with Rutherford

backscattering spectrometry 628dark-field imaging .441-446defect analysis by TEMISTEM .464-468deformation, recovery, and recrystallization

structures by TEM .468-470diffusion-induced grain-boundary migration

analysis by EDS/CBED .461-464diffusion measurements by AEM .476-478dislocation cell analysis by AEM .470-473electrochemical thinning vs electrojet

thinning .451electron beam/specimen interactions . .432-434

Index / 695

electron diffraction .436-440electron energy loss .432, 435electron energy loss spectroscopy

and .449-450electron optics .432estimated analysis time .429general uses .429grain-boundary segregation analysis by

AEM .481-484image morphology 309imaging, analytic electron

microscope .440-446introduction .430ion beam milling .451-452Kikuchi line patterns .437-438lattice imaging .445-446light-element analysis by EDSIUTW-EDS/

EELS .459-461limitations .429microtomes, for sample sectioning .452orientation relationships and habit plane

determination by .453-455phase diagrams determined by AEM . .473-476related techniques .429replicas, extraction .452sample preparation .450-453samples .429, 432-434, 450-453selected-area diffraction .436signal detectors .434-436unknown phase identification by electron

diffractionlEDS .455-459weld metal microstructure, by AEM . .478-481x-ray microanalysis in .446-449

Analytical wavelength, defined 668Analyzers

cylindrical mirror. 554, 571defined 668double-pass cylindrical mirror 571electron energy, or velocity 570-571electrostatic LEISS 607hemispherical, for AES analysis 554for image analysis , 310-313retarding field, for AES analysis 554sector, for AES analysis 554semiautomatic digital image 310systems, x-ray spectrometers 91velocity 570-571

Analyzing crystalscommon 88in wavelength-dispersive x-ray

spectrometers 88Angle

between normal to the diffracting latticeplanes and the sample surface, symbolfor 692

conversion factors 686of incidence 114, 668symbol for 692

Angstrom 669, 691Angular acceleration, SI derived unit and

symbol for 685Angular distribution functions, nuclear

transitions of rnultipolarity 290Angular measure, symbol for 691Angular scan, channeling, lattice strain

measurement by 635Angular velocity, SI derived unit and symbol

for 685Anhydrides, boric acid, as flux 167Animal tissue

AAS analysis of trace metals 55NAA analysis of retention of toxic elements

in 233voltammetric detection of herbicide/pesticide

residues in 188Anions

defined 669determined on contaminated surfaces, by ion

chromatography 658



696/ Index

Anions (continued)exchange resins, use in anion

chromatography 659green and yellow, as determined by single-

crystal analysis 354inorganic, determined by ion

chromatography 663as negatively charged ions 659potentiometric membrane electrodes

quantification 181qualitative and quantitative analysis by ion

chromatography 658-667Anisotropic effects, ESR studied 256Anisotropic hyperfine coupling constants,

electron spin resonance 261Anisotropic thermal expansion coefficients,

XRPD analysis 333Anisotropic thermal motions, and crystal

structure determination 352, 353Anisotropy

constants, FMR for obtaining 272, 273magnetic, determined 272-273

Annealing(growth) twin, rutile images of 443improper, defect depth distribution from ..628molybdenum-implanted aluminum .486Raman analysis of 133SAS techniques for .405studies, by NMR 277

Anode materials, x-ray tubes 89Anodes, dual, in electrogravimetry 199Anodic overvoltage, in electrogravimetry 198Anomalous transmission

divergent beam topography 370in x-ray topography 367

Anthracene, and naphthalene, totalluminescence spectrum (EEM) ofmixture 78

Antiferromagnetic materialsESR identification of magnetic states in 253variable temperature studies of 257

Antihistamines, coulometric titration of 205Antimony

in copper alloys, determined byiodoantimonite method 68

determined by controlled-potentialcoulometry 209

epithermal neutron activation analysis(ENAA) 239

gaseous hydride, for ICP sampleintroduction 36

as halogen trap material. 224photometric analysis methods 64quartz tube atomizers for .49species weighed in gravimetry 172TNAA detection limits 237, 238volatilizing 166volumetric procedures for 175weighed as the sulfide 171

Antioxidants, GCIMS analysis of 639Antiphase boundaries, in ordered alloys,

effect in FIM images 589Anti-Stokes Raman line, defined '" 669Anti-Stokes scattering

energy-level diagram 127in Raman spectroscopy 126-128

Antiwear films, AES characterized 566AP. See Atom probe; Atom probe

microanalysis.Aplanatic, defined 669Apochromatic lens, defined 669Apparent density, defined 669Applications and examples

(Ill) pole figures from Cu tubing 363300/400 series stainless steels, analysis

of. 100AAS instruments as detectors for other

analytical equipment 55acids, determined 215-216

activated carbon, analysis of 399-400AES application to tribology 566alcohols, determined 216-217aldehydes and ketones determined 217alignment of silicon boule for cutting along

crystallographic planes 342alkenes, determined 219AI-killed steel, analysis of. 231amines, determined 217-218anisotropy, magnetic, determined 272-273archaeological samples, copper determined

in 186aromatic hydrocarbons, determined 218atmospheric particles, analysis of 106atomic number contrast, in analysis of

two-phase alloys 508baby lotion, analysis of parabens in ..655-656biological materials, powdered, analysis

of 106-107blocking and channeling surface structure

study by 633borosilicate glass, determination of Band F

in 179brine analysis, geological 665bromine, indirect determination of 70bulk samples, composition of 631calcite, quantitative analysis of ZnO in 342carbon, surface, determination of 224carbon, activated, analysis of. 399-400carbon determined by combustion 214catalysts, chromia alumina 265cellular decomposition of martensite in

uranium alloy, kinetics of 316-318cement, analysis of. 99-100ceramic nuclear waste form simulant study

of 532-535ceramics, SAXS/SANS analysis of. .405channeling and blocking, surface structure

study by 633chemical reaction products, analysis

of 656-657chloride ions, nickel determined in samples

containing 201chromia alumina catalysts 265chromium depletion in weld zone 179coal fly ash, determination of Cu and Pb

in 147-148cobalt compounds, trace nickel determined

in 194-195cold-rolled steel, corrosion

resistance 556-557combustion, determination of carbon,

hydrogen, and nitrogen by 214complex, number of ligands determined in 70composition fluctuations, local, in ternary

3:5 semiconductor 601composition of bulk samples 631composition, of mixtures, determined 213composition vs depth, passive film on Sn-Ni

substrate 608-609compounds, organic, identification of ....213concentrations, high, and well-resolved peaks,

gold-copper alloy analysis with 530coordination geometry, determination of ..354copper determined in archaeological

samples 186copper, hydrogen determined in 231-232copper-manganese alloy, copper content

estimated 201copper oxidation using 18 0 609copper tubing, (Ill) pole figures from 363corrosion and surface strains, connector 607corrosion in pyrotechnic actuators ....510-511corrosion of Ni and Co in aqueous alkaline

media 135corrosion on lead surfaces 135corrosion on metals, analysis of 134-135corrosion resistance of cold-rolled

steel 556-557

crystal growth and electronic device materialstudies 375-376

crystal kinetics and materialtransformation 376

crystalline phase, unknown, use of unit cellsto identify 353

crystallographic planes, alignment of siliconboule for cutting along 342

curing mechanism of a polyimide resin 285de arc excitation to determine trace metal

impurities in CaW04 •••••••••••••••••29deer hair, analysis of sulfur in 224defects, analysis of .464-468deformation analysis 376-378, 468-470depth profiles, heavy element

impurities 632-633depth profiling, granular sample using ATR,

DRS, and PAS 120detection of phase changes 282-283detection of surface phase 293determination of BTU and ash content in

coal 100determination of Cr, Ni, and Mn in stainless

steel 146-147determination of trace Sn and Cr in HOz, by

GFAAS 57-58determination of ultra trace uranium by

laser-induced fluorescence spectroscopy ..80diamond, synthetic, characterization of metal

impurities in .417diffusion-induced grain-boundary migration,

analysis of. .461-464diffusion measurements 476-478diffusion of plutonium into thorium 249diffusion phenomena, investigation

of 576-577direct determination of benzo(a)pyrene 79direct solid-sample AAS analysis 58dislocation cell structure analysis .470-473dopant atoms, lattice location of 633-634electrical contacts, surface films on 578-579electrochemically based corrosion systems in

aqueous environments 134-135electrolytically generated radical ions 265electronic device material studies, and crystal

growth 375-376electronic structure, liquid metals and

alloys 284elemental analysis, Schoniger flask method

for 215elemental mapping of high-temperature

solder 532elements, light, analyses

of .459-461, 558-559empirical formulas, determination of .....213enzymatic determination of glucose using

oxygen quenching of fluorescence 79-80enzyme activity, assay of '" ..70esters, determined 218estimation of Cu in a Cu-Mn alloy 201exchange stiffness 275exotic effects, studied in disordered magnetic

material 276explosive actuator, determination of oxygen

isotopes in 625-626extended solubility of iron in

aluminum 294-295factor analysis and curve fitting applied to

polymer blend system " .118failure of Al wire connections 531-532failure, overload, of steel threaded

rod 511-513fcc materials, features of rolling textures

in '" 363-364ferromagnetic alloys, order-disorder

in 284-285films, grain size of silver 543films, thick, analysis of 561fingerprinting, multielement 195



flame AAS for elemental analysis 55-56flame analysis determination of alloying

elements in steels 56formulas, empirical, determination of 213fracture behavior and deformation 376-378fracture surfaces, SCC 562-564free lime in portland cement, determination

of. 179geological brine, analysis of 665geometric and elemental analysis, particles

produced by explosive detonation ..318-320GFAAS determination of Bi in Ni 57glasses, SAXSISANS analysis of .405glass microballoons, analysis of 665-667glass surface layers, analysis of. 624-625glow charge to determine C, P, and S in

low-alloy steels and cast iron 29gold-copper alloys, analysis with well

resolved peaks and high concentrationsfor 530

gold determined 210-211grain-boundary chemistry, study of. ..561-562grain-boundary migration, diffusion-induced,

analysis of .461-464grain-boundary segregation, analysis

of .481-484grain size, Ag film grown on mica 543-544graphites, analysis of 132-133graphites, wettability of 543grinding, local variations in residual stress

produced by 390habit plane and orientation

relationships .453-455heavy element impurities, depth profiles

of 632-633hexamethyldisiloxane, structure and

degradation of plasma-polymerized 285-286

high resolution, analysis of Jominy jarusing " ..508

high-temperature solder, elemental mappingof. 532

historical objects, analysis of 107hydrided TiFe, phase analysis of 293-294hydrocarbons, aromatic, determined 218hydrogen determined by combustion 214hydrogen determined in copper 231hydroxyl and boron content in glass,

quantitative analysis 121-122impurities, heavy element, depth profiles

of 632-633impurities in nickel, determined 240impurities in U02, determination of .. 149-150impurity analysis inLPCVD thin films,

quantitative 624Inconel 600 tubing, residual stress and percent

cold work distribution 390indirect determination of bromine 70inhomogeneities, magnetic,

determined 274-275integrated circuit problems, SEM analysis

for 513-514interatomic bond lengths and physical

properties 355interfacetsuperlattice studies 634-635interfacial segregation studies in Mo ..599-601intermetallic compounds, sublattice ordering

in 283-284internal electrolysis, separation of Cd and Pb

by 201ion-implantation profile in silicon,

phosphorus, quantitative analysisof 623-624

ion-implanted ions, microstructural analysisof .484-487

iridium anomaly at Cretaceous-Tertiaryboundary 240-241

iron-base magnet alloy, spinodaldecomposition of 598-599

iron in copper, analysis of phases of .....294iron oxide films, composition

determined 135isotopes, oxygen, determined in explosive

actuator 625-626Jominy bar, use of high resolution in analysis

of. 508Karl Fischer method, water

determination 219ketones and aldehydes determined 217kinetics, crystal, and material

transformations 376kinetics of cellular decomposition of

martensite in uranium alloy 316-318kinetics of radical production and subsequent

decay 265-266Kjeldahl method, to determine

nitrogen 214-215Knight shift measurements on metallic

glass 284Kovar-glass seals, shear fracture studies

of 577-578laser treatment, of stainless steel, surface

composition effects during 622-623lattice location of dopant atoms 633-634lead surfaces, corrosion on 135ligands in complex, numbers determined 70light element analysis ..... .459-461, 558-559liquid metals and alloys, electronic structure

of 284local composition fluctuations in ternary 3:5

semiconductor 601-602local variations in residual stress produced by

surface grinding 390-391longitudinal residual stress distribution in

welded railroad rail. 391-392LPCVD thin films, quantitative impurity

analysis of. 624machining, magnitude and direction of

maximum residual stress producedby 392

magnetic anisotropy, determined 272-273magnetic disordered materials, exotic effects

in 276magnetic inhomogeneities,

determined 274-275magnetization, determined 271major constituent analysis with peak

overlap 530material transformations and crystal

kinetics 376maximum residual stress, magnitude and

direction produced by machining 392mercury switch, analysis of surface films on

electrical contacts in 578-579metallic glass, Knight shift measurements

on 284metal oxide systems, analysis of 130-131metals, analysis by SAXS and SANS .405metatorbernite, analysis of 265microballoons, glass, analysis of 665-666microcircuit process gas analysis 156-157microstructure, ion-implanted alloys,

determined .484-487microstructure, weld metal. .478-481mixtures, composition determined 213molecular orientation in drawn polymer films,

determined 120molybdenum, interfacial segregation studies

in 599-601monitoring polymer-curing reactions using

ATR 120-121monolayers adsorbed on metal surfaces,

examined 118-120multielement fingerprinting and approximate

quantification in effluent samples 195natural waters, analysis of .41Nd2(CoFeo.9h4B, Rietveld analysis

of. .425

Index / 697

near-surface defects in single-crystals, studyof 633

nickel-base superalloy, phase chemistry andphase stability of 598

nickel determined in samples containingchloride ions 201

nickel, impurities determined in 240nickel-phosphorus film, coverage determined

on platinum substrate 608nitrogen determined by combustion 214nitrogen determined by Kjeldahl

method 214-215nontransparent samples, surfaces

characterized 70-71nuclear waste form simulant, ceramic, study

of 532-535optical microscopy, complementarity of SEM

and SAM in 509-510order-disorder in ferromagnetic

alloys 284-285organic compounds identified 213orientation relationships and habit

plane .453-455overload failure, quench-cracked steel

threaded rod 511-513oxidation of Ag electrodes in alkaline

environments 135oxidation of copper using 180, study of. ..609oxygen in silicon wafers, quantitative analysis

of 122-123oxygen in Ti, determined 231oxygen isotopes determined in explosive

actuator 625-626parabens, analysis in baby lotion 655-656particles produced by explosive detonation,

geometric and elemental analysis ...318-320passive film on Sn-Ni substrate, composition

vs depth of 608passive films, study of thin 557-558peak overlap, analysis of major constituents

with 530peaks, well resolved, and high concentrations,

gold-copper alloy analysis with 530pearlite growth, use of SACP to

understand r ..•.••••...•508-509peroxides, determined 218petroleum products, analysis of 100-101phase analysis of hydrided TiFe 293-294phase analysis of iron in copper 294phase changes, detection of 282-283phase chemistry and phase stability of Ni-base

superalloy 598phase diagrams, determination of .473-476phases, surface, on silicon, qualitative

analysis of. 341-342phases, unknown crystalline, unit cell

information to identify 353phases, unknown, identification of .. .455-459phenols, determined 218phosphorus ion-implantation profile in silicon,

quantitative analysis of. 623-624PIXE and proton microprobe 107plant tissues, analysis of .41plasma-polymerized hexamethyldisiloxane,

structure and degradation of. 285-286platinum substrate, determined coverage of

Ni-P film on 608plutonium diffusion into thorium 249pole figures (111), from copper tubing 363polyimide resin, curing mechanism of 285polymer and plasticizer materials in vinyl

film, identification of 123-124polymers, analyses of 131-132, 405, 647-648porous graphite atomizers as filters for air

particulates 58powdered biological materials, analysis

of 106-107praseodymium and neodymium, separation

of 249-250



698/ Index

Applications and examples (continued)preferred crystallographic growth, use of

SACP to establish 509pyrotechnic actuators, corrosion in 510-511radical ions, electrolytically

generated 265radical production and subsequent decay,

kinetics of ' 265recovery, analysis of .468-470recrystallization structure analysis .468-470relay weld integrity, determined 156residual stress analyses 390, 392, 425-426Rietveld analysis .425rod, overload failure of 511-513rolling textures in fcc materials, features

of 363-364SACP 508-509sampling a trainload of metal pipe for

percentage of alloying element 15SAXSISANS analyses .405Schoniger flask method for elemental

determinations 215seals, shear fracture studies of Kovar-

glass 577-578segregation, analysis of grain-

boundary .481-484segregation, interfacial, in

molybdenum 599-601segregation, of Pb to surface of Sn-Pb

solder 607-608segregation, surface 564-566SEM analysis of integrated circuit

problems 513-514SEM and SAM, complementary contributions

of optical microscopy 509-510semiconductor, local composition fluctuations

in 601-602separation of Cd and Pb by internal

electrolysis 201separation of praseodymium and

neodymium 249-250shear fracture studies of Kovar-glass

seals 577-578silica glass, x-ray diffraction pattern

of 398-399silicon, analysis of phosphorus

ion-implantation profile in 623-624silicon boule, alignment for cutting along

crystallographic planes 342silicon, qualitative analysis of surface phase

on 341-342silver film grown on mica, grain size

in " ..543-544silver scrap metal, analysis of. .41single crystals, study of near-surface defects

in 633solder, analyses of. 179, 532, 607-608solubility, extended, of iron in

aluminum 294-295spark source excitation for elemental analysis

of metal or alloy 29spectrophotometric titrations 70spinodal decomposition of Fe-base magnet

alloy 598-599spin relaxation rates, determined 275-276spin wave resonances 275stable free radical hydrazyl 265stainless steel alloy, "umpire" analysis

of 178-179stainless steels, surface composition effects

during laser treatment of 622-623strains, measurement of 275strains, surface, and corrosion products,

connector 607stress-corrosion crack fracture

surfaces 563-564structure and degradation of

plasma-polymerizedhexamethyldisiloxane 285-286

sublattice ordering in intermetalliccompounds 283-284

subsurface residual stress and hardnessdistributions in induction-hardened steelshaft. 389-390

sulfur in deer hair, analysis of 224superlattice/interface studies 634-635surface carbon, determined 224surface composition effects during laser

treatment of stainless steels 622-623surface effects, determined 273surface films on electrical contacts, mercury

switch, analysis of 578-579surface layers, glass, analysis of 624-625surface-phase detection 293surface phase on silicon, qualitative

analysis 341-342surface segregation 564-566surfaces of nontransparent samples,

characterization of. 70-71surface species on nonmetals, analysis of 134surface strains and corrosion products on

connector, identification of 607surface structure, analysis of 133-134surface structure study, by channeling and

blocking 633surfactant molecules in water, examination of

structural changes in 118synthetic diamond, metal impurities in .417synthetic substance, analysis of new ..353-354texture, measurement and analysis of .425thermite, flame AAS analysis of 56-57thick films, analysis of 561thickness, of thin films, determination

of. 100, 631-632thin film composition and layer

thickness 631-632thin films, passive 557-558thin films, quantitative impurity analysis in

LPCVD 624tin-nickel substrate, composition vs depth of

passive film on 608titrations, spectrophotometric 70toxic trace elements in ground water,

measurement of 148trace amounts of Ni in Co

compounds 194-195transformations, material, and crystal

kinetics 376transformer cores, analysis 224tribology, AES application to 566turquoise, analysis of. 265two-phase alloys, atomic number contrast in

analysis of. 508umpire analysis, stainless steel alloy .. 178-179unit cells, use to identify unknown crystalline

phase 353unknown phases, identification of .455-459unsaturation, determined 219uranium, determined 211vanadium determined in compounds 206water determination, Karl Fischer method

for 219welded railroad rail, longitudinal residual

stress distribution in 391-392weld metal microstructure, interpretation

of .478-481wettability, of graphite 543wire connections, aluminum, failure

of 531-532x-ray diffraction pattern, of silica

glass 398-399ZnO in calcite, quantitative analysis of ...342

Applied electromotive force (emf), inelectrogravimetry 197

Approximation, single-scattering, inEXAFS .409

Aqueous environments, electrochemicallybased corrosion systems determined in .. 134

Aqueous media, Raman analyses of polymersin 131

Aqueous samples, optical emissionspectroscopy 21

Aqueous solutionscontaining nickel and cobalt ions, spectra

compared 65ionic, use in ion chromatography 658-664

Are, direct-current. 25Arc butt weld, optical macrograph 303Archaeological samples

of books and artifacts, PIXE analysis for .. 102ion selective electrode to determine copper

in 186as NAA application 234

Arc sourcesapplications 29compared 27for optical emission spectroscopy 25

Areaconversion factors 686SI derived unit and symbol for 685

Area channeling analysis. See also Channeling.crystallographic texture measurement and

analysis by 357Area fraction, effects of varying in image

analysis 311-312Area scan, EMPA analog mapping as 525Argon

adsorbed, effects in FIM 588continuous-wave gas lasers 128ion etching, use in XPS 575ionization potentials and imaging fields

for 586ion-sputtering, XPS analysis 575, 576plasma, use in ICP-AES 31in weld relay, gas mass spectrometry of .. 156

Argonne National Laboratory, Intense PulsedNeutron Source .424

Aroma components, IR determination of 109Aromatic, defined 669Aromatic hydrocarbons, determined 218Aromatic silicones, Raman analysis 132Arrangement of atoms, as x-ray diffraction

analysis 325Arsenic


epithermal neutron activation analysis of ..239evaporation fields for 587gaseous hydride for ICP sample

introduction 36in glass, K-edge EXAFS spectra .411ICP-determined in natural waters .41iodimetric titrations of 174photometric analysis methods 64quartz tube atomizers for .49sample modification, for GFAAS analysis .. 55in silicon on ion-implanted silicon

samples 632species weighed in gravimetry 172TNAA detection limits 237volatilizing 166Volhard titration for. 173volumetric procedures for 175weighed as the sulfide 171

Arsenic chloride, distillation 169Artifacts

distorting SIMS depth profiles 619peaks, as AEM-EDS microanalytic

limitation .448spectral, sum and escape peaks as 520in wavelength-dispersive spectrum 520

Ash, and BTU, determined in coal. 100Ashing

of organic liquids and solutions, foranalysis 10

of organic solids, for analysis 9oxygen plasma dry .. '" 167



of samples, GFAAS analysis 55in second-phase testing 177

Assay, defined 669Astrophysical research, qualitative spectral

analysis for .43Asymmetric reflections, in double-crystal

spectrometry 371Asymmetric transmission, Guinier camera

arrangement 335ATEM. See Analytical transmission electron

microscopy.Atmospheric

aerosol sample collection 94aerosols, PIXE analysis by particle

size 102, 106physics and chemistry, PIXE studies in 106pressure, abbreviation for 691

Atomic absorption spectrometersalternative designs 53, 54double-beam 50multielement. 52

Atomic absorption spectrometry .43-59accessory equipment 55advantages .46analytical sensitivities, hydride-generation

AAS systems 50applications .43, 55-58atomizers . . . . . . . . . . . . . . . . . . . . . . . . . .46-50Boltzman equation .44capabilities 31, 102, 181, 233, 333capabilities, compared with x-ray

spectrometry 82capabilities, compared with ion

chromatography 658capabilities, compared with UVNIS

absorption spectroscopy 60capabilities, compared with molecular

fluorescence spectroscopy 72continuum-source 52-53direct solid-sample analysis 58discrete atomic line-source lamps, effects

of 52electrothermal vaporization technique for 36estimated analysis time .43flame atomizer versions .44-46hydride-generation system 50of inorganic liquids and solutions 7of inorganic solids .4-6instruments, as detectors 55introduction .43-44limitations .43neutron activation analysis and,

compared 233and optical emission spectroscopy 21of organic solids ~ 9principles and instrumentation : .44-46quantitative elemental analysis by .43related techniques .43, 44-46research and future trends 52-55sampling .43, 47, 54-58sensitivities .46signal error in .45spectrometers 50-52

Atomic absorption spectrophotometrycapabilities, compared with electrometric

titration 197capabilities, compared with classical wet

analytical chemistry 161residue analysis by 177

Atomic coordinatesfor defining crystal structure 348effect of Rietveld method on .423

Atomic emission, optical systems for 23-24Atomic emission spectrometry

atomic absorption spectrometry,compared .44-46

capabilities 102, 181,333energy-level transitions 44principles and instrumentation 44-45

Atomic fluorescence spectrometryand atomic absorption spectrometry,

compared 44-46energy-level transitions 44error sources . . . . . . . . . . . . . . . . . . . . . . . . . .46principles and instrumentation .45-46

Atomic mass unit 669, 689Atomic number

abbreviation for 691and characteristic x-ray wavelength,

relationship between .433contrast, two-phase alloys 508correction (2) 524defined 669of elements 688imaging, defined 669

Atomic number correction, in EPMAanalysis 524

Atomic number imaging, defined 669Atomic order, as fine structure effect .438Atomic percent, abbreviation for 689Atomic scattering factor, defined 329Atomic sensitivity factors, x-ray photoelectron

spectroscopy 574Atomic spectroscopy. See also Spectroscopy.

energy-level transitions .44Fourier transform spectrometers in 39

Atomic structuredefined ... . . . . . . . . . . . . . . . . . . . . . . . 669of lanthanum-nickel-platinum alloy 284neutron diffraction analysis for .420symmetry related to crystal symmetry and

crystal systems 348Atomic theory

basic 33and optical emission spectroscopy 21-23

Atomic weight, defined 669Atomization

defined . . . . . . . . . . . . . . . . . . . . . . . . . . . . .669flame, typical system .48systems, AAS sample introduction 54-vaporization interferences 33, 34and volatilization, in graphite furnace

atomizers 53Atomizers

for atomic absorption spectrometry .46-50air-acetylene flame, characteristics .48defined 669electrical plasma 53-54flame .47-49furnaces .48, 49graphite furnace .48, 49Langmuir torch 54nitrous oxide-acetylene flame .48quartz tube for .48

Atom probeabbreviation 689defined 584, 669principle of 591voltage-pulsed and laser-pulsed,

compared 597Atom probe microanalysis. See also Field ion

microscopy 583-602alternate data representation 594calibration 592complete system 591-592composition profiles 593-594field evaporation as basis of 587field ion microscopy and 583-602high-resolution energy-compensated atom

probe 592, 597imaging atom probe 596-597instrument design and operation 591mass resolution, ECAP effect 597mass spectra and interpretation 591-593mass spectra of 'V matrix, IN 939, and

primary 'V' precipitates 598, 599principles 591pulsed laser atom probe 597-598

Index / 699

quantitative analysis .594-595single-layer depth resolution of 595spatial resolution, factors limiting 595-596

Atomsabsolute configurations 344arrangement of. 287, 325black 348-349chemisorbed, EXAFS for geometry of .407coordination numbers and geometries 344defined 669dopant, lattice location of 633electronic structure by UVNIS 60energy-level diagram of 570field-evaporated, effects of 590, 602fluorescent. 72-74geometry around 345, 352hydrogen .410, 420inorganic, MFS analysis 74interstitial, AM images of. 588irradiated, decay rate equals production

rate 235layered, in AM images 590location 344, 349, 350near-neighbor environment, analysis in solids

by NMR 277phase difference in scattering from different

electrons within 328scattering factor 349shells, photoejection of electrons from 85single-layer depth analysis 595sputter removal of 554surface positions of 536wave from, mathematical form of 349white 348-349x-rays generated from disturbance of electron

orbitals of 83ATR. See Attenuated total reflectance

spectroscopy.Attenuated total reflectance

spectroscopy 113-114depth profiling granular sample by 120for monolayer adsorption on metal

surfaces 119and photoacoustic spectroscopy,

compared 115of polymer curing reactions 120-121Wilks' ATR attachment 120-121

Attenuation, defined 669Auger chemical shift, defined 669Auger electrons. See also Electrons.

chemical effects 552-553defined 669energy, principal 550, 551escape depths, and x-ray emission depths,

compared 552inner-shell ionization and de-excitation by 433kinetic energy of 550, 551peaks 551produced 550spectra 550-551yield, defined 669

Auger electron spectroscopy 549-567applications 549, 556-566capabilities 333, 490, 516, 603, 610capabilities, and FIMIAP 583capabilities, compared with classical wet

analytical chemistry 161capabilities, compared with x-ray

photoelectron spectroscopy 568chemical effects 552compared with XPS and x-ray analysis 569data acquisition 555defined 669electron beam artifacts 556elemental detection sensitivity 556estimated analysis time .549experimental methods 554-556general uses 549high vapor pressure samples 556



700/ Index

Auger electron spectroscopy (continued)of inorganic solids, types of information

from .4-6instrumentation 554introduction 550limitations 549, 556point analysis 557-558principles 550-554quantitative analysis 553related techniques 549sample charging 556samples 549, 556-566sensitivity 550, 556spectral peak overlap 556sputtering artifacts 556

Auger electron yield, defined 669Auger emissions

and light-element sensitivity 550probabilities, and qualitative analysis 550

Auger imaging, of integrated circuit 555Auger map, defined 669Auger matrix effects, defined 669Auger microprobe analysis, capabilities 516Auger parameter, in XPS analysis 572Auger process, defined 669Augers, as sampling tools 16Auger transition designations, defined 669Austenite

bright-field image and diffraction pattern . .440retained in steels, Mossbauer analysis of ..287

Austenitic stainless steels, dislocationinteraction .469

Autocorrelation analysis, of atom probecomposition profiles 594

Autocorrelogramsfor iron-chromium-cobalt alloy, effects of

aging 599of spinodally decomposing iron-chromium

cobalt permanent-magnet alloy ....594, 600Automated image analysis. See Image

analysis.Automatic frequency control,

abbreviation 689Automobile

exhaust extract, fluorescence spectrum ofliquid-chromatographic fraction of 79

paint, NAA forensic studies of 233Average grain dislocation density 358Average grain orientation, texture as measure

of. 358Avogadro's number, defined 162, 669

B11- and o-flbers, in rolled copper. 363ll-diketones, as extractant. 170b. See Burger's vector.b. See under Crystal lattice.B. See Magnetic flux density,Babington nebulizers, for ICP sample

introduction 36Baby lotion, liquid chromatographic analysis of

parabens in 655-656Background

correction systems, atomic absorptionspectrometry 51-52

defined 669fluorescence 130intensity, abbreviation for 690parameters defining, RDF analysis 396removal, in EXAFS analysis .412spectral, defined 682

Back-reflection Laue method, x-raydiffraction 329, 330

Backscattered electron 669, 689Backscattered electron detectors

contrast with 502-504ring geometry 503

Backscattering. See also Rutherfordbackscattering spectrometry; Scattering,

analysis and signal processing 631in EPMA quantitative analysis 524fine structure from .408in Rutherford backscattering

spectrometry 629as two-body elastic collision process 629

Back-titrationsin nitrogen determination 173yield of analyte concentration 173

Bakelite mounting, for optical metallographysample 300

Ball and roller bearings, measurement ofresidual stress and hardness of racewayof 380

Ball cratering, for AES sputteringproblems 556

Ball mill, ore samples crushed in 165Band head, in molecular emission 23Bands, molecular, in emission spectroscopy 23Barium

gravimetric finishes 171species weighed in gravimetry 172sulfate ion separation 169sulfuric acid as dissolution medium 165TNAA detection limits 237, 238weighed as sulfate 171weighed as chromate 171

Barium oxide, in binary phosphate glasses .. 131Barkhausen magnetic methods, capabilities

of. 380Barn 669, 691Base-line technique, defined 669Bases

and acids, indicators 172and acids, titrations 172-173analytic methods for. 7

Base SI units, guide for 685Basic chemical equilibria, and analytical

chemistry 162-165Basic NMR frequency, defined 669Baths, chemical, UVIVIS analysis 233Batteries, lead-acid, cycle life and failure

mechanisms in 135bee. See Body-centered cubic materials.BE. See Backscattered electron.Beam-condensing optics, use in IR diamond-

anvil cells 113Beams. See Electron beams.Becquerel, as SI derived unit, symbol for ...685Beer's law

as basis for IR quantitative analysis 117defined 669-670deviations from 70in ion chromatography 665in UVIVIS absorption spectroscopy 61-63, 70

Bend contourspattern, for strain fields in crystals 368polycrystalline molybdenum-rhenium

alloy .445Bending moment, conversion factors 686Benzene, adsorbed, SERS analyses for 136Benzo(a)pyrene, direct determination of 79Benzoic acids, as ion chromatography

eluents 660Berg-Barrett reflection topography method

applicability 368camera for. 369topographs of shadowing due to cleavage

steps 369Beryl

fusion flux for 167sintering agent for 166

Berylliumevaporation fields for. 587photometric analysis methods 64precipitation 169species weighed in gravimetry 172

UVIVIS analysis for chromium, bydiphenylcarbazide method 68

window " 519, 670Beryllium-copper alloys

metallographic AES study 558-559secondary electron micrograph 559

Beryllium oxide, in binary phosphateglasses. . . . . . . . . . . . . . . . . . . . . . . . . . .. 131

Beryllium window 519, 670BESSY, as synchrotron radiation source ... .413Best image voltage 588, 689Best line fit, x-ray spectrometry 97Beta-particle emission, as radioactive decay

mode " 245Beta-ray emission, radiochemical, destructive

TNAA 238Biamperometric titration 204Bias

defined 670of test methodologies, and sampling 12, 13

Binary collisions, low-energy ion-scatteringspectroscopy 604

Binary gold-copper alloys, EPMA analysisof. .. " 530

Binary phosphate glasses, cations bondingin 131

Binding agents, x-ray spectrometry 94Biochemical mixtures, liquid chromatography

of. 649Biological materials

characterization of 1ESR analysis of 264fluid, potentiometric membrane electrode

analysis 181freeze-dried, as x-ray spectrometric

samples '" 93GC/MS analysis of. 639MFS analysis of carcinogenic polynuclear

aromatic compounds in 72NAA determination of toxic elements in ..233PIXE analysis of. 106-107powdered, analysis of. 106-107use of ICP-AES for 31voltammetric monitoring of metals and

nonmetals in " 188Biomolecules, EXAFS analysis of .407Biopsy, GFAAS detection of metals in 55Bipotentiometric titration, as

electrometric 204Birefringence 115, 129Birefringent crystal, defined 670Bismuth


gaseous hydride, for ICP sampleintroduction 36

gravimetric finishes 171in nickel, determination by GFAAS 57photometric analysis methods 64quartz tube atomizers with .49separated from copper 200species weighed in gravimetry 172as trace metal in iron-based steel, AAS

analysis 55weighed as the phosphate 171

Bismuth oxide, in binary phosphateglasses 131

BIV. See Best image voltage.Blackbody, in emission spectroscopy 115Blackening

line 142as optical density 143photoplate 143

Blanksdefined 222, 670preparation, in UVIVIS analysis 68sampling error reduction by 12

Blendingand grinding, of samples 17



and sampling '" 16Blind sample, defined 670Bloch equations, T1 and Tz 280Blocking and channeling, for surface

structure 633Block polymers, SAS applications .405Blooming, dot mapping and 526-527Blue, thymol and bromthymol, as acid-base

indicators 172Body-centered cubic materials

abbreviation for 689and fcc materials, Kurdjumov-Sachs

orientation relationship .439iron-nickel alloy as, EXAFS analysis 416-417

Bohr magneton, in electron spin resonance 254Boltzmann

distribution, defined 670equation 24, 44

Bomb, acid digestion 165Bomb calorimeter ignition, for sample

dissolution 167Bond distances, determined by single-crystal

analysis 354Bonded-phase chromatography

defined 670stationary phases 652

BondingAuger spectrallineshapes showing 552and bonding distance, EXAFS

determined .407, 415infinite nature, and single-crystal analysis 345interatomic bond-lengths, and physical

properties 355pi, defined 679sigma, defined 681substance differences due to 345topologies, RDF analysis and 393, 398

Bond lengths, interatomic, and physicalproperties 355

Borax, as flux 167Borax bead tests, as qualitative wet

analyses 168Borehole logging, PGAA use in 240Boric acid, as binding agent for samples, x-ray

spectrometry " 94Boron

AAS analysis of .46acid-base titrations 172content, in glass, IR analysis 121-122determined in borosilicate glass 179photometric analysis methods 64prompt gamma activation analysis of 240in seawater, determined by electrometric

titration 205separation by distillation 169-shielded samples for epithermal neutron

bombardment 234UVIVIS analysis in aluminum alloys,

Carmine method 68volumetric procedures for 175

Boron nitride, sulfuric acid as dissolutionmedium for 165

Boron tetrafluoride, electrode 184Boron trioxide, as flux 167Borosilicate glass, determination of Band F

in 179Borrmann effect. See also Anomalous

transmission.diffraction geometry for 370in x-ray diffraction 367

Borrmann fan, effect of crystal thicknesson 367

Boule, silicon, alignment for cutting alongcrystallographic planes 342

Boundary structureand crystals, compared 358EPMA analysis of compositional gradients

in " 516Bragg angle, XRPD analysis 337

Bragg-Brentano diffractometers. geometryof. 337

Bragg-Brentano geometry, XRPDanalysis 337

Bragg case, reflection topography 366Bragg equation. See also Bragg's law.

derivation of 327Bragg's law

defined 670in determining pole figures 360diffraction defined by 381electron diffraction patterns in TEM .436electron probe x-ray microanalysis 520-521in single-crystal analysis 348-349in x-ray diffraction 329in x-ray powder diffraction 337and x-ray spectrometers 87

Brasscartridge, EDS and WDS analysis of 530isolation of lead in 173recovery, by microelectrogravimetry 200texture orientations 360

Breaking radiation. See Bremsstrahlungradiation.

Bremmstrahlung radiation. See alsoContinuum; Radiation.

defined 83, 325-326as inelastic scattering process .433Ku aluminum or magnesium x-ray lines as

filter for 570and synchrotron radiation, compared .411as x-ray source for EXAFS .411

Bridgewire, SEM micrograph of corrosion andcorrosion product in 511

Bright-field imagesof annealing twin in rutile .443in ceramic containing crystalline and

amorphous phases .445fcc matrix (austenite) .440for image analyzer microscopes 310iron-base superalloy .442of polycrystalline aluminum 444precipitates on grain boundary, iron-base

superalloy .447transmission electron

microscopy .441-446, 457of unknown phase/particle .457

Brinegeological analysis 665-667as ion chromatography solution 658

Brinell hardness, abbreviation for 690Briquets, as samples 93-94Brittle fracture. See also Embrittlement;

Fracture.of AM samples 587

Broadband tunable dye lasers 128Broad-beam SIMS instrument, for qualitative

analysis 613Broadening. See also Line broadening.

dipole-dipole, in ESR spectra 255separation, x-ray diffraction residual stress

techniques 386Bromcresol green, as acid-base indicator 172Bromides

anions, separation by ionchromatography 659

determined by precipitation titration 164as electrodes 184ion chromatography analysis of geological

waters for 665-666ion chromatography calibration curves

for 666Bromine

epithermal neutron activation analysis 239in graphites, Raman analysis 133indirect determination of 70and methanol, for isolating inclusions from

steel. 176methyl acetate, second-phase test method 177

Index /701

species weighed in gravimetry 172titration with 205TNAA detection limits 237

Bromthymol blue, as acid-base indicator 172Bronzes, isolation of lead in 173BTU, and ash content, in coal 100Buffers

defined 670effects in de arc sources 25potential, use in electrogravimetry 200

Bulk analysis. See also Bulk characterization;Macroanalysis.

of inorganic gases, analytic methods for ....8of inorganic liquids and solutions, applicable

methods 7of inorganic solids, applicable analytical

methods .4-6of organic solids and liquids, techniques

for 9,10Bulk characterization. See also Bulk analysis.

atomic absorption spectrometry .43-59classical wet analytical chemistry 161-180controlled-potential coulometry 207-211crystallographic texture measurement and

analysis 357-364electrochemical analysis " 181-211electrogravimetry 197-201electrometric titration 202-206electron spin resonance 253-266elemental and functional group

analysis 212-220extended x-ray absorption fine

structure .407-419ferromagnetic resonance 267-276gas chromatography/mass

spectrometry 639-648inductively coupled plasma atomic emission

spectroscopy 31-42infrared spectroscopy 109-125ion chromatography 658-667liquid chromatography 649-657molecular fluorescence spectrometry 72-81Mossbauer spectroscopy 287-295neutron activation analysis 233-242neutron diffraction .420-426nuclear magnetic resonance 277-286optical emission spectroscopy 21-30optical metallography 299-308particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187radial distribution function analysis 393-401radioanalysis 243-250Raman spectroscopy 126-138Rutherford backscattering

spectrometry 628-636single-crystal x-ray diffraction 344-356small-angle x-ray and neutron

scattering .402-406spark source mass spectrometry 141-150ultraviolet/visible absorption

spectroscopy 60-71voltammetry 188-196x-ray diffraction 325-332x-ray diffraction residual stress

techniques 380-392x-ray powder diffraction 333-343x-ray spectrometry 82-101x-ray topography 365-379

Bulk materials, sampling of 12-18Bulk samples

composition of. 562, 631defined as gross sample 674DRS analysis for 114electron beam spreading in .434preparation for AEM analysis .450surface, SEM chemical composition .490

Bulk sampling programs, design of 12Bunge formalism

ODF coefficient determined 362



702/ Index

Bunge formalism (continued)and Roe formalism, compared 362in specifying orientation in crystallographic

measurement 359-361Buret

defined 670titrimetry and coulometry 205walls, wetting of 172

Burger's vectorabbreviation for 689one-dimensional defect analysis .465orientation, effect on FIM contrast from

dislocations 588-589Burners, as OES flame source 28Butadiene, polymerization of 132

cc. See under Crystal lattice.c. See under Velocity.Cadmium

air-acetylene flame atomizer for .48in blood, GFAAS analysis 55constant-current electrolysis 200determined by controlled-potential

coulometry 209in furnace atomizers .49gravimetric finishes 171ICP-detennined in plant tissues .41and lead, separated by internal

electrolysis 20 Imicroelectrogravimetry of 200prompt gamma activation analysis of 240-shielded samples for epithermal neutron

bombardment 234species weighed in gravimetry 172volumetric procedures for 175weighed as the phosphate 171

Cadmium oxide, in binary phosphateglasses 131

Caking, of sampling materials 16Calcite, XRDP analysis of ZnO in 342Calcium

added to nuclear waste, EPMAanalysis 532-535

in cement, optical emission spectroscopyfor 21

determination in paint, absorption andenhancement effects 98

EDTA titration 173as electrode 184gravimetric finishes 171ICP-detennined in plant tissues .41ions, exchanged in water softeners 658-659species weighed in gravimetry 172sulfate ion separation 169sulfuric acid as dissolution medium 165TNAA detection limits 237volumetric procedures for 175weighed as the fluoride 171

Calcium chloride, effect on vaporizationinterferences 29

Calcium/magnesium (water hardness) aselectrode 184

Calcium oxidein binary phosphate glasses 131uncombined, analysis in Portland cement. .179

Calcium phosphate, and vaporizationinterferences 29

Calculators, desktop 310Calibration

classical wet analyses for. 162curves, for quantitative x-ray

spectrometry 97-98energy, in spectrum-fitting programs 91for ICP-AES 34samples, by RBS 628for TNAA 236

wavelength, MFS analysis 77of wavenumber, FT-IR spectroscopy 112for XPS qualitative analysis 572

Californium-252 neutron sources, use inborehole logging 240

Calomel electrode, defined 670Calorie, abbreviation for. 691Cambridge Crystallographic Data File 355Cameras

back-reflection pinhole, schematic 334Debye-Scherrer, XRPD analysis 335Gandolfi, XRPD analysis 335glancing-angle, XRPD analysis 336Guinier, in asymmetric transmission

arrangement 335Guinier, XRPD analysis 335-336Huber Guinier. 336Laue, XRPD analysis 334-335micro-, XRPD analysis 336pinhole, XRPD analysis 334-335Read, XRPD analysis 336reflection 369transmission pinhole, schematic 334

Cam lobe, anti wear film analyzed for ..565-566Candela, as SI base unit, symbol for. 685Capacitance

effects in pulse polarography 193SI derived unit and symbol 685

Carbidesas inclusions 176particles of, atom probe mass spectrum 592

Carbonactivated, RDF analysis of 399-400AES analysis of surface chemistry 552-553amorphous, EELS edge shapes for .460Auger chemical map for 557combustion method for elemental

analysis 214content, sink/float density separations

for 177determination by high-temperature

combustion 221-225electrode systems based on 191glow discharge to determine 29graphitic, determined by selective

combustion 223-224graphitic, neutron, x-ray scattering and

absorption characteristics .421infrared detection, high temperature

combustion 223in inorganic solids, applicable analytical

methods .4, 6interstitial, content in silicon wafers 123KVV lineshapes, effect on quantitative

analysis 553in metal carbide, EELS edge shape for .. .460mobile, determined in iron/steels 178prompt gamma activation analysis of 240removal from organic matrix 167surface, determined 223-224vitreous, Raman analysis 132

Carbon dioxidegas mass analysis of. 155as SFC solvent 116use to determine carbon 221-225in weld relay, gas mass spectroscopy of .. 156

Carbonic acid, conductometric titration of ..203Carbonitrides, as inclusions 176Carbon monoxide, electrometric titration

for 205Carbon steels. See also Steels.

polished, monolayers adsorbed on 118-120residual stress distribution in 389surface effects of grinding analyzed by

Miissbauer. 287Carburizing steels, compressive layer and

hardness produced by 380CARCA. See Computer-assisted rocking cllrve

analysis.

Carcinogenic polynuclear aromaticcompounds, MFS analysis of. 72

Carmine method, for boron in Al alloys 68Carrier

defined 670effects in de arc sources 25gas, in analytic ICP systems 34

Carrousel sample holder, in Augerspectrometer 554

Cartridge brass, EDS and WDS analysisof. 530

Case hardening, chemical surface studiesof. 177

Cassiterite, fusion flux for 167Castings, preferred crystallographic orientations

in 358Cast iron, glow discharge to determine C, P,

and Sin 29Catalysis

heterogeneous, FIMIAP study of 583surface, AES analysis for 549

Catalystsanalytic methods applicable 6chlorine in, determined by electrometric

titration 205chromia alumina 265effects, neutron diffraction .420electron spin resonance for 263EXAFS structural analysis of .407influence of surface stucture on 536metal oxide, Raman analysis 133prompt gamma activation analysis of 239surfaces of, studies 114, 253

Catalytic techniques, and electrometrictitration, compared 202

Cathodebombardment 26mercury, in electrogravimetry 199metals adherence, in electrogravimetry 198sputtering 27

Cathode-ray tube 670, 690Cathodoluminescence 507,670,689Cations

defined 670ion chromatography analyses 658-667inorganic, determined by ion

chromatography 663as positively charged ions 659potentiometric membrane electrode

quantitative analysis 181Cauchy peak location method, XRD residual

stress techniques 386Caustic fusion, use in ion

chromatography 664Cavities, microwave-resonant. 256CBED. See Convergent-beam electron

diffraction.CBEDP. See Convergent-beam electron

diffraction pattern.CDF. See Centered dark-field (image).Cell configuration, as electrolytic inclusion and

phase isolation 176Cells

classical types 199constant-current. 199-200

. controlled-potential 199-200and electrodes, for

electrogravimetry 199-200electrolysis 199, 207-208electrolytic, to decrease concentration

polarization 200half-, volumetric analysis of 163for internal electrolysis 199kinetics of martensite decomposition

in 316-318small, rotation about axes .473structure, dislocation analysis of .470-473structure factor equation for 329typical dual anode ·199



Cellulosepowdered, as binding agent for x-ray

spectrometry samples 94removal of sulfur trioxide, in high-temperature

combustion " 222as x-ray tube filter 90

Cementanalyses of 99-100calcium in, optical emission spectroscopy

for 21Portland . . . . . . . . . . . . . . . . . . . . . . 30, 179

Centered dark-field image 689Central electronic processor, image

analyzers .310Centrosymmetry, determining effect on ODF

coefficient. 362Ceramic nuclear waste forms, EPMA study of

simulant. 532-535Ceramics. See also Ceramics, characterization

of.analytic methods applicable 5characterized 1containing crystalline and amorphous

phases .445crystalline materials 381crystallographic texture measurement and

analysis 357metallized, electron diffractionlEDS method to

identify unknown phase in .457-458microstructural changes 366multiphase, IA quantitative determination of

second-phase phenomena 309multiphase, SIMS phase distribution analysis

in 610Permalloy film thickness, x-ray spectrometry

for 100-101phase separation analysis by SAXSISANSI

SAS .402, 405powder, XRPD analysis of crystalline phases

in 333SAS applications .405SIMS analysis of surface layers 610single-phase, image analysis of. 309TEM bright-field images and diffraction

patterns .445Ceramics, characterization of. See also

Ceramics.analytical transmission electron

microscopy .429-489atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206

.electron probe x-ray microanalysis 516-535electron spin resonance 253-266extended x-ray absorption fine

structure .407-419inductively coupled plasma atomic emission

spectroscopy 31-42infrared spectroscopy 109-125ion chromatography 658-667low-energy electron diffraction .536-545low-energy ion-scattering

spectroscopy 603-609neutron activation analysis 233-242neutron diffraction .420-426optical emission spectroscopy 21-30particle-induced x-ray emission 102-108potentiometric membrane electrodes ..181-187radial distribution function analysis 393-401Raman spectroscopy 126-138Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627single-crystal x-ray diffraction 344-356

small-angle x-ray and neutronscattering .402-406

spark source mass spectrometry 141-150ultraviolet/visible absorption

spectroscopy 60-71voltarnmetry 188-196x-ray diffraction 325-332x-ray diffraction residual stress

techniques 380-392x-ray photoelectron spectroscopy 568-580x-ray powder diffraction 333-343x-ray spectrometry 82-101x-ray topography 365-379

Ceriumredox titration 175TNAA detection limits 238volumetric procedures for 175

Cesiumcations, in glasses, Raman analysis 131epithermal neutron activation analysis 239organic precipitant for 169species weighed in gravimetry 172TNAA detection limits 238use with flame emission sources 30

CESR, as synchrotron radiation source .413CHA. See Concentric hemispherical analyzer.Change in quantity, symbol for 692Change of state, as x-ray diffraction

analysis 325Channeling. See also Electron channeling.

angular scan, lattice strain measurementby " 635

and blocking, surface structure study by ..633contrast, source of 504and dechanneling 634effect, RBS analysis 630-631electron, capabilities 365electron, patterns and contrast 504-506ion scattering to study surface structure

by 633for lattice location of solute atoms 633patterns 504-506, 670selected-area patterns 505-506spectrum 632-633

Channeling angular scan, lattice strainmeasurement by 635

Channeling patterns 504-506, 670Channel plate multiplier, for x-ray

photoelectron spectroscopy 571Characteristic electron energy loss

phenomena, defined 670Characteristic Ka peaks, and bremsstrahlung

radiation 571Characteristic radiation

defined 670spectra 326

Characterizationtechniques, acronyms for. 689of thin films 559-561

Characterization of ceramics. See Ceramics,characterization of.

Characterization of corrosion products. SeeCorrosion products, characterization of.

Characterization of gases. See Gases,characterization of.

Characterization of geologic samples. SeeGeologic samples, characterization of.

Characterization of glasses. See Glasses,characterization of.

Characterization of inorganic materials. SeeInorganic materials, characterization of.

Characterization of liquids. See Liquids,characterization of.

Characterization of metals and alloys. SeeMetals and alloys. characterization of.

Characterization of minerals. See Minerals,characterization of.

Characterization of organic materials. SeeOrganic materials, characterization of.

Index /703

Characterization of solids. See Solids.characterization of.

Characterization of surfaces. See Surfaceanalysis and characterization; Surface.

Charcoal, activated, Raman analysis 132Charged particle beam, in x-ray

spectrometry 82Charged particle detectors, for x-ray

diffraction 245-246Charred carbon, ESR studied 263Chelate, defined 670Chelometric titration 164, 173, 174Chelons, formation 164Chemical bonding

defined 670effects in EXAFS .415

Chemical complexes, ESR studied 263Chemical equilibrium, defined 163Chemical etching. See also Etching 144-145Chemical microanalysis, FIMIAP 583Chemical preparations, radioanalysis 247Chemical reactions

products, liquid chromatography analysisof 656-657

rates of, measured 60, 243surfaces (chemisorbed layers), LEED

analysis 536Chemical reagents. See also Reagents.

analytic methods for 6-10GFAAS analysis of 58inorganic, analytic methods for 6, 7organic, analytic methods for 9, 10

Chemicalsanalysis 72, 177commercial, voltammetric characterization of

metals in 188surface species identified 568systems, analyzed ' 263wastes assay for toxic elements, NAA for .233

Chemical shifts, in XPS analysis 572Chemical surface studies, classical wet

chemistry 177-178Chemisorption, defined 670Chemistry. See also Analytical chemistry;

Classical wet analytical chemistry.atmospheric, PIXE studies in 106of elements at surfaces, AES lineshapes

showing 552-553of grain boundaries 561-562irradiation 235

Chips, steel, AAS analysis 55Chloride

anions, separation by ion chromatography 659determined by precipitation titration 164as electrode 184ferric, analysis in graphite 133ions 169, 201Mohr titration for 173quantitative determination of metals in

presence of, electrogravimetry 197weighing as the, gravimetry 171

Chlorinationinclusion testing by 176for iron and manganese carbides and sulfides

in residues 177as second-phase test method 177

Chlorinein coal or catalysts, determined by

electrometric titration 205as NAA sample contaminant 236species weighed in gravimetry 172TNAA detection limits 237volumetric procedures for 175

Chloroform, extractants for 170Chloroplasts, ESR studied 264Chord measurements, image analysis 316Chromate, weighing as the, gravimetric

analysis 171Chromatic aberration, defined 670



704/ Index

Chromatogramscommon anions separated by single-column

ion chromatography 661defined 670eluent-suppressed ion 660fiber-suppressed ion 660for geological brines 666for glass microballoons 667for ion chromatography separation and

detection of alkali and transitionmetals 660-661

ion-exchange, of radioactive alkali metals 653ion-pair, of napthylamine sulfonic acids 653normal phase .. , 652reverse-phase, of an organic mixture 653reverse-phase, of parabens and baby lotion

extract 655single-ion 645size-exclusion 654typical total ion 644

Chromatographic effluents, IR identificationof 109

Chromatographshigh-performance liquid 665liquid 650-651, 665liquid, essential components 650

Chromatographybonded-phase 652defined , 670gas chromatography/mass

spectroscopy 639-648ion 658-667ion-exchange 168, 653liquid , 649-657liquid-liquid 652liquid-solid 651-652normal-phase 652paper 168potentiometric membrane electrodes as

detectors for 181preparative liquid 654reversed-phase 652-653size-exclusion 654

Chromatopyrogramfailed nitrile sheath 648intact neoprene sheath 648

Chromia alumina catalysts, ESR analysisof. , 265

Chromindur ductile permanent magnets,FIMIAP analysis of 598-599

Chromite oressample dissolution mediums 166sulfuric acid as dissolution medium 165

Chromiumdepletion, in a weld zone 179determined by controlled-potential

coulometry .. , 209determined in stainless steel 146in dichromate ion, analysis for 70evaporation fields for 587frequency-distribution curves 601in hydrogen peroxide, GFAAS analysis 57-58ICP-determined in plant tissues .41ICP-determined in silver scrap metal .41in iron-base alloys, flame AAS analysis 56isotope composition and intensity 146loss, analysis at weld zone 179neutron and x-ray scattering, and absorption,

compared .421partitioning oxidation states in 178permanganate titration for 176phosphoric acid as dissolution medium 165photometric analysis methods 64qualitative tests to identify 168redox titrations 175sensitization, Inconel 600 .483TNAA detection limits 238trace, in hydrogen peroxide, GFAAS analysis

for , 57

trace levels in H202 , GFAAS,determined 57-58

UVNIS analysis in beryllium, bydiphenylcarbazide method 68

volumetric procedures for 175Chromophores, isolated, in UVNIS

analyses 63Churchill two-line method, SSMS calibration

curves 143Cinchonine, as narrow-range precipitant 169CIRCLE. See Cylindrical internal reflection

cell.Circuits

electrical, EPMA failure analysis for 531for electrolysis 199polarographic 189

CL. See Cathodoluminescence.Classical, electrochemical, and radiochemical

analysiscapabilities 333classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrogravimetry 198-201electrometric titration 202-206elemental and functional group

analysis 212-220high-temperature combustion 221-225inert gas fusion 226-232neutron activation analysis 233-242potentiometric membrane electrodes .. 181-187radioanalysis 243-250voltammetry 188-196

Classical gravimetric analysis 170-171Classical wet analytical chemistry 161-180

applications 161, 178-179appropriateness of methods 162basic chemical equilibria and analytical

chemistry of 162-165as basis for spectrographic calibration ., .. 162buffer solution 163capabilities compared with ion

chromatography 501capabilities, compared with voltammetry .. 188chemical equilibrium 162-165chemical surface studies 177-178common ion effect 163coprecipitation 163estimated analysis time 161general uses 161gravimetry 170-171half-cell reactions 163-164inclusion and second-phase testing 176-177introduction 162Jones reductor 175-176Kjeldahl determination 172-173limitations 161partitioning oxidation states 178qualitative methods 167-168reduction-oxidation reactions 163-164related techniques 161sample dissolution 165-167samples 161, 165, 178-179separation techniques 168-170solubility products constant 163techniques for subdividing solids in 165titrations, acid-base 172-173titrimetry 171-176

Classical wet chemistry. See Classical wetanalytical chemistry.

Classical wet methods, appropriateness of .. 162Cliff-Lorimer (standardless ratio) technique,

microanalysis .447Clinging, electrostatic, of sample materials .. 16Clustering, atom probe composition profile

of. 593CMA. See Cylindrical mirror analyzers.Coal

analysis, PGAA for 240analytic methods for 9

analyzed by x-ray spectrometry 100ash, XRPD study of phases in 333BTU and ash content in 100chlorine in, determined by electrometric

titration 205derivatives, analytic methods for 9fly ash, SSMS analysis 147-148gasification and liquefaction products, GC/MS

analysis of volatile compounds in 639hydrosulfurization, Raman surface analysis of

molybdenum oxide catalysts used for ... 133local structure of trace impurities, EXAFS

determined .407sintering agents for. 166x-ray spectrometric results 100

Coal fly ash, copper and lead determinedin 147-148

Coarsening, and crystallization, aluminum,by x-ray topography 376

Coating intensity method, for thin-film samplepreparation 95

CoatingsAES in-depth compositional analysis 549metal, measurement 177organic, measurement 177PIXE analysis of 102products of, x-ray spectrometric analysis .. 100system, diffusion phenomena in .....576-577tallow-base, gas chromatographic

measurement. 177zinc-phosphate, Auger imaging 558

Cobalt. See also Cobalt-base alloys.compounds, trace nickel determined

in 194-195determined by controlled-potential

coulometry 209determined in samples containing chloride

ions 201evaporation fields for. 587in iron-base alloys, flame AAS analysis of 56isolation in high-temperature alloys 174neutron and x-ray scattering, and absorption,

compared .421and nickel, corrosion in aqueous alkaline

media 135photometric analysis methods 64qualitative tests to identify 168separation, by phenylthiohydantoic acid 169species weighed in gravimetry 172TNAA detection limits 238volumetric procedures for 175

Cobalt-base alloys. See also Cobalt.hydrogen peroxide dissolution medium 166stacking faults in fcc phase .466yttrium segregation in .483

Cobalt nitrate, de and differential pulsepolarograms of nickel in 194-195

Codeposition, in constant-current methods ofelectrogravimetry 198

Coefficients, mass absorption 85Coherent atomic scattering intensity,

abbreviation for 690Coherent Bragg diffraction, analytical

transmission electron microscopy .436Cold finger, defined 670Cold-rolled steel, AES analysis of corrosion

resistance in 556-557Cold work

percent, measured 380, 390plastic strain, topographic methods for ... .368

Collection optics 24, 128Collector slit, in gas mass

spectrometers 153, 154Collimate, defined 670Collimation

defined 670neutron diffraction .422x-ray, basic methods .403

Collimators, Soller 87



Collision-activated dissociation mass spectra,gas chromatography/mass spectrometry 647

Collisional line broadening, in emissionspectroscopy '" 22

Collision kinematics, RBS analysis 629Collisions, binary, LEISS analysis 604Color

development and stability, in UVNISanalysis 68

or tint etching, of image analysis samples 313Color centers

defined 670detected by ESR 263

Color comparisonkits '" " .66-67in UVNIS absorption analysis 66

Colorimetry, schematic of Nessler tube 66Color-producing groups. See Chromophores.Coma, defined 670Combustion

accelerators 221-222determination of carbon, hydrogen, and

nitrogen by 214furnaces, high-temperature

combustion 221-225high-frequency 221-225high-frequency, typical configuration 222products, detection in high-temperature

combustion 222total and selective, sample

preparation. . . . . . . . . . . . . . . . . ....223-224Combustion method, for elemental analysis of

carbon, hydrogen, and nitrogen 214Committee on Characterization of Materials,

Materials Advisory Board, NationalResearch Council 1

Common ion effect, in gravimetric analysis 163Common logarithm (base 10), abbreviation

for 690Compensating eyepieces, defined 671Complex, numbers of ligands determined in ..70Complexation

defined 671in internal electrogravimetry, effects of 200organic complexing agents and metals

determined fluorimetrically by 74selected, UVNIS '" " 65-66separation, for interferences 65in voltammetry 193-194

Complexing agentseffect on decomposition potentials 198effect on UVNIS analysis 64organic, determined fluorimetrically 74

Complex multicompoilent glass, EDS andWDS x-ray spectra of 521

Complexometric titrationsclassical wet chemical analysis 164in internal electrolysis 201

Compositesanalytic methods applicable 6defined 671microstructural changes studied by x-ray

topography 366organic, analytic methods for 9

Composite sample, defined 13Composition

atomic-scale, FIMlAP for 584of bulk garnets 628bulk, of nickel alloys 562of bulk samples .. " 631bulk, XRS analysis 83chemical, determined by atom probe

microanalysis 591chemical, of surfaces, AES analysis for 549vs depth, passive film on tin-nickel

substrate 608-609of iron oxide films, determined 135and layer thickness, of thin films 631-632of lunar surface, NAA application for ....234

of materials, and materials characterization .. 1microanalysis, electron probe x-ray

microanalysis. . . . . . . . . . . . . . . . 517-518of mixtures, EFG analysis 213nondestructive XPS 568and purity, NAA analyis for 233SSMS verification of alloy .......•..... 141

Compositional depth profile. See alsoComposition; Compositional mapping;Composition profiles.

defined 671Compositional gradients, microbeam

analysis 530Compositional mapping

digital. 528-529by electron probe x-ray microanalysis 525-529of heterogeneous specimens 516

Composition profiles. See also Depth profiles;Depth profiling.

depth, atom probe microanalysis 593depth, gold-nickel-copper metallization

system " 560depth, LEISS analyses for 603of elemental distribution in thin films, by

XPS 568of FIMlAP analyzed ductile magnets 599for iron-chromium-cobalt alloy 600low-level dopants 610x-ray microanalysis, AI-4.7Cu .462

Compound analysis. See also Compound orphase identification; Compounds.

chemical, flame AAS for major and minorcomponent analysis 56

gas analysis by mass spectroscopy 151-157of inorganics 7, 8of organics 9, 10

Compound or phase identificationanalytical transmission electron

microscopy .429-489electron probe x-ray microanalysis 516-535elemental and functional group

analysis 212-220field ion microscopy 583-602gas analysis by mass spectrometry 151-157gas chromatography/mass

spectrometry 639-648infrared spectroscopy 109-125liquid chromatography 649-657molecular fluorescence spectrometry 72-81Mossbauer spectroscopy 287-295neutron diffraction .420-426nuclear magnetic resonance 277-286optical metallography 299-308Raman spectroscopy 126-138single-crystal x-ray diffraction 344-356small-angle x-ray and neutron

scattering .402-406x-ray diffraction 380-392x-ray powder diffraction 333-343

Compounds. See also Compound analysis;Compound or phase identijication; Organiccompounds.

chemical analysis by controlled-potentialcoulometry 207

chemical, flame AAS for major and minorcomponent analysis " 56

cobalt, voltammetric analysis of trace nickelin 194-195

extended x-ray absorption fine structurefor .407

fluorescent organic, in volumetricanalysis 164

identification of, as x-ray diffractionanalysis 325

inorganic, applicable analyticmethods 6, 151

inorganic, gas analysis of . . . . . . . . . . . . . .151inorganic, molecular requirements for

fluorescence in 73-74

Index /705

inorganic solid, bulk analyses methods for ..6for molecular structure, dynamics and

environment of 109NMR analysis 277organic, analysis of 60, 73-74, 151, 213purified, liquid chromatography isolation for

synthetic purposes 649sublattice ordering in intennetallic, NMR

analysis 283vanadium determined in 206weighing as the, gravimetric analysis 171

Compton scatter/scatteringdefined 671intensity, effect of decreasing mass absorption

on 99and Rayleigh scatter, x-rays 85for rhodium tube 99from x-ray absorption 84

Compton wavelength, defined 84Computer-assisted rocking curve analysis

with position-sensitive detector 372abbreviation 689

Computer disks, as samples, XRS 95Computer-related materials, XRS analysis

of 82, 95Computers. See also Microcomputers.

-controlled gas mass spectrometer. 152for ICP-AES systems 39for MFS analysis 77x-ray powder diffraction 340

Computer software. See Software.Concave grating, defined 671Concentration

absorbance as function of 63, 64of amount of substance, SI derived unit and

symbol for 685of analyte elements, and intensity in x-ray

spectrometry 99atomic, of surface elements 603component, constant, maintained by

electrometric titration 202defined 671and diffusion current 190exponential decay of radiant power as

function of 62high, and well-resolved peaks, gold-copper

alloy analysis with 530profiles .475, 610spin wave stiffness as function of 273vs sputter etching time, Inconel 558, 625UVNIS measured 63-66weight fractions as, EPMA quantitative

analysis 524Concentration profiles

elemental, by SIMS 610hydrogen 610molybdenum, in Ni-Cr-Mo alloy .475oxide surfaces, SIMS 610

Concentric hemispherical analyzer,abbreviation 689

Concentric nebulizers, for analytic ICPsystems 34-35

Condensates, as ion chromatographysolutions 658

Condenserdefined 671lens, defined 671

Conductancedefined 671mho, as original ion chromatography unit

of. 659SI derived unit and symbol for 685

Conduction electronsESR study 261-263excitation leading to secondary-electron

(low-energy) emission .433-434Conductive solids nebulizer

abbreviation for 690as solid-sampling device 36



706/ Index

Conductive-thermal detection, inert gasfusion 229-230

Conductivitydetection, ion

chromatography 659-661, 663, 665electrical, as ion chromatography

detector 659lower, PLAP analysis of 597thermal, conversion factors 686thermal, SI derived unit and symbol for. ..685

Conductivity detectioneluent-suppressed 659-660of inorganic anions and cations determined by

ion chromatography 663of inorganic ions determined by ion

chromatography 663single-column ion chromatography

with 660-661Conductivity detectors, ion

chromatography 665Conductometric oxidation-reduction titrations

(redox), rarity of 203Conductometry

and amperometry, compared 204capabilities, compared with voltammetry .. 188

Conductorsone-dimensional, nonstoichiometric salts

as 355use of glow discharges with 28

Cone blenders, for sampling 17Cones

deficiency and diffraction 327, 371formation, AES analysis 556

Confidence level, defined 671Confidence limits, in sampling bulk

materials 13Configuration, SAS techniques for 0405Conformation

effects, polymer blend system IRanalysis 118

molecular, and stereochemistry, IRdetermination of 109

Connectorsfailure of aluminum wire 531-532LEISS identification of surface stains and

corrosion products on 607stained, LEISS analysis 607surface strains and corrosion products on ..607

Connes's advantage, in Ff-IRspectrometers 112

Conostan C-20, EDS determination of sulfurin , 101

Constant cell potential, abbreviation for 690Constant-current cells, for

e1ectrogravimetry 199-200Constant-current electrolysis, separation and

analysis of metal ions by 200Constant-current methods, of

electrogravimetry 198Constant-voltage electrogravimetry 199Contacts, electrical, XPS analysis of surface

films on 578-579Contamination

of apparatus or reagents, controlling for. ... 12by nonvolatile organics, in XPS samples ..575radioactive, in NAA samples 236sampling, quality assurance and 17surface, RBS analysis 628surface, trace analysis 177

Continuous-wave gas lasers, Ramanspectroscopy 128

Continuous-wave NMR spectrometer, withfield sweep and crossed coil detector ...283

Continuous-wave spectrometers 258, 283, 690Continuum

defined 671effects, electron probe x-ray

microanalysis 527-528emission, intensity of 83-84

overlap, as spectral interference in ICP-AES 34

-source background correction, atomicabsorption spectrometry 51

-source systems, atomic absorptionspectrometry 52-53

x-rays, as inelastic scattering process 0433Continuum radiation, defined 83Contrast

absorption, analytical electronmicroscopy .444-445

atomic number, use in two-phase alloyanalysis 508

with backscattered electron detector ..502-504channeling, source of. 504diffraction, analytical electron

microscopy .444-445electron channeling 504-506emission, scanning electron microscopy ...502image, scanning electron microscopy 500-504magnetic, as SEM special technique 506mechanisms, analytical electron

microscopy .444-445phase, analytical electron microscopy 445sample material influence on 0497voltage, as SEM special technique 506-507

Control, process or production. See Processcontrol.

Controlled-potential cells, forelectrogravimetry 199-200

Controlled-potential coulometry 207-211apparatus for 208applications 207, 210-211capabilities 188, 197and controlled-potential electrolysis 208-210defined 671electrometric titration and, compared 202estimated analysis time 207general uses 207introduction 207, 210limitations 207related techniques 207reversible processes 208samples 207technique 210

Controlled-potential electrogravimetry,automatic potentiostat for 200

Controlled-potential electrolysiscapabilities 207, 208-210as electrogravimetric method 199

Controlled tilting experiment, for unknownphase/particle confirmation 0458

Controlled waveform spark, optical emissionspectroscopy 25, 26

Convection, effects in voltammetry 189Convergent-beam electron diffraction

analytical transmission electronmicroscopy 0438-440

defined 671in diffraction-induced grain boundary

migration 0462-464patterns 441, 439, 689for phase diagram determination 0474structural analysis by 0461-464

Convergent-beam electron-diffraction patternabbreviation 689with analytical electron microscopy . .431, 439

Conversion electron Miissbauer scattering,austenite result of. 294

Convertercurrent/voltage 199microchannel plate-image, field ion

microscopy 584Convolutional integral, ESR line and 261Coolidge x-ray tubes, in wavelength-dispersive

x-ray spectrometers 88Coordination compound, defined 671Coordination geometry

determination of 354

effects on XANES spectrum 0415Coordination number, defined 671Copolymer

block, microphase separation by SAXS/SANS/SAS 0402

ratios, NMR determination of 277Copper. See also Copper alloys. Copper alloys,

specific types.analysis in presence of lead, cell for 199in archaeological samples 186chip combustion accelerators 222constant-current electrolysis 200controlled-potential electrogravimetry of ..200deposition 198, 199determination using internal electrolysis ...200determined by controlled-potential

coulometry 209determined in coal fly ash 147dominant texture orientations 359as electrode 184estimated in copper-manganese alloy 201evaporation fields for. 587excitation and emission for photoejection of

electrons 85, 87films, LEISS study of oxidation of. 609finished, cracking problems analyzed by inert

gas fusion 231-232gravimetric finishes 171high-purity, SSMS analysis 144hydrogen determined in 231-232ICP-determined in plant tissues AlICP-determined in silver scrap metal Alingot, spider cracks 302ion-scattering spectra from 604in iron-base alloys, flame AAS analysis 56iron in, phase analysis 294LEISS study of oxidation, using oxygen ..609in magnesium alloys, by hydrobromic

acid-phosphoric acid method 65mass absorption coefficient vs x-ray

energy 85,87metallochrome color, use in titration 174mills, prompt gamma activation analysis use

in 240mining, prompt gamma activation analysis use

in 240oxidation using 180 609photoejection of electrons in 85photometric analysis methods 64qualitative tests to identify 168radiation 326recovery in copper foil. 200rolled, Euler space 363separation, from zinc 198as SERS metal 136species weighed in gravimetry 172strip combustion accelerators 222surface, oxidized, LEISS spectra from 609TNAA detection limits 237transition diagram for. 87transition for K lines of. 86, 87tubing 361, 363tubing, (Ill) pole figures from 363volumetric procedures for 175zinc at grain boundaries of 527zinc-containing, digital composition map ..528

Copper alloys. See also Copper; Copper alloys,specific types.

AEM analysis in .471-473analysis for nickel, by dimethylgloxime

method 66FIM sample preparation of 586UVIVIS analysis for antimony, by

iodoantimonite method 68Copper alloys, specific types. See also Copper;

Copper alloys.10100 tubing, (Ill) pole figure from inside

wall 36310100 tubing, ODF using Euler plots 361



10100 tubing, pole figure, from midwall ..36226000 (cartridge brass, 70%), microstructure

from several directions 305Cu-3Zn, expected pole orientations of

preferred orientations 360Cu-3Zn, grain orientations 360Cu-3Zn, measure (111) pole figure for. 360ETP, dislocation cell structure, by cold

rolling . . . . . . . . . . . . . . . . . . . . . . . . . . . .469OFHC, dislocation cell structure

analysis .472-473Copper-beryllium alloys

analysis for copper by aluminon method 65analysis for iron, by thiocyanate method 68

Copper chip combustion accelerator 222Copper-iron alloys

Miissbauer absorption spectrum 294phase analysis, Miissbauer spectroscopy ..294

Copper-manganese alloyscopper content estimated 201estimation of copper in 201

Copper strip combustion accelerators '" .222Copper sulfate, formation, in high-temperature

combustion 222Copper-titanium alloys, high-resolution mass

scan for 616Copper tubing

ODF using Euler plots 361pole figures from 363

Copper-zinc alloys, grain orientation in 360Coprecipitation, in gravimetric analysis 163Core excitation, effect on Auger electrons ..551Corers; as sampling tools 16Cores, transformer, analysis of 224Correlated fluctuations, SAS techniques

for .405Corrosion. See also Corrosion products;

Corrosion products, characterization of;Corrosion resistance.

AES identification of chemical-reactionproducts in 549

and corrosion products, SEM analysis ofbridgewire 511

effect of boundary precipitation and solutesegregation on 549

electrochemically based, determined inaqueous environments 134

electrochemically based, Raman studies 135gas-phase, Raman analysis 135metal, Raman analysis 126, 134-135on metals, analysis of. 134-135Miissbauer analysis of 287of nickel and cobalt in aqueous alkaline

media 135of nickel and cobalt, Raman studies 135in pyrotechnic actuators 510surface, AES analysis for 549and surface stains, LEISS identified on

connector '" 607Corrosion products

IR determination of molecular structure andorientation in 109

LEISS determined '" 603on steel, Miissbauer analysis 287XRPD analysis of crystalline phases in 333

Corrosion products, characterization ofanalytical transmission electron

microscopy .429-489atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis 516-535inductively coupled plasma atomic emission

spectroscopy 31-42infrared spectroscopy 109-125

ion chromatography 658-667low-energy ion-scattering

spectroscopy 603-609Miissbauer spectroscopy 287-295optical emission spectroscopy 21-30particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187Raman spectroscopy 126-138scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627spark source mass spectrometry 141-150voltammetry 188-196x-ray photoelectron spectroscopy 568-580x-ray spectrometry 82-101

Corrosion resistanceof cold-rolled steel 556-557of nebulizers 35painted, cold-rolled steel 556of spray chambers 35

Corundum, fusion with acidic fluxes 167Cosmochemical research, use of NAA in ..233Cotangent, abbreviation for 690Coulomb, symbol and abbreviation

for. 685, 691Coulometers, electronic 203Coulometric titration

capabilities, compared with electrometrictitration 197

cell, with platinum generator electrode 205as electrometric 204-205measured electric quantities in 202

Coulometry. See also Controlled-potentialcoulometry.

capabilities, compared with voltammetry .. 188defined 671

Counterelectrodedefined 671x-ray diffraction 246

Countseffect of image analysis on 309in image analysis 312per second, abbreviation for 690pulse, Auger spectrometer 554x-ray diffraction 246

Couples, diffusion .477-478Covalent bond, defined 671Cracking, in finished copper, IGF

analysis 231-232Crazes, structure in glassy polymers, by

SAXS/SANS/SAS .402Creep strengthening, effect of segregation

in 598Cretaceous-Tertiary boundary, iridium

determined by NAA at 240-241Critical micelle concentration .. 118,671,690Critical-point phenomena, Miissbauer analysis

of. 287CrossOow nebulizers, for analytic ICP

systems 34-35Cross-section transmission electron

microscopy, capabilities 628Crown polyethers, as solvent extractant 170CRT. See Cathode-ray tube.Crucibles

graphite, for IGF analysis 227for sinters/fusions 166-167

Crushers, for sampling 16Crushing, as wet chemical technique for

subdividing solids 165Cryogenic ESR studies 257Cryogenic grinding, for samples 16Cryopump, defined 671Cryptands, as general-use reagent 170Crystal classes, described 346-347Crystal Data, data base 326, 355Crystal diffraction 346Crystal geometry, as x-ray diffraction

analysis 325Crystal lattice. See also Lattices; Superlattices.

Index / 707

length along the a axis 689length along the b axis 689length along the c axis 689strain measured, for residual stress

calculation 381Crystalline materials

membrane electrodes, solid 182powder compacts, preferred orientations

in 358solids, ESR detection of color centers and

defects in 253-266x-ray diffraction residual stress techniques

for 381Crystalline phases

from crystal structures 345identified by XRPD 333unknown, unit cell identification 353use of cell information to identify

unknown 353Crystalline state, defined 326Crystallinity, of fossil fuels, ESR

determined 253Crystallite size

EPMA analysis 516-535field ion microscopy 583-602measured, scanning electron

microscopy .490-515and subgrain size/shape, measured by

x-ray topography 365x-ray diffraction 325-332

Crystallization, and coarsening, in aluminumx-ray topographs 376

Crystallographic growth. See Preferredcrystallographic growth.

Crystallographic information. See alsoCrystallographic texture measurement andanalysis; Texture.

analytical transmission electronmicroscopy .429-489

crystallographic texture measurement andanalysis 357-364

electron spin resonance 253-266extended x-ray absorption fine

structure .407-419ferromagnetic resonance 267-276field ion microscopy 583-602infrared spectroscopy 109-125low-energy electron diffraction 536-545Miissbauer spectroscopy 287-295neutron diffraction .420-426nuclear magnetic resonance 277-286radial distribution function analysis 393-401Raman spectroscopy 126-138scanning electron microscopy .490-515single-crystal x-ray diffraction 344-356small-angle x-ray and neutron

scattering .402-406x-ray diffraction 325-332x-ray powder diffraction 333-343x-ray topography 365-379

Crystallographic phase transitions, by ESRanalysis 257

Crystallographic planes, alignment for cuttingalong 333, 342

Crystallographic preferred orientations,measurement and analysis 357-364

Crystallographic texture. See alsoCrystallographic information;Crystallographic texture measurement andanalysis; Texture.

anisotropic Young's modulus 358measurement and analysis " 357-364topographic methods for 368

Crystallographic texture measurement andanalysis. ;See also Crystallographictexture; Orientation distribution junction;Preferred orientation; Texture 357-364

applications 357,363-364Bragg's law 360



708/ Index

Crystallographic texture measurement andanalysis (continued)

descriptions of preferred orientation .. 358-361estimated time analysis 357introduction 358limitations 357, 362-363pole figure 360related techniques 357samples 357series method of ODF analysis 361-363texture measurements , 358

Crystallographysurface, LEED analysis 536surface, vocabulary of 537-538

Crystal orientation, as x-ray diffractionanalysis 325

Crystal-particle statistics, as XRPD source oferror 340

Crystal perfection, as x-ray diffractionanalysis 325

Crystals. See also Single crystals.analyzing, by x-ray spectrometry 87, 88axes, stereographic projection of. 359and boundary structure, compared 358classes of. 346-347defect intensities, measured by x-ray

topography .365diffraction of 346effect of cooling on analysis 352effect of thickness on topographic

methods 367-370effects of rotation 368EXAFS analysis of .407forces, Raman analyses lattice vibrations to

obtain , 130fracture surface of. 376-377growth , 365, 375-376ideal 351ideally imperfect. 351imperfections 332ionic, ESR studied 263as isotropic 358kinetics of 376local environment around transition ions,

characterized by ESR 253-266mosiac , 351near-perfect, diffraction in 365, 367next-nearest neighbors EXAFS

determined .407perfect 325, 351point-group symmetry of 346polar, LEISS identification of faces 603silicon, spin-dependent recombination

analysis of 258single 129, 256size of, as x-ray diffraction analysis 325structural information by EXAFS .407structure definition 348symmetry of 346systems 347

Crystal structureanalysis, assumptions of 352and boundary structure, compared 358calculating intensities from 349"cat" layer crystallized in monoclinic space

group P2 347,349defining 348determined 345of diamond and graphite 345, 355illustrated by Oak Ridge Thermal Ellipsoid

Program 352, 354initial guessing procedure 350of inorganic solids, applicable analytical

methods .4-6least squares refinement of atomic positions to

determine 351by neutron diffraction .420of organic solids, methods for analysis 9of two carbon forms 345

Crystal symmetry 346Crystal systems 347, 348Cubic unit cells 346-348Cupferron

as precipitant 169as solvent extractant. 170

Curie and Neel point measurements, byMossbauer spectroscopy 287

Curie point. See Curie temperature.Curie temperature 671,691Curing

mechanism, of polymide resin 285of polymers, ATR monitoring of. 120-121

Currentelectric, SI base unit and symbol for 685flowing, effect on electrolysis 197-198

Current densityconversion factors 686as electrolytic inclusion and phase

isolation 176SI derived unit and symbol for 685

Current-sampled polarography, as improvedvoItammetry 193

Current-voltage relationships, voltammetryand dc polarograms for 189, 190

Curvature, radius of, abbreviation for .....691Curve fitting, and factor analysis, IR

application to polymer blendsystem 117-1I8

Cuttingalignment of silicon boule for 342residual stress distributions from 392of samples 16

Cutting tool, AES thick films analysis of 561Cutting torches, for samples 16Cyanide ions, ion chromatographic analysis

of. 661Cyanides

as electrodes 185nickel titration using 174

Cyanogenabbreviation for 690emission molecule 25

Cycles per second, abbreviation for 690Cyclic voltammetry, fundamentals 192Cyclodextrin, defined 671Cylindrical internal reflection cell 1I8, 689Cylindrical mirror analyzers 554, 689Czerny-Turner monochromators 23, 38Czerny-Turner spectrometers, with Triplemate

device 129

DDaly collector, in gas mass

spectrometers 154-155Damping, Debye-Waller and mean-free-

path .410Dark-field illumination 690Dark-field images

of annealing twin in rutile 443band of precipitate particles .460iron-base superalloy 442nitrogen-implanted Ti alloy .485transmission electron

microscopy .441-446, 460Data bases

infrared spectra 1I6in single-crystal analysis 355-356x-ray energy 522-523

Data reductionoptions in stainless steels, x-ray spectrometry

for 100RDF analysis 396-398for silica glass 397

Dating of prehistoric materials, radioanalysisof. 243

Daughter ion scans, gas chromatography/massspectrometry 646

dc arc source, for optical emissionspectroscopy 25

dc intermittent non capacitive arc,defined 671

DCI, as synchrotron radiation source .413DCP. See Direct-current plasma.dc plasma excitation, defined 671de polarography. See Polarography.Dead-stop end-point titration. See

Biamperometric titration.Dead time

correcting, EDS dot mapping 528-529defined 519, 671practical effect of 519-520wavelength-dispersive spectrometer 520x-ray spectrometry 92

Deboronization, chemical surface studies .. .\77Debye-Scherrer

camera, for XRPD analysis 335diffracted x-rays, imaging polycrystalline

substructure by 374powder method, schematic 335

Debye-Waller damping, EXAFS analysis . .410Decarburization, chemical surface studies

of 177Decay

constant (X), defined 671kinetics of radical production and 265-266spin lattice relaxation time and 257

Deceleration, atomic number correction for 524Dechanneling, lattice strain measurement

by 634-635Decomposition

cellular, image analysis kineticanalysis 316-318

Freiberger 167potential 198,201of sample, in Raman analyses 130spinodal 583, 593

Deconvolution, based on multiplet splitting 573Dedicated SIMS instrument, for probe

imaging 613Deer hair, analysis of sulfur in 224De-excitation

atomic fluorescence spectrometry .46Auger electron .433, 550in neutron activation analysis 234processes, and molecular absorption,

Jablonsky diagram 73by x-ray photon emission .433

Defect analysis. See also Defects; Defects,analytical methods.


electron spin resonance for 254experimental parameters .464-465of inorganic solids, applicable analytical

methods .4-6by nulcear magnetic resonance 277one-dimensional .465-466by SAXS/SANS/SAS .402by scanning electron microscopy .490three-dimensional .466two-dimensional .466weak-beam microscopy .466-467

Defect centers, ESR detected 253Defect imaging 367-368, 370Defects. See also Defect analysis; Defects,

analytical methods.accumulations of, characterized by x-ray

topography 365buried distribution of 632centers of 253in crystalline solids, ESR detection of 253distribution depth profile, in single

crystal 51IFIM images, in pure metals 588-589



imaging of 367-368in imperfect crystals 365interfacial, imaged by x-ray

topography 365near-surface, in single crystals 633observable using optical microscopy 307point. 358, 556-559, 583, 588strain-induced, as fine structure

effect .438, 440Defects, analytical methods. See also Defect

analysis: Defects.analytical transmission electron

microscopy .429-489electron spin resonance 253-266field ion microscopy 583-602Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515x-ray powder diffraction 325-332x-ray topography 365-379

Deficiency cones, in divergent-beamtopographs 371

Deformationanalysis of .468-470cold, substructure due to .468-469crystallographic texture of 357-364and fracture behavior 365, 376-378hot, substructure due to .469-470plastic, effect on fringe patterns 368recovery, and recrystallization structure

analysis .468-470texture, due to mechanical processing, PST

for 374Degradation

of polymers, Raman analyses 131and structure 285-286

Delayed fluorescence, in molecularfluorescence spectroscopy 73

Delayed-neutron counting 238, 690Demagnetizing field 690Dendrites, SEM analysis .490Dendritic solidification structure, Ni-5Ce

alloy 307Denitriding, surface, chemical studies 177Densification, SAS techniques for .405Density

crystal defect, measured by x-raytopography 365

current. 685defined 671electric charge 685energy 685mass " 685optical, blackening as 143symbol for 692

Depletionchromium, in a weld zone 179rate, in calibration of gas mass

spectrometers 155Deposition

conditions for complete,electrogravimetric 198

of copper on platinum cathode, aselectrogravimetry example 198

effect of medium 198electrolytic, piezoelectric effect in 198and electrometric titration 203incomplete, use in electrogravimetry 198physical properties of deposits 198reversal 198

Depthvs composition, passive film on tin-nickel

substrate 608-609vs elements, semiquantitative PIXE analysis

for 102Depth analysis. See Depth profiles: Depth

profiling.Depth of field .497, 671Depth of penetration 113, 671

Depth profiles. See also Composition profiles:Depth profiling.

from ATR spectra 113Auger, antiwear films analysis 565-566Auger elemental 554compositional 304 stainless steel. 555compositional, AES 549of granular sample, using ATR, DRS, and

PAS 120of heavy-element impurities 632-633negative, LPCVD thin films 624organometallic silicate film 617phosphorus, for ion-implanted silicon

substrate 624RBS defect distribution, in single

crystals 628secondary ion mass

spectroscopy 617-620, 623-626of solid samples, infrared

spectroscopy 109, 115spark source mass spectrometry 142x-ray photoelectron spectroscopy 573-574

Depth profiling. See also Composition profiles:Depth profiles.

Auger electron spectroscopy 549-567electron probe x-ray microanalysis 516-535field ion microscopy 583-602granular sample using ATR, DRS, and

PAS 120low-energy ion-scattering

spectroscopy 603-609neutron diffraction .420-426particle-induced x-ray emission 102-108photoacoustic spectroscopy 115Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627

Derived SI units, guide for 685Design verification, semiconductors, SEM

for .490Desmearing, parameters for .403Desorption

of adsorbed layers, LEISS analysis of ....603images, gated 596, 600-601

Destructive interference, x-rayspectrometers 88

Detected area fraction, effects of varying iniron-carbon alloys 309

Detectionautomated, electrometric titration for .....202of combustion products in high-temperature

combustion 222-223electronics and interface, inductively coupled

plasma 39of ESR spectrometers 256-257feature, by image analysis 310fluorescence, EXAFS analysis .412infrared 223, 230minimum, electron spin resonance 259modes, ion chromatography 659-662of phase changes 282-283preferential, image analysis of AISI 416

stainless steel 311of radioactivity 245-246redox endpoint 164setting, effects on area fraction detected ..312spectrophotometric, with ion

chromatography 661surface-phase 293techniques, EXAFS analysis .418thermal-conductive 223, 229-230transmission mode, EXAFS analysis .412of x-rays 326XRPD methods of 331

Detection limitsAuger electron spectroscopy 556defined 671elemental, AEM-EDS .449

Index / 709

fluorescence analysis 76gas chromatography/mass spectrometry 645for ICP-AES analysis 33of minor elements in oil 101PIXE vs XRF analysis 106radioanalysis 246-247single-element interference free, for

TNAA 238thermal neutron activation analysis 237-238UVIVIS absorption spectroscopy 70varying 96

DetectorsAAS instruments as 55backscattered electron, contrast

with 502-504backscattered electron, ring geometry of ..503backscatter, effect on SEM .490charged particle 245-246early gas x-ray 83energy-dispersive spectroscopy, cross

section .435electron multiplier, x-ray photoelectron

spectroscopy 571electron probe x-ray microanalysis, resolution

(peak broadening), 519electro-optical, UVIVIS absorption

spectroscopy 67of energy-dispersive x-ray spectrometer 519flow proportional 521for gamma-rays 235gas-filled 88germanium, and x-ray spectrometry 83glowing-gas proportional 88and image formation, SEM

microscopes .493-494imaging, for retrofitting spark 145lithium-doped silicon 83, 519mercuric iodide 95molecular fluorescence spectroscopy 77multichannel. 128, 137photographic film 326photon 246, 326photoplate 143position-sensitive 326, 372,422preamplifier and amplifier, x-ray

spectrometers 91scintillation 88-89secondary electron .495, 554signal, analytical transmission electron

microscopy .434-436solid-state lithium-drifted silicon 89, 90specimen current 506vidicon and diode array, use in Raman

spectroscopy 129for x-ray spectrometry 88-91

Detergentsanalytic methods for. 9powder, as binding agents for samples 94

Determination, defined 671Determination of structure. See Structure

determinations.Deuterium lamp, for UVIVIS analysis 66Deuteron, defined 671Dewar flask, defined 671Df. See Dilution factor.Di-(2-ethylhexyl)phosphoric acid, as solvent

extractant. 169-170Diameter 198, 690, 692Diamond

and graphite, crystal structures of ...345, 355local structure of trace impurities, EXAFS

determined .407synthetic, EXAFS characterization of metal

impurities in .417thin Type II, for diamond-anvil cell 113

Diamond-anvil cell 113, 116Diaphragm, defined 671Dies, axisymmetric, for wires and rods 359Differential pulse polarography ..... 193, 194



710/ Index

Differential pulse stripping voltammetry,principles 193

Differential sputtering, as artifact in AESanalysis 556

Differential thermal analysis, for second-phase testing 177

Diffracted beams, intensities of 328-329Diffracted intensities, resolving of .424Diffraction. See also X-ray diffraction.

angle, diffraction x-ray beam at 381angle, symbol for 692coherent Bragg .436cones 327,371contrast. .444, 671convergent-beam electron .438-440crystal 346dynamical theory of 366-367electron .410, 436-440experiments, two types of single

crystal 330geometry of 326-327grating, defined 672intensities, in single-crystal x-ray

diffraction 348-349intensities, kinematic and dynamic effects

in 366-367kinematical theory of 366of light by line gratings 345line intensity 328of monochromatic x-ray beams at high

diffraction angle 381in near-perfect crystal 367pattern, to determine atom locations within

unit cells 345-346peaks, in surface stress measurement 385selected-area .436-438single-crystal, principles of 350single-crystal methods 329-331spots 345-346, 351, 366from surfaces, principles of 538-539techniques, recommended for ferrous and

nonferrous alloys 382vector 690wave theory of 83and x-ray topography 366-367

Diffraction angle, symbol for 692Diffraction cones 327, 371Diffraction contrast 444, 671Diffraction grating, defined 672Diffraction methods


extended x-ray absorption finestructure .407-419

neutron diffraction .420-426polycrystalline 331-332radial distribution function analysis 393-40Isingle-crystal. 329-331small-angle x-ray and neutron

scattering .402-406x-ray diffraction 325-332x-ray diffraction residual stress

techniques 380-392x-ray powder diffraction 333-343x-ray topography 365-379

Diffraction patternsdefined '" 345, 672GaAs, LEED analysis 541oriented pyrolytic graphite 543point-group symmetry from 346precession photographs showing three layers

of. 346for single crystals 345, 351from superlattice 540as three-dimensional. 346

Diffraction-peak locationmethods, compared 385-386x-ray diffraction residual stress

techniques 385-386

Diffraction spotsdiffraction patterns at 345-346identification, for single-crystal analysis ..351intensity variation within 366

Diffraction vector 690Diffractometers

0-0 337automated single-crystal. 351Bragg-Brentano 337conventional four-circle 351conventional x-ray powder diffraction 337double-crystal 371-372Eulerian cradle mounted on 360Guinier 337horizontal laboratory 389low-energy electron diffraction 540micro- 337-338neutron powder. .422Seeman-Bohlin 337thin film 337time-of-flight powder .422time-of-flight single-crystal, at pulsed neutron

source .424use in x-ray diffraction residual stress

techniques 387Diffuse reflectance spectroscopy 114, 120Diffuse transmittance, defined 672Diffusion

coefficients .478couples .477-478, 503current, voltammetry 190in electrogravimetry 198grain-boundary vs volume .478-induced grain-boundary migration, EDSI

CBED analysis of .461-464measurements 243, 476-478natural, in voltammetry '" .189of nickel into iron, radioanalytically

measured 243phenomena, XPS analysis 576-577of plutonium into thorium 249SIMS tracer studies 610studies, by Miissbauer spectroscopy 287surface, FIMIAP study of 583

Diffusion current 190Diffusion-induced grain-boundary migration

analysisabbreviation for 690in AI-4.7Cu .461-464convergent-beam electron diffraction. .462-464by EDSICBED .461-464EMPA dot map of 527x-ray microanalysis .462

Diffusion measurementsadvantages of AEM analysis .476data analysis .476-478diffusion coefficients .478diffusion couples .477-478radioanalytical tracer for 243sample preparation .476by SIMS profiles 610

Diffusion vacuum pumps, in gas massspectrometer 151-152

Digestion, as sample preparation .. 165-167, 176Digital compositional mapping

flexible processing 528relation of intensity to constituent 528-529of zinc-containing copper 528

Digital imagingand analog imaging, of iron in aluminum

matrix '" .448semiautomatic analyzer for 310

DIGM. See Diffusion-induced grain-boundarymigration.

Diketones, Il, as extractants 170Dilation/voiding, SAS techniques for .405Dilute systems, EXAFS fluorescence analysis

of. .418Dilution factor, defined 672

Dimer, defined 672Dimerization, defined 672Dimethylglyoxime

in amperometric titration 204complex, weighing as the, gravimetric

analysis 171as narrow-range precipitant 169

Dioctadecyldimethylammonium bromide,orientation of long-chain molecule ..... 119

Diode array detectors, use in Ramanspectroscopy 128-129

Diperoxydodecanedioic acid, ATR, DRS, andPAS granular analysis of 120

Diphenylcarbazide method, UV/vIS analysisfor chromium in beryllium by 68

Dipoledislocation, in ferrite .469moment, effect in solvent extraction 164strength of transition, molecular

vibrations 111Direct chemical separation, for UV/VIS

interferences 65Direct-current arc, defined 25Direct-current arc emission spectroscopy

and ICP-AES 31precision 25

Direct-current plasma atomic emissionspectrometry 21, 43

Direct-current plasma .40, 690Direct-current polarograms, current-voltage

curves as 189-190Direct-current polarography, circuit and cell

arrangement 189Direct-imaging ion microscopes, for SIMS

analysis 613, 614Direct injection burner, defined 672Direction

and magnitude of maximum residualstress 392

of reaction, symbol for 691Direct memory access, use in x-ray

spectrometry 92Direct method, to produce electron density

maps 351Direct potentiometry, ion-selective electrodes

and 204Direct-reader spectrometer, inductively

coupled plasma 37Direct sample insertion device 36, 690Discrimination, in sampling 16Dislocation cell structure analysis

by analytical electron microscopy ... .470-473computerized misorientation

determination .471-472limitations and conditions for orientation

determination .471misorientation determination for small

cells .472-473Dislocations

in bright-field images, polycrystallinealuminum .444

of cell structure, analysis of. .470-473cell structure, by cold rolling ETP

copper .469dipoles and loops, in ferrite .469effect of Burgers vector orientation on FIM

contrast from 588-589elastic displacement field associated with. .464in FIM samples 587glissile, fcc material. .465imaged by x-ray topography 365imaged in aluminum alloy .465imaging by topography 367-370loops, ATEM imaged .465partial, stacking-fault region between 589perfect, effect in FIM images 588point defects and 583study of alloy elements and impurities to ..583SAS techniques for .405



tangle of. 358, 467Disodium salt, of EDTA, use in

electrogravimetry 201Disordered materials, magnetic, exotic

effects 276Disordered structure, defined 672Disordered systems, EXAFS analysis .407Dispersion

device, x-ray spectrometers 89lineshape, and Lorentzian absorption

lineshape 280, 281Dispersive EXAFS detection technique .. .418Dispersive infrared spectroscopy,

instrumentation 111Dispersive spectrophotometers

dual-beam 67-68single-beam 67

Dissection techniques, general, capabilitiesof. " 380

Dissolutionanalytical methods requiring .4and electrometric titration 203and reprecipitation, as gravimetric sample

preparation 163sample, for classical wet analytical

chemistry 165-167of samples, flame AAS analysis of 56-57

Distillationefficiency measured 243separation by 169steam, in nitrogen determination 172-173

Ditallowdimethylammonium chloride,evaporated film, ATR spectrum of 119

Dithizone, as solvent extractant 170Divergent beam method, x-ray

topography 370-371DNC. See Delayed-neutron counting,Dodecanedioic acid, ATR, DRS, and PAS

granular analysis 120Dolomite

containing manganese, ESR studied 264dissolution in hydrochloric acid 165

DomainSEM observed in ferromagnetic materials 490structures, evaluated by x-ray

topography 365Donnan exclusion 662, 672Dopants

atoms of, lattice location of. 633low-level, GFAAS analysis of 58low-level, SIMS concentration profiles of 610

Doping method, XRPD analysis 340Doppler effect, defined 672Doppler line broadening 22Doppler shift, defined 672DORIS, as synchrotron radiation source .413Dosimeter, defined 672Dot mapping. See also Elemental mapping:

Mapping: X-ray maps.for aluminum, at aluminumlbrass interface of

aluminum wire connections 531-532for copper, at aluminumlbrass interface of

aluminum wire connections 531-532effect of brightness on sensitivity of ..526-527electron probe x-ray microanalysis ...525-527of iron/aluminum interface in aluminum wire

connections 531-532limitation of 527-528on photographic film 527for zinc, at aluminumlbrass interface in

aluminum wire connections 531-532of zinc, at grain boundaries 527

Double-beam spectrophotometers, UVIVISabsorption spectroscopy 67

Double containment, of NAA samples 236Double-crystal spectrometers, for polycrystal

rocking curve analysis 371-372Double-crystal spectrometry, as x-ray

topographical. 371-372

Double-deflection scanning electronmicroscopic system .493

Double nuorescence EXAFS detectiontechnique .418

Double-focusing mass spectrometers, in gasmass spectrometry 154

Double monochromators, stray light rejectionfor 129

Double-pass cylindrical mirror analyzer, forx-ray photoelectron spectroscopy 571

Double resonance method, as supplemental toelectron spin resonance 258

DPPH standard free radical, ESR spectrumof 259

Drawing of wire and rod, preferred orientationduring 359

Drawn polymer films, molecular orientationdetermined 120

Dredges, as sampling tools 16Drill cores, resource evaluations by neutron

activation analysis 233Drilling, as wet chemical technique for

subdividing solids 165Drills, as sampling tools 16Droplet sequence, flame emission

spectroscopy 29Dropping mercury electrode, for

polarography 189DRS. See Diffuse reflectance spectroscopy.Drugs, GC/MS analysis of volatile compounds

in 639Drying, of gravimetric samples 163Dry spike isotope dilution, for SSMS

analysis 146DSID. See Direct sample insertion device.d-spacings

formulas for 328use in unknown phase/particle

identification .455-456Dual-beam dispersive spectrophotometers,

UVIVIS absorption spectroscopy .....67-68Dual-phase steels, manganese segregation

in .483Dumas method, of elemental analysis for

nitrogen 214Duoplasmatron, defined 672Duplicate measurement, defined 672Duplicate sample, defined 672Dye-penetrant techniques, for optical

metallography specimens 302Dyes, analytic methods for 9Dynamical diffraction, in defect

imaging 367-370Dynamic range, fluorescence analysis 76Dynamic viscosity 685Dysonian shapes, in ESR spectra 261Dysprosium, TNAA detection limits 237

Ee. See Electrons.E. See Energy.E. See Modulus of elasticity.Earth elements

alkali, eluent suppression ion chromatographytechniques for. 660

alkaline, complexometric titrations for 164EBIC. See Electron beam induced current.ECAP. See Energy compensated atom probe.E eell • See Measured cell potential.Echelle grating spectrometer .40-41E eonst • See Constant cell potential.Edge. See also Absorption; K-edge.

absorption, defined 85effects, in image analysis of low-carbon sheet

steel. 316K-shell ionization, pre- and post-structures

in .450

Index / 711

shapes, characteristic EELS, for amorphouscarbon and carbon in metal carbide ... .460

EDL. See Electroless discharge lamp.EDM. See Electric discharge machining.EDS. See Energy-dispersive spectrometry.EDTA. See Ethylenediaminetetraacetic acid.EDTA titration, elements determined by 173Effective magnetization 690Effective mean potential, EXAFS analysis 409Efficiency

of combustion accelerators 222in separations, radioanalysis measurement

of. 243Effluent gas analysis, of residues 177Effluents

analytic methods ai.plicable 6, 7, 8, 11chromatographic, IR identification of. .... 109differential pulse polarogram in analysis

of. 195industrial water, x-ray spectrum 95inorganic, analytic methods 7, 8of liquid chromatographs, UVIVIS detection

of species in 60multielement fingerprinting and voltammetric

analysis 195organic gas, analytic methods for 11voltammetric monitoring of metals and

nonmetals in " 188Einzellens, in gas mass spectrometer .. 153, 155Elastic collisions, as energy-level diagrams 127Elastic constants 382, 387, 672Elastic displacement field, associated with

dislocations .464Elastic scattering .432-433, 672Elastic strain, effect on diffraction

patterns .438, 440ELDOR. See Electron-electron double

resonance.Electrical circuits, residential, EPMA failure

analysis 531Electrical contacts, XPS analysis of surface

films on 578-579Electrical ion detection method 144Electrical plasma atomizers, atomic absorption

spectrometry 53-54Electrical resistance metals, dislocation

structure in 358Electric charge

density 685SI derived unit and symbol for 685

Electric current, SI base unit and symbolfor 685

Electric dipole, defined 672Electric dipole moment, defined 672Electric dipole transition, defined 672Electric dipole transition moment, in IR

spectroscopy . . . . . . . . . . . . . . . . . . . . 111Electric discharge machining 690Electric field

as field corrosion 587oscillating, wave theory of 82and stress, in field ion microscopy 587

Electric field effect. See Stark effect.Electric field strength 685Electric nux density 685Electricity

conversion factors 686quantity of, SI derived unit and symbol

for 685Electric potential, SI derived unit and symbol

for 685Electric resistance, SI derived unit and symbol

for 685Electroanalytical probes, for process

control. 199Electrochemical analysis 181-211

capabilities, compared with classical wetanalytical chemistry 161

controlled-potential coulometry 202



712/ Index

Electrochemical analysis (continued)of inorganic anions and cations determined by

ion chromatography 663voltammetry and polarography 202

Electrochemical ion detector 661Electrochemical titration, electrometric

titration and, compared 202Electrochemistry

adapted for inorganic solids .4-6for inorganic liquids and solutions 7

Electrodeless discharge lamps, for AASspectrometers 50

Electrodepositionof interferences, UVIVIS absorption

spectroscopy 65-66solid metal 208

Electrode potential 197-198,672Electrodes. See also Ion-selective membrane

electrodes; Potentiometric membraneelectrodes.

boron tetrafluoride 184bromide 184calcium 184calcium/magnesium (water hardness) 184and cells, for electrogravimetry 199-200chloride 184copper 184cyanide 185for dc arc sources 25defined 672determining selectivity 182-183glass membrane 182glass, pH determination by 203iodide 185ion-selective membrane 181-183lead 185liquid membrane 182mercury vs carbon bases for 191nitrate 185perchlorate 185piezoelectric, cadmium analysis with 200platinum gauze 199-200polymer membrane 182potentiometric gas-sensing 183-185processes, reversible and irreversible 191reference 185, 186, 199,200reference, schematic of 186sample pretreatment 186silver, oxidation in alkaline

environments 135solid crystalline membrane 182for spark source mass spectrometry 145storage requirements 186sulfide 185supporting, defined 683surfaces, XPS elemental spectrum 578vibrating, effect in electrogravimetry 200

Electrogeneration, and electrometrictitration 202

Electrographic analysis, electrometric titrationand, compared 202

Electrogravimetry 197-201accuracy and precision 197applications 197, 201capabilities, compared with

voltammetry 188constant-current methods 198constant-voltage 199controlled-potential electrolysis 199and electrometric titration 203estimated analysis time 197, 200general uses 197high precision and automation 199instrumentation 199-200internal electrolysis 199, 200limitations 197microelectrogravimetry 200Nernst equation 197power supplies and circuit requirements 200

principles 197-198related techniques 197samples 197,200-201selection of method 198-199types of analysis 200-201

Electrojet thinning, as sample preparationtechnique for ATEM .451

Electroless discharge lamp 690Electrolysis

cell 199, 207-208cell, internal 199circuit for 199constant-current, separation and analysis of

metal ions by 200controlled-potential 199, 207, 208-210copper in copper-manganese alloy 201current, as function of time 210defined 672factors affecting in electrogravimetry 197-198Faraday's laws of. 203internal. 199, 200internal, copper determined by 200internal, separation of cadmium and lead

by 201nickel in sample containing chloride

ions 201preparation for coulometric titration 204in qualitative, classical wet methods 168as second-phase test method 177in voltammetry 189

Electrolytescomposition, as inclusion and phase isolation

technique 176defined 672effect in voltammetry 189supporting, current-voltage curve of .. 189-190supporting, in effluent samples 195traces, and conductance of water 203weak, dissociated 203

Electrolytically generated radical ions, ESRanalysis 265

Electrolytic conductivity, electrometric titrationand 203

Electrolytic etching, for image analysissamples 313

Electrolytic polishing. See alsoElectropolishing; Polishing.

specimens for optical metallographyanalysis 301

Electrolytic reversibility, bipotentiometrictitration and 204

Electromagnetic enhancement. See alsoEnhancement,

and SERS 136Electromagnetic field, molecular activity, in

Raman spectroscopy 127Electromagnetic lenses .432, 672Electromagnetic radiation

defined 672FMR resonant absorption of 267intensity of 83properties of 83spectrum, high-energy region 83in x-ray spectrometry 83

Electromagnetic theory and radiation 126-127Electromagnets, in gas mass spectrometers 154Electrometric titration 202-206

advantages 202amperometric 204applications 202, 205-206biamperometric 204bipotentiometric 204concentrations and reaction speeds in 202conductometric 203coulometric 204-205defined 672estimated analysis time 202Faraday's laws of electrolysis 203general uses 202

introduction 203limitations 202oscillometric (high-frequency) 203-204potentiometric 204related techniques 202samples 202, 205-206as volumetric analysis 202

Electromotive force, SI derived unit andsymbol for 685

Electron. See Electron beams; Electrondiffraction; Electrons; Secondary electrons.

Electron beam analysis. See also Electronbeam induced current; Electron probe x-raymicroanalysis; Microbeam analysis.

local surface study by 5I7Electron beam induced current

abbreviation for 690arrangement using Schottky barrier

technique 507as SEM special technique 507

Electron beams50-kV 326artifacts, as AES limitation 556diffracted, intensities of 328-329diffracted, two-dimensional angular

profile 542effect of differing energies .498energy distribution of signals generated

by .498factors controlling shape of. 331, 332interaction with specimens .432-434monochromatic, with single-crystal diffraction

methods 329-330monochromatizing 326polychromatic, with single crystal diffraction

methods 329as primary AES excitation 550scanning instruments .497-500spreading, in thin foils and bulk targets,

compared .434total, change in amplitude as function of

scattering angle 329volume of signals produced .498-500in x-ray spectrometry 82

Electron capture, and positron emission, asradioactive decay mode 245

Electron channeling. See also Channeling.capabilities 365contrast 505pattern, of vanadium taken in ECP

mode 504patterns and contrast 504-506

Electron configurations, for elements 688Electron density maps

determined 349by direct method 350, 351by heavy-atom method 350three-dimensional, of potassium benzyl

penicillin 350Electron detection, as EXAFS technique . .418Electron diffraction


defined 672and energy-dispersive spectrometry, unknown

phase identification by .455-459EXAFS analysis as mode of .410fine structure effects .438pattern, effect of tilt. .454patterns, indexing .456-457

Electron effect, final-state .408Electron-electron double resonance ..258, 690Electron energy analyzers, for x-ray

photoelectron spectroscopy 570-571Electron energy distribution

abbreviation for 690Auger electron spectroscopy 550, 551

Electron energy level diagrams. See Energylevel diagrams.



Electron energy loss spectroscopywith analytical electron microscope .432capabilities, and FIMIAP 583defined .449, 671light-element analysis .459-461limitations .450magnetic spectrometer and detector

for .435, 449qualitative analysis .450spectrum with zero-loss, low-loss, and

core-loss regions .449-450Electron energy loss, transmission electron

microscopy .432, 435Electron guns

for AES primary excitation 554analytical transmission electron

microscopy .432conventional tungsten hairpin filament .492field emission guns .432SEM microscope .491-492

Electronic device material studies, and crystalgrowth 375-376

Electronic energy levelsexcitation of 86in optical emission spectroscopy 21-22

Electronic materials, XRS analysis of 82Electronic mean free path, for inelastic

scattering, as function of energy 540Electronic nickel, analysis of aluminum in,

photometric method 65Electron images. See also Images; Imaging.

and x-ray area scans, microanalysis ofcomplex structures by 525

Electron-impact ionization, in gas massspectrometer 152-153

Electron microprobes, capabilities 102, 161Electron multiplier analyzer, for x-ray

photoelectron spectroscopy 571Electron multiplier phototube. See

Photomultiplier tube.Electron multipliers

in Auger spectrometer 554as ion detectors, gas mass spectroscopy 154

Electron nuclear double resonanceabbreviation for 690as supplemental ESR technique 258

Electron optical methodsanalytical transmission

electron microscopy .429-489electron probe x-ray microanalysis 516-535low-energy electron diffraction 536-545scanning electron microscopy .490-515

Electron opticsanalytical transmission electron

microscopy .432columns, SEM, TEM, and AEM analysis 432of electron probe microanalyzer 517

Electron or x-ray spectroscopic methodsAuger electron spectroscopy 549-567x-ray photoelectron spectroscopy 568-580

Electron paramagnetic resonance. SeeElectron spin resonance.

Electron probe microanalyzerelectron optics of 517history 517schematic, with associated circuitry 517

Electron probe x-ray microanalysis ..516-535applications 516, 530-535basic microanalytical concepts 517-518capabilities 102, 309, 429, 549, 610capabilities, compared with optical

metallography 299defined 672elemental mapping 525-529estimated analysis time 516flat, polished specimens for. 516general uses 516homogeneity requirement of 529of inorganic solids .4

introduction 517lateral and depth resolution 516limitations 516limits of detection 525measuring x-ray spectra 518-522nonapplicability of inhomogeneous samples

for 529of organic solids, information from 9physical bases of 518qualitative analysis 522-524quantitative analysis 524-525related techniques 516samples 516, 529-530sensitivity 516and secondary ion mass spectroscopy,

compared 516,517as spatially resolved analysis for micrometer-

sized volumes 529specificity of spectra 518standards, accuracy and precision

of. 524-525, 530strategy for applying microbeam

analysis 529-530Electrons

abbreviation for 690backscattered 669, 689behavior in gas mass spectrometer 152-153binding energy of 569conduction " " .261, 433-434configurations, elements 688deceleration, in EPMA quantitative

analyses 524defined 672detected by secondary electron detector 502diffraction, defined 672energy loss, signal detector for .435escape depth, AES analysis 551high-energy, and x-ray generation 83-84inelastic mean free path 569-571orbitals of, x-ray emission and 83photoejection of 85photoelectric rejection, in x-ray absorption .84pi, defined 679scattering, defined 672scattering volume of. .434secondary 86, 435, 681, 691sources, radial distribution function

analysis 395-396temperature of, as indication of electron

kinetic energy 24transitions, energy-level diagrams 569transmitted and scattered .434-435unpaired, ESR analysis for 253velocity of, abbreviation for 691

Electron scattering, defined 672Electron spectrometers, for AES analyses ..554Electron spectroscopy for chemical

analysis 568, 689Electron spin resonance. See also ESR

spectrometers; Resonancemethods 253-266

acoustic 258anisotropies " .261-262, 265applications " .253, 265-266capabilities 267double resonance 258electron-electron double resonance 258estimated analysis time 253general uses 253information gained using .4, 6, 9, 10, 262of inorganic solids .4, 6instrumentation 254-257introduction and principles 253-254limitations 253lineshapes . . . . . . . . . . . . . . . . . . . . . . . . . . .261NMR, IR, UVIVIS analysis methods and,

compared 265optical double magnetic resonance 258of organics 9, 10

Index / 713

Planck's constant 254related techniques,

compared 253, 257-258, 264-265and relaxation 257-258samples 253, 256, 262-266and saturation 257-258sensitivity 258-259spectra 259-261supplementary experimental

techniques 257-258typical data, summary on first transition

series 263Electron tunneling, rate in field ionization ..585Electron volt, abbreviation for 691Electrophoresis, and electrometric titration ..203Electroplating

baths, voltammetric monitoring of compoundsin '" '" .188

and chemical treatment baths, UVIVISanalyses of 60

solutions, controlled-potential coulometricassays of 207

Electropolishing. See also Electrolyticpolishing; Polishing.

for diffraction samples 382as FIM sample

preparation 584, 586, 598, 599of IN 939, for FIMIAP analysis 598of permanent magnet alloy sample 599for subsurface measurement 388

Electropolymerization, of phenols, SERS studyof. 136

Electrostatic analyzers 607, 690Electrostatic clinging, of sampling materials 16Electrothermal vaporization, for solid-sample

analysis 36Elemental analysis

14-MeV FNAA 239-abundance measurement by NAA 233analytical transmission electron

microscopy '" .429-489atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211Dumas method " .214EFG types 213-215electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis 516-535electron spin resonance 253-266elemental and functional group

analysis 212-220empirical formulas from 213field ion microscopy 583-602gas analysis by mass spectrometry 151-157and geometry, of particles produced by

explosive detonation 318-320inductively coupled plasma atomic emission

spectroscopy 31-42of inorganics .4-8ion chromatography 658-667liquid chromatography 649-657low-energy ion-scattering

spectroscopy 603-609micro-, of inorganic solids, methods for .. .4-6of mixture composition 213molecular fluorescence spectrometry 72-81neutron activation analysis 233-242nuclear magnetic resonance 277-286optical emission spectroscopy 21-30of organic compounds by EFG 213of organics 9, 10particle-induced x-ray emission 102-108of particles produced by explosive

detonation 318potentiometric membrane electrodes .. 181-187prompt gamma activation analysis ....239-240



714/lndex o

Elemental analysis (continued)Rutherford backscallering

spectrometry 628-636scanning electron microscopy .490-515Schoniger flask method 215secondary ion mass spectroscopy 610-627spark emission spectroscopy 25-26, 29spark source mass spectrometry 141-150of surfaces, by x-ray photoelectron

spectroscopy 568ultraviolet/visible absorption

spectroscopy 60-71voltammetry 188-196x-ray photoelectron spectroscopy 568-574x-ray spectrometry 82-101

Elemental and functional groupanalysis 212-220

applications 212, 214Dumas method 214elemental analysis 213-215estimated analysis time 212, 215functional group analysis 215-219general uses 212of inorganic liquids and solutions, information

from 7introduction 212-213Karl Fischer method for water

determination 219limitations 212, 214, 215, 217of organic liquids and solutions, information

from 10of organic solids, information from 9related techniques 212samples , 212, 213unsaturation (alkenes) 219

Elemental distribution maps. See Elementalmapping.

Elemental mapping. See also Dot mapping;Mapping; X-ray maps.

and analog mapping 525-528Auger, gold-nickel-copper metallization

system 559digital compositional. 528-529of high-temperature solder 532SEM image and 532-533spectrometer for 527spark source mass spectrometry 142

Elemental sensitivityLEISS analysis 605-606PIXE analysis 104-105

Elementsabsorption 84-85absorption edges 85analysis by x-ray spectrometry 82, 95-99characteristic emission as basis for x-ray

spectrometry 84vs depth, semiquantitative PIXE analysis

for 102detection by TNAA, optimization of 235heavy, depth profiles of surface impurities

of. 628, 632-633inert, implantation of .485-486interfering, separation in high-temperature

combustion 222light, analysis of .459-461, 516, 559-561location in superlattice planes, alloy IN

939 599low atomic number, x-ray spectrometry

of 86-87lower limit of detection 96mass absorption coefficients 85metallic and semimetallic, partitioning

oxidation states in 178nonmetallic, partitioning oxidation states

in , 178nuclear properties 278-279of transition series, identification by electron

spin resonance 253-266periodic table of the 688

polynuclidic, SSMS analysis 145removed from solution in neutral atomic

form 163single, atomic spatial distribution by lAP

analysis 596single, interference-free detection limits 238on solid surfaces, LEISS analysis of 603at surfaces, AES lineshapes for chemistry

of 552-553symbols for 688toxic, NAA analysis for. 233toxic, SSMS analysis of natural waters

for 141and x-rays, relationship in x-ray

spectrometry 84-85Ellipsometers, for chemical surface studies 177Elueut

as ionic aqueous solutions for ionchromatography 658

suppressed anion chromatography, sodiumbicarbonate and sodium carbonate as ...659

suppressed cation chromatography, nitric orhydrochloric acid solution as 660

-suppressed conductivity detection, ionchromatography 659-660

Embrittlementgrain-boundary, in refractory metals, lAP

studies 599mechanisms, in nickel alloys 561-563SIMS analysis for materials under 610

Emissionalpha-particle 244-245Auger 550beta-particle 245contrast, SEM 502de-excitation by .433defined 85-86, 673fluorescent yield 86-87gamma-ray, as radioactive decay mode 245K lines 86lines, defined 21, 673L lines , ..86maxima, molecular fluorescence

spectroscopy 75maximum depth of. 525M lines 86for photoejection of electrons in

copper. 85, 87photon 61positron, as radioactive decay mode 245profile, self-absorbed line 22secondary electron (low-energy) .433-434silver x-ray, spectrum 90spectra 21,22,75-76,673studies, remote, IR for. 115x-radiation, as basis of x-ray spectrometry ..82x-ray, in x-ray spectrometry 83-84

Emission sourcesarc 25excitation mechanisms for 24flame 28-29glow discharges 26-28ideal. 24-25for optical emission spectroscopy 24-29spark 25-26

Emission spectrometer. See alsoSpectrometers.

defined 673Emission spectroscopy. See also Inductively

coupled plasma atomic emissionspectroscopy.

defined 673infrared 115optical 21-30spectral interferences in 33

Emission spectrum, defined 673Empirical correction software, x-ray

spectrometry 100Empirical formulas, determination of. 213

Emulsion calibration curve, defined 673ENDOR. See Electron nuclear double

resonance.Endpoints

precipitation titrations 164titration, Eriochrome Black T 173-174

Energyabbreviation for 690absorption-edge, defined 85analyzer, LEISS analysis 607basis for electromagnetic radiation 83density, SI derived unit and, symbol for ..685electronic, excitation levels of 86impact, conversion factors 686kinetic, defined 675loss, Rutherford backscallering

spectrometry 630nonimpact, conversion factors 686principal Auger electron 551radiant, defined 680SI derived unit and symbol for 685specific, SI derived unit and symbol for ..685in UVIVIS absorption spectroscopy 61

Energy analyzers, LEISS analysis 607Energy-compensated atom probe

abbreviation for 690high-energy 597

Energy dependence, of electron mean freepath 571

Energy-dispersive spectrometers. See alsoSpectrometers.

basic components 519complete, diagram of. 519dead time 519-520detector resolution (peak broadening) 519efficiency 525sum peaks and escape peaks 520

Energy-dispersive spectrometry. See alsoX-ray spectrometry.

analysis of cartridge brass 530applications 100-10 1and CBED, diffusion-induced grain-boundary

migration analysis by .461-464of cement. 99-100continuous bremsstrahlung background,

effects of. 528dead time 516defined 673detection limits 522detector, cross section .435detector resolution 519dot mapping 525-529and electron diffraction, unknown phase

identification by .455-459of high-temperature solder 532instrument selection 522light-element analysis .459-461, 522peak broadening 519peak identification 522-523peak overlap problem 523, 530pulse processing, long time constant in ...527qualitative 522-523simultaneous multielement capabilities, effects

of. 92spectral resolution 521-522spectrometers for. 89-93and wavelength-dispersive spectrometry,

compared 521-522x-ray lines, 1-10 keV 523

Energy-dispersive x-ray detector, use withimage analysis 318

Energy-dispersive x-ray fluorescence. SeeEnergy-dispersive spectrometry;Spectrometers.

Energy-dispersive x-ray spectrometersanalyzer systems 91-92detectors 90-91, 519operation of. 92-93for x-ray spectrometry 89-93



Energy level diagramsof an atom 570electronic, copper 85, 87electron transitions 569lithium 22of molecular light-scattering processes 126schematic, for an atom .433solvent-relaxation effects 77transitions of atomic spectrometries 44of unpaired electron with two nuclear spins,

electron spin resonance 259Energy levels, electronic, in optical emission

spectroscopy 21-22Energy loss

electrons, signal detector for .435Rutherford backscatlering spectrometry 630

Energy shifts, measurement, for atomchemistry .552

Engineering materialsimplantation in .485stress tensors as function of depth, neutron

diffraction .420Enhancement

effects, interelement , 97electromagnetic, and SERS 136fluorescence, using organized mediums 79resolution, as IR method 1l6-1I7

Entropy, SI derived unit and symbol for. ...685Environmental health hazard, radiation

as '" 247Environmentally important substances

ICP-AES use for 31MFS analysis of carcinogenic polynuclear

aromatic compounds in 72monitoring sampling for 12NAA application to 233pollutants, GCIMS analysis of volatile

compounds in .. " 639radioanalysis of radioactive pollutants in ..243sampling of '" " .12-18UVIVIS trace analysis 60x-ray spectrometry for 82-101

Enzymesactivities, UVIVIS assay of. 70ESR study of 264techniques using, for determination of

glucose 79-80Ep ' See Proton energy.Epidemiology, PIXE analysis in 102Epidiascope, as input device for image

analyzers 310Epitaxial films, rocking curve

profiles " 375-376Epitaxial growth, evolution of crystal structure

in 536Epitaxy, defined 673Epithermal irradiation 234Epithermal neutron activation

analysis 239, 689Epithermal neutrons, defined 234EPMA. See Electron probe x-ray

microanalysis.Equality, symbols for 691-692Equi-inclination contours method, for phase

transformations and precipitationyields 376-377

Equilibria, basic chemical, and analyticalchemistry 161-165

Equilibria chemistrybasic 162-163complexometric titrations 164gravimetric 163ion exchange separation 164-165oxidation-reduction reactions 163-164solvent extraction 164

Equilibriumchemical, defined 163pH, described 163state, defined 163

verification, in phase diagramdetermination .475

Equivalent ionic conductance, conductivity asa function of. 659

Equivalent weight, defined 162Erbium, as SSMS internal standard 145Eriochrome Black T

endpoint, complexation titration 173as metallochromic indicator. 174

Errorsdefined 673operator, controlling for. 12random, in sampling '" 12sampling, sources and control of 12

ESA. See Electrostatic analyzer.ESCA. See Electron spectroscopy for chemical

analysis.Escape depth

Auger electron 551functional dependence on kinetic energy of

electrons 551Escape peaks 520, 673ESR. See Electron spin resonance.ESR spectrometers. See also Electron spin

resonance.detection 256-257magnet 255microwave powered 255-257modulation 255noise elimination 257sample cavity 256scan 255-256typical 254-257variable temperatures 257

Estersanalytic methods for. 9determined 218functional group analysis of 218

Estimation of population characteristics, insampling 13

Etchingargon ion 575chemical attack 301chemical, use in spark source mass

spectrometry 144effect on EPMA accuracy 524-525electrochemical attack 301electrolytic, for image analysis samples 313ion sputter 575by nital and picral, compared for martensite

structure 302nonapplicability for microbeam analysis 530specimens for optical metallography

analysis 301sputter, effect on AES analysis 556surface 575surface, in XPS samples 575techniques, for image analysis samples 313time, effect on measurement of ferrite grain

size 318vacuum cathodic 301

Ethyl alcohol 640Ethylene-butylene copolymer, as irradiation

container material. 236Ethylenediaminetetraacetic acid (EDTA)

detected by ion chromatography 661disodium salt of 201for removal of interferences, UVIVIS

analysis 65titrations 173

Ethyl tritluoracetate, XPS spectrum of carbonIs lines in 572

ETL, as synchrotron radiation source .413Euler angles

defined 673fiber development in 363use in polycrystalline grain

orientation 359-361Eulerian cradle, on diffractometer 360

Index / 715

Euler plotsdefined 361ghost peaks in 362-363ODF for copper tubing using 361and orientation distribution function ..360-361

Euler rotations, defining orientation 359Europium


Jones reductor for 176TNAA detection limits 238

Evaporationfields, for selected metals 587of solvents, as IR sample 112

Event, EXAFS analysis .410Ewald construction, and reciprocal lattice, and

LEED 539Ex. See X-ray energy.EXAFS. See Extended x-ray absorption fine

structure.Examples and applications. See Applications

and examples.Exchange narrowing, as ESR line-broadening

mechanism 255Exchange stiffness

determined 275as ferromagnetic resonance application 275FMR investigated 267, 268

Excitationatomic energy level diagram showing .... .433of conduction electrons leading to secondary

electron (low-energy) emission .433-434in de arc 25emission maxima, fluorescence lifetimes

and 75index, defined 673mechanisms, of emission sources 24of phonons, as inelastic scattering

process .434plasmon, as inelastic scattering process .. .434potential, defined 673primary AES mode of 550spark source, for elemental analysis of metal

or alloy 29spectra, qualitative MFS analysis 74-75thermal, in optical emission sources 24volume, defined 673x-ray tube and secondary-target, in x-ray

spectrometers 89Excited nuclear level, population in Miissbauer

spectroscopy 288Exotic effects, as ferromagnetic resonance

application 276Explosions

with sodium peroxide sinters and fusions .. 167and volatility, sample dissolution

treatments 166Explosive actuator, SIMS determined isotopes

of oxygen in 625-626Explosive detonation, geometric and elemental

analysis of particles produced by 318Exposure, defined 673Exposure index, defined 673Expoxies

analytic methods for 9as optical metallography cold-mounting

materials 300Extended solubility, of iron in

aluminum 294-295Extended x-ray absorption fine

structure .407-419apparatus .411-412applications .407, 417-418capabilities 393data analysis .412-415defined 673detection techniques .418estimated data analysis time .407estimated experimental scan time .407



716/ Index

Extended x-ray absorption fine structure(continued)

event .410fluorescence detection mode .412fluorescence enhancement technique for. . .411Fourier transform to .412-413general uses .407importance of multiple scattering .410introduction and fundamentals .408-411limitations .407multiple-scattering effects .410-411near-edge structure .415-416physical mechanism .409reflection, for subsurface study .418related techniques .407samples .407, 417-418scan, germanium in GeCl4 molecule .408scan, nickel. .408synchrotron radiation as x-ray source

for .411-412transmission detection mode .412typical data analysis .413-414unique features of .416-417and x-ray diffraction, compared .417

External beam proton milliprobe, samplesfor 102

Extinction distance 367Extraction

efficiency measured 243replicas, for sample preparation, ATEM

analysis .452solvent, classical wet chemical analyses 164

Extrusion of wires and rods, preferredorientation during 359

Eyepiece, defined 673

FF. See Fluorescence.F. See Faraday constant,Fabrication history, determined by optical

metallography 299Face-centered cubic crystals. See also Face-

centered cubic materials.copper, EXAFS analysis .410diffraction in 360dominant texture orientations of 359Euler angles for 361fibers in Euler angles in 363rolling textures in 363-364variance of Young's modulus with preferred

orientation 358Face-centered cubic materials. See also

Face-centered cubic crystals.and bee materials, Kurdjumov-Sachs

orientation relationship .439matrix, bright-field image and diffraction

pattern .440rolling textures in 363-364

Factor analysis 118Failure. See also Failure analysis.

measurement of residual stress associatedwith 380

overload, of AISI 4340 steel threadedrod 511-513

Failure analysisof aluminum wire connections 531-532fracture surface for. . . . . . . . . . . . . . . . . . . .304by optical metallography 299sampling protocol for 15-16semiconductors .490semiconductor, SEM for .490

False silicon peaks, in EDS spectra 520Families of x-ray lines, EPMA

analysis 522-524Faradaic currents, in pulse polarography ... 193Faraday constant

96 486 Clmol, abbreviation for 690

in electrometric titration 203Faraday cup

in gas mass spectrometers 154use in microbe am analysis 530

Faraday's lawcontrolled-potential coulometry 210of electrolysis 203

Far-infrared radiation, defined 673Fassel torches, for analytic ICP

systems 36-37Fast Fourier transform 117, 690Fast neutron activation analysis 239, 689Fast-passage effect. See Electron nuclear

double resonance.Fatigue

-caused failures, measurement of associatedresidual stress 380

crack, in clamp, fractographs of 305FEG. See Field emission guns.Feldspar

flame emission sources for 29sintering agent for 166

Fellgett's advantage 112, 129Fermentation, maintenance of constant

conditions in 202Ferric chloride, in graphites, Raman

analysis 133Ferrimagnetic materials, ESR identification of

magnetic states in 253Ferrite, grain size, effect of etch time on

measurement. 318Ferroalloys. See also Iron alloys.

sodium peroxide fusion 167Ferrochromium slags, partitioning oxidation

states in 178Ferromagnetic antiresonance

abbreviation for 690spectrometers for 271, 272

Ferromagnetic materialsESR identification of magnetic states in ...253order-disorder in 284-285relaxation parameters for 276SEM-observed grain boundaries in .490

Ferromagnetic nuclear resonance 281Ferromagnetic resonance 267-276

applications 267,271-276defined 673estimated analysis time 267general uses 267homogeneity and inhomogeneity 274introduction and theory 267-270limitations 267low-temperature, probe for 270microwave spectrometers 270-271related techniques 267resonance parameters of resonance field and

Iinewidth 267-268samples 267,268,271-276

Ferromagnetismdefined 673onset of. 257

Ferromagnets 253, 690Ferromanganese isolation, in manganese ...174Ferrosiliconlferroboron, analysis for

aluminum, by aluminon method 68Ferrous ion, for titration of oxidants 205FET. See Field effect transistor.FFT. See Fast Fourier transform.FlA. See Flow injection analysis.Fibers

II and 13 in rolled copper 363EFG composition analysis 212in Euler angles of rolled fcc materials 363lines, ODF along, as function of rolling

reduction 364in rolled fcc materials 363textures, in wire and rod 359

Field adsorption 588Field corrosion, FIM electric field as 587

Field-dial Hall effect device, in ESRspectrometers 255

Field effect transistorabbreviation for 690in energy-dispersive spectrometry 519effect in x-ray detectors 91preamplifier, EPMA analysis 519

Field emission guns .432, 690Field-emission microscopy, defined 673Field evaporation

in FIMIAP .584, 585-587in AM/PLAP analysis of semiconductor ..601importance 586-587potential energy diagram 587progressive, in the atom probe 591rate variation with temperature 594sequences, atom layers counted in 590

Field ionizationcritical distance 585defined 584, 673in field ion microscopy 585potential-energy diagram illustrating 586

Field ion micrograph, stereographic projectionof 585

Field ion microscopefeatures 584improved vacuum of 587magnification, resolution, and image

contrast 588modified, atom probe as 591working field 587-588

Field ion microscopy and atom probemicroanalysis 583-602

applications 583, 598-602estimated analysis time 583general uses 583limitations 583related techniques 583samples 583, 584-585, 598-602

Field ion microscopy 583-602and atom probe microanalysis 583-602defined 673disadvantage 585electric field and stress 587field evaporation 585-587field ionization 585image, absolute depth scale from 593image formation 584images of alloys and semiconductors .589-590images of defects in pure metals 588-589of IN 939 nickel-base superalloy 598magnification, resolution, and image

contrast 588principles 584quantitative analysis of images 590sample preparation 584-585sample tip, ball model of 585stable operating conditions for 587of ternary 3:5 semiconductor .481working range 587-588

Field measurement, and magnification, effecton inclusion volume fraction 314

Field modulation, use in ESR analysis 255Field sampling 16Film, photographic 334, 527Film readers, automated, XRPD analysis ..338Films. See also Film thickness measurement;

Passive films; Thick films; Thin films;Ultrathin films.

antiwear, AES characterized 566deposited, ATR spectroscopy of 113drawn polymer, molecular orientation

determined 120epitaxial, rocking curve profiles 375-376heterogeneous surface, AES analysis

of 566layer thickness, RBS analysis for 631-632organometallic silicate, depth profiles

for 617



organometallic silicate, on silicon substrate,positive SIMS spectra for 617

passive, LEISS analysis of depth vscomposition on tin-nickelsubstrate 608-609

surfaces, of electrical contacts in mercuryswitch, XPS analysis 578-579

thick, analysis of 561, 603thin, AES analysis of 557-561thin, characterization

of .. .452-453,536,559,583,603,631-632thin, FlMJAP study of local composition

variations 583thin, FlMJAP study of nucleation and growth

of. " 583thin oriented, LEED determined grain size

in 536thin, RBS compositional analysis 631-632thin, sample preparation for ATEM

analysis .452-453ultrathin, LEISS analysis 603vinyl, identification of polymer and plasticizer

materials in 123-124vinyl, polymer and plasticizer materials

identified in 123Film thickness measurements. See also Films;

Thickfilms; Thin films; Ultrathin films.Auger electron spectroscopy 549-567electron probe x-ray microanalysis 516-535optical metallography 299-308Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515x-ray spectrometry 82-101

Filter photometers, UVIVIS analysis 67Filters

for anodes, x-ray tubes 90colored, image analyzers 310composition 94defined 673detection limits 95ion-exchanged resin-impregnated 94for sampling 16, 94as sampling substrates, x-ray spectrometry 94

Filter sampling, applications 16, 94Filtration, in gravimetric analysis 163FIM. See Field ion microscopy.Final state, electronic .408, 569Fine structure effects

atomic order .438electron diffraction .438orientation relationships .438satellite spots .438strain-induced defects .438, 440

Fingerprintinghalf-wave potentials as 190multielement, and approximate quantification

in effluent samples 195multielement, of voltammetric study in

effluents 195for oil spill identification 72

Finishescommon gravimetric 171for extracts 179

Firebrick, flame emission sources for 29-30First-order Laue zone

abbreviation for 690in electron diffraction .439, 442

Fissionprocess, neutron production .421spontaneous, as neutron source for NAA ..234thermal-neutron, of uranium 238

Flame atomic absorption spectrometryanalytical sensitivities of .47flame AES and flame AFS, compared .45and GFAAS, compared 58parameters, for alloying elements in steels ..56

Flame atomic emission spectrometry, flameAES and flame AAS, compared .45

Flame atomic fluorescence spectrometry,flame AES and flame AAS, compared .. .45

Flame atomization .48Flame atomizers

atomic absorption spectrometry .44-49modification or salting 54technology of 53

Flame emission spectroscopy 28-29, 72droplet sequence 29ionization interferences 34

Flame sourcesapplications 29-30burner selection for 28as emission source for optical emission

spectroscopy 28-29Flame tests, as qualitative wet analyses 168Flash, FlM sample rupture as 587Flashback, in premix burners 28Flask method, Schtiniger, for common

elements 215Flavor components, IR determination of 109Flight tube, for atom probe microanalysis ..591Flow cell systems, absorbance-subtraction

studies of 116Flowing-gas proportional detectors, for x-ray

spectrometers 88Flow injection analysis 55, 690Flow lines, in wrought products, as optical

metallography structural parameter 302-303Flow proportional detector, wavelength-

dispersive spectrometer 520Flow rate, conversion factors 686Fluoboric acid, as dissolution medium 165Fluorescence

abbreviation for 690in absorption/enhancement effects 97analysis, selectivity 76background, as problem in Raman

analyses 130correction 524crystallophosphor host matrices and metals

determined by inducing 74defined 673delayed, in molecular fluorescence

spectroscopy 73effect in AEM-EDS microanalysis .448effect in microbeam analysis 530enhancement, using organized mediums, as

MFS special technique 79in glow discharge emissions 29in the infrared 115intensity, as measure of absorption

probability, EXAFS analysis .411lifetimes 75,79mechanism, EPMA analysis 524molecular, of organic compounds and atoms,

and inorganic atoms 73-74oxygen quenching of, enzymatic

determination of glucose using 79-80quantum yields, structural effects 74spectrum, liquid-chromatographic fraction,

automobile exhaust extract 79and x-ray absorption, effect in

microanalysis .448Fluorescence correction, in EPMA

analysis 524Fluorescence EXAFS detection

technique .418Fluorescence lifetimes (dynamic

measurements), as MFS specialtechnique 79

Fluorescent metals, minimum detectablequantities for 74

Fluorescent molecules, in molecularfluorescence spectroscopy 73-74

Fluorescent yield 86-87Fluorides

anions, separation by ion chromatography 659gravimetric weighing as 171

Index /717

titration, thorium solution 173Fluorimetry. See Fluorometric analysis.Fluorine

determined in borosilicate glass 179distillation 169species weighed in gravimetry 172TNAA assayed 235-236volumetric procedures for 175

Fluorocarbons, oil of, IR split mull 113Fluorometers, single-beam 76Fluorometric analysis, defined 673Fluorspar, dissolution in hydrochloric acid.. 165Fluosilicic acid, distillation 169Fluxes

acidic 167density, heat 685fusion of sample materials with 93-94, 167luminous, SI derived unit and symbol for 685magnetic, SI derived unit and symbol for 685properties, compared 167

FM. See Ferromagnets,FMAR. See Ferromagnetic antiresonance.FMR. See Ferromagnetic resonance.FNAA. See Fast neutron activation analysis.FNR. See Ferromagnetic nuclear resonance.Foams, analytic methods for 9Focusing

automated 310diffractometer, for x-ray diffraction residual

stress techniques 387effect, extended x-ray absorption fine

structure .411Fogging 143, 144Foil

electrojet thinning for samples of .451platelet geometry in .455thin, AEM-EDS quantitative analysis of . .447thin, electron beam spreading in .434

FOLZ. See First-order Laue zone.Food products. See also Agricultural materials.

and natural products, liquid chrmoatographyanalysis for high molecular weightsugars 649

potentiometric membrane electrode analysisof. 181

voltammetric monitoring of pollutant metalsand nonmetals in 188

Forbidden (diagram) lines, x-radiation 86Force

conversion factors 686fields, atomic, use in IR normal-coordinate

analysis 110-111moment of, SI derived unit and symbol

for 685per unit length, conversion factors 686SI derived unit and symbol for 685

Forensic studiesNAA analysis for 233PIXE analysis for. 102by x-ray spectrometry 82

Formation constants, as voltammetricinformation 193

Formatting, automated 310Form factor, defined 329Formula weight, single-crystal x-ray diffraction

determined 344Fossil fuels. See also Fuels.

assay for toxic elements, neutron activationanalysis for 233

Fourier self-deconvolution, as method ofresolution enhancement 116-117

Fourier transformin analysis of iron and nickel. .416-417data, multiple scattering effects in .410of diffraction-peak profile 386in EXAFS data analysis .412-413to r space .412-413

Fourier transform infrared spectroscopyadvantages 112



718/lndex

Fourier transform infrared spectroscopy(continued)

capabilities 277and chromatographic techniques 115-116as computerized IR 109defined 673infrared spectrum of glass 122of inorganic gases, information from 8of inorganic liquids and solutions, information

from 7of inorganic solids .4-6interferometers 111-112of organic gases, information from 11of organic liquids and solutions, information

from 10of organic solids, information from 9and photoacoustic spectroscopy,

compared 115for polymer curing reactions 120and Raman spectroscopy 126of silicon 123spectrometer, optical diagram 112

Fourier transform spectrometers ..39-40, 690Fractionation, in gas mass spectroscopy 152Fractographs, fatigue cracks in clamp 305Fracture

behavior, and deformation 365, 376-378brittle, of FIM samples 587ductile, in overload region 513during analysis, pulsed-laser atom probe to

overcome , 597growth direction 512intergranular, final gray area of flaw 512and scraping, of XPS samples 575shear, of Kovar-glass seals, XPS

analysis 577-578strength, average, vs firing atmosphere 577toughness, conversion factors 686transverse, of 1075 steel railroad rail 304

Fracture analysis or mechanismAuger electron spectroscopy 549-567scanning electron microscopy 549-567x-ray topography 365-379

Fracture surfaceair-fired, XPS survey of 577line scan across .497nitrogen-fired, XPS survey 577oxygen-fired, XPS survey 577SEM analysis 490, 497showing failure origin 304stress corrosion crack 562-564

Fracture toughness, conversion factors 686Fragment ions, defined 153Frank-Condon principle, defined 673Franke method, for free lime content 179Frank-Read source, in transmission

topography 370Free lime, classical wet chemical analysis in

Portland cement 179Free radicals

content, of fossil fuel 253defined 673electron spin resonance 253-266intermediates , 263kinetic reactions of inorganic and

organic 253reaction kinetics in formation and decay

of. 266reactions, of catalyst surfaces 253stable hydrazyl 265standard, DPPH, ESR spectrum of 259

Freeze-pump-thaw technique, for ESRstudies 263

Freiberger decomposition, for specific sampledissolution 167

Frequencydefined 110,673group, molecular vibration as 111infrared 111

or Poisson's ratio, symbol for 692power reflected from microwave-resonance

cavity as function of 256SI derived unit and symbol for 685

Friction, adhesion theory and AES analysisof. 566

Friedel's law, and determination of ODFcoefficient. 362

Fringeseffects of crystal thickness 368fault-causing 369-370moire, observed by x-ray

interferometry 371origin as interferences in x-ray

diffraction 368Pendellosung 368

Fritted disk nebulizers 36, 55Fr-IR. See Fourier transform infrared

spectroscopy.FrS. See Fourier transform spectrometers.Fuels

EFG composition analysis 212fossil, assay for toxic elements 233nuclear 207

Full-tensor determination, plane-elasticmodel 384

Full width at half maximum 519, 674, 690Fume hood, for safety in acid dissolution

treatments 166Fuming, in perchloric acid 166Functional group

defined 674effect in ion exchange separation 164-165molecular, IR determination of 109UVIVIS identification in organic

molecules 60Functional group analysis

acids 215-216alcohols 216-217aldehydes and ketones 217amines 217-218aromatic hydrocarbons 218characterization of unknowns 215composition of a mixture , ..215esters 218peroxides 218phenols 219-220purity determination 215types of 215-219

Function control, semiconductor, SEManalysis for .490

Fundamental parameter software, x-rayspectrometer calibration 98

Furnace atomizers, atomic absorptionspectrometry .49

Furnace emission spectroscopy capabilities,molecular fluorescence spectroscopycompared 72

Furnaceshigh-temperature, use in combustion ..221-225muffle or gas burners, for sinters and

fusions 166simplified impulse, for IGF analysis 228simplified inductive, for IGF analysis ., ..228for single-crystal neutron diffraction ..... .424

Fusionfluxes for 167glass-forming 94low-temperature 94as sample preparation technique 93-94sodium peroxide 166-167solid sample digestion by 166-167

Fuwa tube, for flame atomizers .48FWHM. See Full width at half maximum.

Gg. See Diffraction vector.

Gadolinium, prompt gamma activation analysisof. 240

Galactose, in serum, indirect iodometry todetermine 205

Galliumepithermal neutron activation analysis 239evaporation fields for 587species weighed in gravimetry 172TNAA detection limits 237

Gallium arsenideFIM sample preparation of 586in thin-film semiconductors, FIMIPLAP

analysis 601-602Gallium oxide, in binary phosphate glasses .131Galvanic cell, short-circuited, for internal

electrolysis 199Gamma rays

defined 674detector for 235emission, as radioactive decay mode 245emission, in neutron activation analysis 234polarization, Mossbauer

spectroscopy 288, 295Gamma ray spectroscopy, defined 674Gamma ray spectrum

changes as function of time 236high-purity nickel, neutron activation

analysis 240of iridium by radiochemical neutron activation

analysis 241of irradiated ore 235

Gandolfi camera, for XRPD analysis 335Garnets, bulk composition of. 628Gas analysis

gas chromatography/massspectrometry 639-648

mass spectrometry 151-157Raman spectroscopy 126

Gas analysis by mass spectrometry 151-157applications 151, 156-157double-focusing mass spectrometer. 154estimated analysis time 151gas mass spectrometry 151-157ion quadrupole mass filter 153-154of inorganics 7, 8limitations 151of mixtures 151of organics 10, 11related techniques 151results of analysis 155-156sampling 151-152scanning modes 154spectrometer components 151-155

Gas burners, for sinters and fusions 166Gas cells, IR sampling 113Gas chromatography. See also Gas

chromatography/mass spectrometry.defined 674and gas analysis by mass spectrometry,

compared 151of volatile metal-organic complexes, as

separation tool 170Gas chromatography-infrared

spectroscopy 115Gas chromatography/mass

spectrometry 639-648applications 639, 647-648capabilities 212,277,649complementary techniques 645-647estimated analysis time 639and FT-IR techniques 115and gas analysis by mass spectrometry,

compared 151general uses 639of inorganic gases 8of inorganic liquids and solutions 7interpreting mass spectrum 641-642introduction 640limitations 639



methodology 643-645of organic gases Ilof organic liquids and solutions 10of organic solids 9principles, gas chromatography 640-641principles, mass spectrometry 640pyrolysis 647-648related techniques 639, 645-647samples 639, 644-645for tallow-base lubricant coatings 177

Gas constant, defined 674Gases. See also Gases, characterization of.

acid, as gas samples 152analytic methods adapted for 8carbon dioxide and sulfur dioxide, use in

high-temperature combustion 221-225characterized 1filters used with 94image, low ionization, for field ion

microscopy 587inclusions in glasses, Raman analysis 131inert, for FIM operations 587infrared absorbances by, PAS analysis

of. Il5infrared analysis of 113, Il5inorganic, analytic methods for 8ionization potentials and imaging fields for

selected 586molecules, three-dimensional structure of 393natural, analytic methods for. Ilorganic, analytic methods for Ilpotentiometric gas-sensing electrodes

for '" 183-185processes of, analytic methods for 8, IIRDF determination of interatomic distance

distributions and coordination numbersof 393

removal, and chemical equilibrium 163samples of 16thermal conductivity of 223, 230x-ray detector for, early 83

Gases, characterization of. See also Gases.extended x-ray absorption fine

structure .407-419gas analysis by mass spectrometry 151-157gas chromatography/mass

spectrometry '" 639-648infrared spectroscopy 109-125molecular fluorescence spectrometry 72-81Raman spectroscopy 126-138ultraviolet/visible absorption

spectroscopy 60-71Gas-filled detectors, for x-ray spectroscopy ..88Gas kinetic temperature 24Gas mass spectrometer

analysis, summary of. 155capability 156double-focusing 154instrument set-up and calibration 155introduction system 151-152ion detection " 154-155ion source 152-153mass analyzer 153-154output, computerized 155resolution of 155schematic 153Y and Z lenses 153

Gas mass spectrometrydefined 674gas chromatography and 639-648

Gas/metal environments, SERS studiesin 136, 137

Gas-phase corrosion, Raman analysis 135Gas tungsten arc welding, weld soundness

analysis of .478-481Gated desorption images, lAP analysis

for 596, 600-601Gaussian absorption curve, ESR

spectrum 259

GCIMS. See Gas chromatography/massspectrometry.

Gel-permeation chromatography. SeeSize-exclusion chromatography.

General dissection techniques, capabilitiesof. 380

Generators, radio-frequency, for ICPsystems 37

Genzel interferometer, in FI'-IRspectroscopy Il2

Geochemical research 82, 233Geological materials. See also Geologic

samples, characterization of.brine, ion chromatography of 665crystallographic texture measurement and

analysis 357-364ICP-AES use in 31NAA application in 234OES analysis of 21powder, PIXE analysis 102SIMS phase distribution analysis in 610

Geologic samples, characterization of. Seealso Geological materials.


atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-2Ilelectrochemical analysis 181-2Ilelectrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis 516-535electron spin resonance 253-256extended x-ray absorption fine

structure. . . . . . . . . . . . . . . . . . . . . . .407-419inductively coupled plasma atomic emission

spectroscopy 31-42infrared spectroscopy 109-125ion chromatography 658-667low-energy ion-scattering

spectroscopy 603-609molecular fluorescence spectrometry 72-81Mossbauer spectroscopy 287-295neutron activation analysis 233-242neutron diffraction .420-426optical emission spectroscopy 21-30particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187radial distribution function analysis 393-401radioanalysis 243-250Raman spectroscopy 126-138scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627single-crystal x-ray diffraction 344-356spark source mass spectrometry 141-150ultraviolet/visible absorption

spectroscopy . . . . . . . . . . . . . . . . . . 60-71voltammetry 188-196x-ray diffraction 325-332x-ray powder diffraction 333-343x-ray spectrometry 82-101

Geometryof applied field and magnetization, FMR

analyses 269of Bragg-Brentano diffractometer 337of chemisorbed atoms or molecules, EXAFS

determined .407factors, in microbe am analysis 529of lattices 327-328of microdiffractometer 338of particles produced by explosive

detonation 318-320platelet, in foil .455of powder diffraction 331sample, effect on X-ray diffraction residual

techniques 387of Seeman-Bohlin diffraction

arrangement 337

Index /719

of single-angle x-ray diffraction residual stressmeasurement. 384

of unit cells and diffraction 326-327variable wavelength, RDF analysis 396

Geometry, coordination. See Coordinationgeometry.

Germaniumas common analyzing crystal, in x-ray

spectrometry 88intrinsic, gamma-ray detector 235as internal reflection element. 113quartz tube atomizers with .49semiconductors, ESR studied 263

Gettering processes, monitored by x-raytopography 376

GFAAS. See Graphite furnace atomicabsorption spectrometry.

g-factorin ESR analysis 254as independent of temperature 257variation in 262-263

Ghost peaks, in Euler plots 362Glancing-angle camera, XRPD analysis 336Glancing-angle x-ray diffraction, capabilities

compared with LEED 536Glasses. See also Ceramics; Glasses,

characterization of.analytic methods applicable 5ASzTe" K-edge EXAFS spectra of arsenic

in .4Ilbinary phosphate, influence of cations on

bonding in 131bond distance, coordination, and neighbors

EXAFS determined .407borosilicate, Band F determined in 179calcium-boroaluminosilicate, SIMS depth

profiles 624characterized 1ground, AAS analysis for silver, lead, and

cadmium in 55hydrofluoric acid as dissolution medium

for 165hydroxyl and boron content, quantitative

analysis 121-122inclusions that contain gases, Raman

analysis 131K-edge EXAFS spectra of arsenic in .4IlKnight shift measurements on metallic 284and Kovar seals, XPS analysis 577-578metallic, NMR Knight shift measurement

on 284metallic, SAS applications .405metal oxide, Raman spectroscopy 130-131MOLE technique for 131multicomponent, EDS and WDS x-ray spectra

of. 521phase separation analysis by SAXS/SANS/

SAS .402Raman spectroscopy for 126, 130, 131SAXS/SANS analysis of .405silica, RDF analysis 397-399silicate, bonding topologies in 393SiOz Raman analysis 131small-angle scattering analysis .405spin, abbreviation for. 691surface layer analysis in 610, 624typical FI'-IR spectrum 122variation of long-range order, as function of

preparation 393Glasses, characterization of. See also Glasses.


atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrochemical analysis 181-2Ilelectrogravimetry 197-201electrometric titration 202-206



720/ Index

Glasses, characterization of (continued)electron probe x-ray microanalysis ...516-535extended x-ray absorption fine



spectroscopy 603-609neutron activation analysis 233-242neutron diffraction .420-426optical emission spectroscopy 21-30particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187radial distribution function analysis 393-401Raman spectroscopy 126-138Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627small-angle x-ray and neutron


spectroscopy 60-71voltammetry 188-196x-ray photoelectron spectroscopy 568-580x-ray spectrometry 82-101

Glass fiber filters, for sample preparation 94Glass membrane electrodes 182Glass microballoons, ion chromatography

of 665-667Glassware, cleanliness for UVIVIS analysis ..69Global illumination, MOLE/Raman

analysis 129-130Glow discharges 26-29, 142Glucose, enzymatic determination using oxygen

of fluorescence 79GMS. See Gas analysis by mass spectrometry.Gold

-copper alloys, EPMA analysis 530determined by controlled-potential

coulometry 209-211field evaporation in 586, 587gravimetric finishes 171high-purity, SSMS analysis 144ICP-determined in silver scrap metal .41L-family x-ray lines 522-nickel-copper metallization systems, Auger

elemental mapping 559nitriclhydrochloric acids as dissolution

medium 166particles, line scan across .496as SERS metal 136TNAA detection limits 237

Gold-plated stainless steel lead frame, Augermicroprobe of. 560

Goniometersand analyzing crystals 88defined 674use for Raman analysis 129in wavelength-dispersive x-ray

spectrometers 89in x-ray spectrometers 87

Gradient elution, defined 674Grain

average dislocation density 358in cast ingot, sketch 304individual, SEM analyzed .490interaction stresses .420, 424internal structure 357morphology, topographic methods for 368orientation specifying 359shape, determination by image analysis 309structures and dimensions, optical

metallography for 299Grain boundaries

in AI-4.7Cu alloy .462

by channeling contrast 505chemistry, AES analysis 549, 561-562compositions, nickel alloys 562contrasts, FIM image of 589diffusion-induced, migration analysis by

EDSICBED .461-464digital compositional map of 528dot map for zinc at. 527embrittlement in refractory metals, lAP

studies 599-600field evaporation and 587FIMIAP study of point defects in 583FIM image showing gated desorption in

molybdenum 600and interfaces by fracture, AES analysis

of. 549migration, diffusion-induced .461-464in molybdenum, atom probe

analysis 600, 601precipitate along 307-308precipitation and solute segregation, AES

analyzed 549quantitative determination by image

analysis 309segregation, analysis of. .. .481-484, 544, 549SEM-observed .490in U-700 nickel-base alloy 308yttrium segregation at .483

Grain-boundary area per unit volume, imageanalysis determined 309

Grain-boundary segregation analysisby analytical electron microscopy .481-484applications .483broad segregant distributions .482narrow interfaces .482-483

Grain sizecoarse, effect in surface stress

measurement. 387determination by image analysis 309, 313,

318effect of prior cold work on

recrystallized 308electron probe x-ray microanalysis

for 516-535ferrite, influence of etch time on

measurement of 318LEED analysis in thin oriented films 536mean linear intercept measure of 358measurements, sample preparation 313scanning electron microscopy .490-515of silver film grown on mica 543-544

Gram-atom, equivalence 162Gram-equivalent weight, defined 674Gram-molecular weight, defined 674Granular materials, thieves as sampling tool

for ; 16Graphite crucibles, IGF analysis 227Graphite furnace atomic absorption

spectrometryanalytical sensitivities .47applications 55atomizers as air filters 58and flame AAS, compared .49, 58sample preparation 55spectrometers 50-51of trace metals in hydrogen peroxide 57-58

Graphite furnace atomizers .48, 49, 53Graphites

activated charcoal. 132determined in steel or iron 178and diamond, crystal structures of 345, 355diffraction patterns from oriented

pyrolytic 543highly oriented pyrolytic 132intercalated 132powdered, effect in de arc sources 25quantitative effect of carbon KVV

Iineshapes 553Raman analyses of 126, 132-133

single-crystalline 132SSMS analysis 144stress-annealed pyrolytic 132structural integrity of 133vitreous carbon 132wettability of 543

Graphitic carbonsdetermined by selective combustion ..223-224determined in steel or iron 178oxidized in resistance furnace 224surface, XPS analysis of 568

Gratingsdiffraction 23holographic 128line, diffraction of light by 345monochromators, as wavelength sorting

devices 23polychromators 23, 37in Raman spectrometer 128use to determine atom location in unit

cells 345Gravimetric analysis. See Gravimetry.Gravimetric finishes, common 171Gravimetry

common finishes 171of compounds 171described 162goal of 163of moisture and water 171species weighed in 171-172vs volumetric analysis 171-172weighing as the chloride 171weighing as the chromate 171weighing as the dimethylglyoxime

complex 171weighing as the metal. 170-171weighing as the oxide 170weighing as the phosphate or

pyrophosphate 171weighing as the sulfate 171weighing as the sulfide 171

Grayabbreviation for 691-levels .310-level thresholding 309scale 526, 528as SI derived unit, symbol for. 685

Grazing angle electron incidence, effect onsample charging 556

Greek alphabet 692Green, bromcresol, acid-base indicator 172Grim glow discharge emission sources 27Grinding

effect on surfaces, Mossbaueranalysis of 287fine, for samples 16local variations in residual stress produced by

surface 390-391to powder, of XPS samples 575Raman analysis of 133as sample preparation, x-ray spectrometry ..94of soft materials, for samples 16specimens for optical metallography ..300-301

Gross sample, defined 674Ground water, SSMS toxicity analysis

of 148-149Group frequencies, molecular vibrations

as 111Group theory, prediction for graphite surface

analysis 132Growth

epitaxial, evolution of crystal structure in 536kinetics, LEED analysis 536thermally activated, effect on isothermal

phase transformations 317Guard-frame procedure, image analysis 315Guinier camera 335-336Guinier diffractometer, for XRPD analysis 337Guinier-Preston zones .405, 589-590Gypsum, determining calcium content in ... 173



Gyromagnetic ratio, symbol for 692

Hh. See Planck's constant.Ha• See Applied magnetic field.Habit plane

HN, stereographic projection .455and orientation relationships .453-455

Hafniumevaporation fields for .587organic precipitant for 169species weighed in gravimetry 172

Hairfollicles, deer, high-temperature combustion

analysis of sulfur content in 224single, IR spectroscopy 113

Half cells .164-165Half-life

defined 244, 674of radioisotopes 235in UVNIS analysis 62

Half-wave potential 190Halides '" 181,658Hall effect, defined 674Halogens 162, 224, 664Hamiltonian parameters

anisotropies of 262in ESR analysis '" 256-257

Hanging mercury drop electrode 191, 690Hankel function, EXAFS analysis .410Hanning window, in EXAFS data

analysis .413, 414Hardness

determined by residual stress techniques ..380determined in thin layered

steels 380, 389-390distributions and subsurface residual stress,

steel shaft 389-390and subsurface residual stress

distributions 389Hard x-rays, defined 83Harmonic-oscillator approximation, IR

normal-coordinate analysis 110-111Harmonics. See Spherical harmonics.HB. See Brinell hardness.HCL. See Hollow cathode lamp.Hd • See Demagnetizing field.Health hazards, radiation as 247Health studies, NAA application in 234Heat

content, conversion factors 686input, conversion factors 686quantity of, SI derived unit and symbol

for 685Heat capacity 685Heat flux density 685Heat treatments

of alloy steels, atom probe compositionprofiles for 594

history by optical metallography 299Heavy-atom method, to produce electron

density maps 350-351Heavy elements, depth profiles of

impurities 628, 632-633Helium

gas mass analysis of 155as image gas, field ion microscopy ..585, 600implantation .485ionization potentials and imaging fields

for 586in weld relay, gas mass spectroscopy of .. 156

Helium-neon laserscontinuous-wave 128in Ff-IR spectroscopy 112

Hemispherical analyzers, for AESanalysis 554

Hemoglobin, ESR study of. 264

Herbage, voltammetric monitoring of metalsand nonmetals in 188

Herbicide residues detected in plant andanimal tissue 188

Hermann-Mauguin space group, in EXAFSapplication .417

Hermeticity, in weld relays, gas massspectroscopy tested 156

Hermetic sealing, for samples 16Heteroepitaxy layers, RBS interfacial studies

on 628Heterogeneity

compositional, micrometer scale in single-phase materials 516

defined 674detected in solids/liquids .402SAS techniques for .402, 405

Heterogeneous catalysis, FIMIAP study of 583Heterogeneous surface tilms, AES

analyzed 566Heterojunctions, topographic imaging

techniques for 376Heteropolytungstates, heavy-atom method to

determine crystal structure of 351Hexagonal ring stretching, Raman microprobe

analysis 133Hexamethyldisiloxane, plasma-polymerized,

NMR analysis of structure and degradationof 285-286

Hexane, as solvent for volatile materialremoval. 575

hfs, See Hyperfine structure.High-carbon steels, carbon content isolated 177Higher-order Laue zone

for aluminum-copper alloy .463in electron diffraction .439-440

High-frequency furnaces 221-222Highly oriented pyrolytic graphite 132, 690High-performance liquid chromatography

and IR spectroscopy 116and mass spectrometry, with gas

chromatography/massspectroscopy 645-646

MFS detection for 72of organic gases 11of organic liquids and solutions 10of organic solids 9

High-purity austenitic stainless steels, atomprobe analysis 595

High-purity metals, voltammetric analysis .. 188High-purity nickel, trace impurities in .....240High resolution, for analysis of Jominy

bar 508High-resolution electron energy loss

spectroscopy 109, 126High-resolution energy-compensated atom

probemicroanalysis 597with pulsed-laser capabilities 598spectrum of tungsten by 597

High-temperature alloysisolation of nickel and cobalt in 174nitric/hydrochloric acid as dissolution

medium 166High-temperature combustion. See also

Combustion; Combustion method 221-225applications 224combustion principles 221-222defined 674detection of combustion products 222-223determinator systems, automatic, manual, or

semiautomatic 222estimated analysis time 221general use 221of inorganic solids, types of information

from .4, 6limitations 221of organic solids 9related techniques 221

Index / 721

sample preparation 223-224samples 221, 223selective and total combustion 223-224separation of interfering elements 222

High-temperature solder, elemental mappingof. 532

Histogram, for IA particle analysis 320Historical studies

of books and artifacts, PIXE analysis for .. 102milliprobe PIXE analysis 107hkl tables, in single-crystal analysis 346

HMDE. See Hanging mercury drop electrode.Holding time, of samples 16Hole drilling, capabilities of 380Hollandite, in ceramic waste form simulant,

EPMA analysis for 532-535Hollow cathode lamp 50, 690Holmium, epithermal neutron activation analysis

of. 239Holographic gratings 37, 128Holtzmann constant, in ESR analysis 254HOLZ. See Higher-order Laue zones.Homogeneity

defined 674of single-phase materials, EPMA micrometer

analysis 516Homogenization, procedures and sampling 16Homologous pairs, defined 674Hooke's law

defined 674molecular vibrations and 111

HOPG. See Highly oriented pyrolytic graphite.Hot extraction, capabilities 226How to use the Handbook 2-11HPLC. See High-performance liquid

chromatography.HR' See Magnetic resonance.HR. See Rockwell hardness.Huber Guinier camera, for XRPD

analysis 336Humans

hair, NAA forensic studies of 233NAA analysis of toxic element retention

in 233Hydrazyl

stable free radical. 265stable free radical, ESR analysis of 265

Hydrided TiFe, phase analysis of 293-294Hydrlde-generation systems

atomic absorption spectrometry 50in analytic ICP systems 36

Hydride generator, for ICP spectrometers 36Hydrobromic acid

with bromine, as sample dissolutionmedium 166

-phosphoric acid method of analysis forcopper in magnesium alloys 65

Hydrocarbonsanalytic methods for 10aromatic, determined 218as fluorescing surface impurities in Raman

analyses 130long-chain, analytic methods for 9oil of, IR split mull of. 113oxidation, Raman analysis 133oxidized in high-temperature combustion

resistance furnaces 224polynuclear aromatic 74surface, determination by selective

combustion 223-224Hydrochloric acid

residue isolation using 176sample component losses in 165for sample dissolution 165solution, as eluent for suppressed cation

chromatography 660Hydrofluoric acid

analysis of solutions in 35as nonoxidizing dissolution medium 165



722/ Index

Hydrogenanalysis by SIMS 610analyzed in microcircuit fabrication

process 156-157atoms, by focusing effect in EXAFS .411atoms, located in organometallic or

intermetallic compounds .420combustion method for elemental analysis

of. 214concentration profiles 610determined by combustion 214determined in copper 231-232dissolved in TiFe crystal structure 294effects as image gas in FIM 587,588gas mass analysis of. 155IGF determination 226, 231in inorganic solids, applicable analytical

methods .4, 6ionization potentials and imaging fields

for 586ion, monitoring by acid-base titration 172in weld relay, gas mass spectrometry of .. 156

Hydrogen-bonded pyridine, Ramananalyses 134

Hydrogen diffusion, NMR study in metals ..277Hydrogen lamp, for UVIVIS analysis 66Hydrogen peroxide

GFAAS analysis of trace tin and chromiumin " 57-58

with hydrochloric acid, as sample dissolutionmedium 166

Hydrogen sulfate, as carcinogenicprecipitant. 169

Hydrolysisto oxides, precipitation by 169sample, nitric acid to prevent 166

Hydroxides, as precipitants 168-169Hydroxyl

content in glass, quantitative analysis 121-122groups, content in glass 121-122ion, monitoring by acid-base titration 172

Hyperfine interaction constants, effect of lowtemperature on 257

Hyperfine splittingin analysis of transition group metals 260and sensitivity reduction 258

Hyperfine structureabbreviation for 690determination of intensity ratios 261ESR spectrum 259patterns 260unresolved, as ESR line-broadening

mechanism 255Hypophosphorous acid, as reducing agent .. 169Hypothesis, testing, and systematic

samples 12-13

II. See Intensity.IA. See Image analysis.lAP. See Imaging atom probe.IC. See Ion chromatography.Ie' See Coherent atomic scattering intensity.ICP. See Inductively coupled plasma;

Inductively coupled plasma atomic emissionspectroscopy.

ICP-AES. See Inductively coupled plasmaatomic emission spectroscopy.

ICP-MS. See Inductively coupled plasma massspectroscopy.

ICP sample introduction, to analyticalsystem 34-36

ICP torch, and gas supplies 34, 36-37Identity operation, defined in crystal

symmetry 346IGF. See Inert gas fusion.Ii' See Incoherent atomic scattering intensity.

IIIeorundum method, XRPD analysis ... '" .340Illuminance, SI derived unit and symbol

for 685Illumination. See also Bright-field images;

Dark-field images.bright-field 310, 689dark-field 690global and punctual, in MOLE/Raman

analyses 129-130Image analysis. See also Metallographic

identification 309-322applications 309,316-320data analysis 313defined 674estimated analysis time 309general uses 309image analyzers 310-313of inorganic solids .4-6introduction 309-310limitations 309NMR, ESR, and UVIVIS analysis,

compared 265of organic solids 9possible errors 313-316related techniques 309samples 309, 313, 316-320types of image analyzers 309

Image analyzerscomponents of. 310-313data analysis 313detection and measurement 311-313input devices 310scanners 310-311

Image contrastdefined 674field ion microscope 588in scanning electron microscopy 500-504

Image gas atom, potential energy of outerelectron 586

Image gases, low ionization, for field ionmicroscopy 587

Image preprocessing, image analysis 310Images

contrast. 500-504, 588, 674FIM, formation of 584FIM, quantitative analysis 590-591typical field ion micrograph (tungsten) ....585

Image-verification procedure .438, 440Imaging

in the analytical electron microscope . .440-446of crystalline structure of integrated circuit,

Auger electron spectroscopy 555defects, x-ray topography 367-368detectors 144, 493-494digital micro- .447, 448flicker-free 525image-verification procedure .438, 440secondary electron, AES detector for .....554second phase, by scanning electron

microscopy .490in the STEM mode .442surface features, by scanning electron

microscopy .490system, molecular optical laser

examiner 129-130TEM and STEM modes, relationship

between .442in the TEM mode .440-442of topographic or microstructural

features 299Imaging atom probe

advantage for single elements 596and atom probe analysis, as

complementary 596-597of interfacial segregation in

molybdenum 599-601schematic 595

Immunoassays, MFS use of fluorescent labelsfor 72

Implantation. See also Ion implantation.as effect of primary ion bombardment 611helium, in bee iron alloy .485of inert elements .475of inert gas elements .485

Impuritiesdepth profiles of heavy element. 632-633determined in nickel. 240liquid chromatography compound analysis

for 649LPCVD thin film analysis for 624metal, in synthetic diamond .417RBS analysis of surface 628in U02 , determined 149-150

Inclusionsanalytical transmission electron

microscopy .429-489Auger electron spectroscopy 549-567defined 176electron probe x-ray microanalysis 516-535image analysis of 314-316as internal defects, in FIM samples 587isolation of residues 176optical metallography 299-308oxide, analysis in steel alloys 162ratings, by image analysis 309refinement of residues 176-177scanning electron microscopy .490-515in steel, isolating 176surface, SEM analysis .490testing 176-177

Incoherent atomic scattering intensity,abbreviation for 690

Inconel nickel-base alloys. See Nickel-basealloys, specific types.

Increment, defined 674Indexing, of electron diffraction

patterns .456-457Index of refraction. See Refractive index.Indicators, acid-base 172Indirect determination, of bromine 70Indirect ion chromatography 661Indium


epithermal neutron activation analysis 239evaporation fields for. 587species weighed in gravimetry 172TNAA detection limits 237

Individuals, defined 674Inductance, SI derived unit and symbol

for 685Induction furnaces, high-frequency 221-222Induction-hardened steel shaft, subsurface

residual stress and hardness distributionsin 389-390

Inductively coupled plasma. See alsoInductively coupled plasma atomic emissionspectroscopy.

electric and magnetic fields 32inhomogeneous, nomenclature of zones 32polychromator or direct-reader spectrometer

for 37Inductively coupled plasma atomic emission

spectroscopy 31-42analytical characteristics 33-34applications 31, 41and atomic absorption spectrometry,

compared 31, 43atomic theory 33calibration curves 33, 34capabilities 141, 233, 333capabilities, compared with X-ray

spectrometry 82capabilities, compared with molecular

fluorescence spectroscopy 72defined 674detection electronics and interface 39detection limits .33



and direct-current arc emissionspectrography 31

direct-current plasma .40direct-reading spectrometer 37-38and emission spectroscopy 21estimated analysis time 31of inorganic liquids and solutions 7of inorganic solids .4-6interference effects 33-34introduction 31-32limitations 31nebulizer 34-36neutron activation analysis and,

compared 233new developments 39-40plasma 32polychromator. 34, 37-38precision and accuracy 33principles of operation 32procedure 34related techniques 31samples 31, 34-36scanning monochromator 38system components 34-39system computer for. 39zones of plasma 32

Inductively coupled plasma massspectroscopy

as new development 39-40capabilities 233instrumentation for .40neutron activation analysis and, compared 233

Industrial materialsquantitative elemental analysis by classical

wet chemistry 162-179raw, sampling of. 12-18waste products, sampling of 12-18

Inelastic mean free path, electron 569-571Inelastic scattering

analytical transmission electronmicroscopy ~ .. .433-434

bremsstrahlung .433defined 674excitation of conduction electrons and

secondary electron (low-energy)emission .433-434

inner-shell ionization .433Inert elements, implantation of 475Inert gas elements, implanted .485Inert gas fusion 226-232

defined 674detection of fusion gases 229-230determination of gases 229-231estimated analysis time 226general use 226of inorganic solids 4, 6introduction 226-227limitations 226operation, principles of 227-228related techniques 226samples 226, 231-232selective fusion 231separation of fusion gases 228-229

Inert gas ion sputtering, LEISS analysis 603Inert gas-purged polychromator 37Infinitely thick/thin samples, x-ray

spectrometry 93Infrared absorption

as detector for C and S in high-temperaturecombustion " 221-222

sulfur determination in high-temperaturecombustion by 221-225

Infrared absorption spectrophotometry,residue analysis by 177

Infrared detectionof carbon and sulfur, high-temperature

combustion 223inert gas fusion 230

Infrared diode lasers, applications 112

Infrared emission spectroscopy 1l5Infrared linear dichroism spectroscopy, for

molecular orientation in drawn polymerfilms 120

Infrared micosampling 1l6Infrared microscopes 1l6Infrared radiation, defined 674Infrared reflection-absorption

spectroscopy 114, ll9Infrared spectra " 1l0, ll6, 674Infrared spectrometers, defined 674Infrared spectroscopy 109-125

absorbance 110, ll7applications 109, ll8-124attenuated total reflectance

spectroscopy 1l3-ll4basic principles ll0-lllBeer's law 1l7capabilities 212, 333, 649chromatographic techniques 1l5-ll6computerized, Fourier transform infrared

spectroscopy as 109curve filling 1l7-ll8defined 674degrees of freedom 1l0depth profiling 113, 115diffuse reflectance spectroscopy 114dipole moment 111dispersive 111emission 115estimated analysis time 109Fourier-transform infrared

spectroscopy 109-110, 111-ll2and gas analysis by mass spectroscopy,

compared 151general uses .. . . . . . . . . . . . . . . . . . . . 109for glasses, compared with Raman ... 130-131infrared reflection-absorption

spectroscopy 1l4of inorganic gases 8of inorganic liquids and solutions 7instrumentation 110-112introduction 109-110limitations 109microsampling for 116molecular vibrations 111of organic gases 11of organic liquids and solutions 10of organic solids 9for orientation of DTDMAC on nonmetallic

surfaces 119photoacoustic spectroscopy 115polarization modulation 114-115qualitative analysis 116-117quantitative analysis 117-118and Raman, compared for polymer

analyses 131and Raman spectroscopy 126-127reflectance methods 113-115reflection-absorption spectroscopy 114related techniques 109samples 109, 112-ll6sampling and sample preparation 112-ll6Snell's law 113specular reflectance 115use of Fourier transform spectrometers in ..39as vibrational surface probe 136

Infrared spectrum, defined 110, 674Infrared-transparent pressing powder,

sample pellets of 113Inhomogeneity

as ferromagnetic resonanceapplication 274-275

magnetic, determined 274-275in surfaces, AES analysis for 549

Initial intensity, abbreviation for 690Inner-shell ionization, as inelastic scattering

process .433Inorganic atoms, MFS analysis of 74

Index / 723

Inorganic compounds, gas analysis of 151Inorganic Crystal Structure Data Base 355Inorganic elements, SSMS analysis of 141Inorganic gases, analytic methods for 8Inorganic liquids, analytic methods for 7Inorganic materials. See also Inorganic

materials, characterization of; Inorganicsolid materials.

for identification and structure determinationin 109

single-crystal, Raman analysis of 129Inorganic materials, characterization of. See

also Inorganic materials; Inorganic solidmaterials.


atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211crystallographic texture measurement and

analysis 357-364electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis 516-535electron spin resonance 253-266extended x-ray absorption fine

structure .407-419ferromagnetic resonance 267-276field ion microscopy 583-602inductively coupled plasma atomic emission

spectroscopy 31-42infrared spectroscopy 109-125ion chromatography 658-667low-energy electron diffraction 536-545low-energy ion-scattering

spectroscopy 603-609molecular fluorescence spectrometry 12-8 IMossbauer spectroscopy 287-295neutron activation analysis 233-242neutron diffraction .420-426nuclear magnetic resonance 277-286optical emission spectroscopy 21-30optical metallography 299-308particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187radial distribution function analysis 393-401Raman spectroscopy 126-138Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627single-crystal x-ray diffraction 344-356small-angle x-ray and neutron


spectroscopy 60-71voitammetry 188-196x-ray diffraction residual stress

techniques 380-392x-ray diffraction 325-332x-ray photoelectron spectroscopy 568-580x-ray powder diffraction 333-343x-ray spectrometry 82-101x-ray topography 365-379

Inorganic mixtures, liquid chromatographyfor 649

Inorganic molecules, MFS analysis of 74Inorganic solid materials. See also Inorganic

materials; Inorganic materials,characterization of.

analytic methods for .4-6chemical reagents, composites, and catalysts,

analytic methods for. 6glasses and ceramics, analytic methods for ..5metals, alloys, and semiconductors, analytic

methods for. .4



724/ Index

Inorganic solid materials (continued)minerals, ores, and slags, analytic methods

for 6pigments, compounds, and effluents, analytic

methods for 6Inorganic solutions, analytic methods for 7Input devices, image analyzers 310Instrumentation

of x-ray spectrometry 87-93as XRPD source of error 341

Instrument response time, defined 674Integral of, symbol for 692Integrated circuits

cross section, LPCVD tungsten layers ....513oxygen in wafers for 122-123secondary electron micrograph 555SEM analysis of 513-514

Integrating spheres, as radiation collector inmid-infrared region 114

Intense Pulsed Neutron Source, ArgonneNational Laboratory .424

Intensityabbreviation for 690absorption/enhancement effects on 97calculating crystal structure from 349coherent atomic scattering, abbreviation

for 690vs concentration nickel, nickel ores 99of diffracted beams 328-329diffracted, resolving of .424diffractional, kinematic, and dynamic effects

in 366-367diffraction, in single-crystal x-ray

diffraction 348-349of electromagnetic radiation 83incoherent atomic scattering, abbreviation

for 690infrared. . . . . . . . . . . . . . . . . . . . . . . . . Ill, 117initial, abbreviation for 690in IR spectra 110luminous, SI base unit and symbol for 685measured by diffractometers 351measurement, as XRPD source of error 341observed, in single-crystal analysis 346profiles, rocking curves as 372radiant, defined 62, 680, 685ratio, defined 674ratio methods, for thin-film sample

preparation 95relative Auger, quantitative AES analysis

based on 553relative, x-ray spectral lines 98scattered . . . . . . . . . . . . . . . . . . . . . . . . . 604theoretical vs thickness, single-element x-ray

spectrometry 100total diffracted, abbreviation for 690

Interatomic bond distances,determined 344, 409

Interatomic bond lengths, and physicalproperties 355

Intercalationdefined 345in graphites 132

Interelement effects. See also Inductivelycoupled plasma atomic emissionspectroscopy.

absorption of x-rays as cause 97in emission spectroscopy 33-34in x-ray spectrometry 87

Interfacesand superlattice studies 634-635cementite/ferrite, atom probe composition

profile across, in pearlitic steel 593FIMIAP study of segregation of alloy

elements and impurities to 583narrow, AEM analysis .482-483segregation, atom probe composition profile

for 593SERS analysis of 136

Interfacial studieson heteroepitaxy layers 628segregation in molybdenum 599-601superlattices 634

Interference, destructive, x-rayspectrometers 88

Interference of waves, defined 675Interferences. See also Spectral interferences.

in collection of x-ray lines in 2.30-keVspectral vicinity 522

effect of complexation reactions 164effects in ICP 33-34, 40electrodeposition of 65-66in EXAFS analysis .408filters for 67fringes as 368intentional addition of 66ionization 29,33,34separation by complexation for 65simultaneous UVIVIS analysis for 65spectral, wavelength-dispersive

spectrometry 521-522of waves, defined 675

InterferogramsFT-IR 112as resolution enhancement 117

Interferometerschanging optical path length 112defined 675FT-IR 111-112Genzel. 112Michelson 39, 112

Intermetallic compoundsneutron diffraction analysis .420TiFe, hydrided, phase analysis by Mossbauer

spectroscopy 293Internal conversion, as radioactive decay

mode 245Internal electrolysis 199-201

cell for 199for copper determination 200separation of cadmium and lead by 201

Internal fluorescence peak, in EDSspectra 520

Internal reflection elementsand sample interface, angle of

incidence 114in ATR spectroscopy 113-114micro KRS-5 (thallium bromide/thallium

iodide) 113top view, micro KRS-5 113

Internal standard, defined 675Internal standard line, defined 675Internal standard method, XRPD

analysis 340Interphase interfaces, FIMIAP study of point

defects in 583Interplanar spacing dh kl . See d-spacings.Interstitial nitrogen, determined in steels 178Intersystem crossing, defined 675Introduction system complex 152Introduction system, gas mass

spectrometer 151-152Invariant phase field determination, by Auger

electron spectroscopy .474Inversion center, in single-cells 347Inverted optics

for liquid x-ray spectrometry 95in wavelength-dispersive x-ray

spectrometers 88In vivo measurement, by neutron activation

analysis 23310 , See Initial intensity,Iodides

determined by precipitation titration 164as electrode 185solvent extractant for 170

Iodimetric titration, indirect 174Iodimetry, as class of redox titration 174

Iodineand absolute methanol, to isolate inclusions in

steels 176determined in water by coulometric

titration 205and methanol, second-phase test method .. 177species weighed in gravimetry 172TNAA detection limits 237

Iodine bromide, in graphites, Ramananalysis 133

Iodine chloride, in graphites, Ramananalysis 133

Iodoantimonite method, analysis for antimonyin copper alloys by 68

Iodometry, indirect 205Ion beam

LEISS analysis 606-607milling, transmission electron

microscopy .451-452mixing, as sputtering artifact. 556in spark source mass spectrometer 142sputtering, Auger electron emission by 550

Ion channeling, for damage depth profiles ..632Ion chromatogram, typical total 644Ion chromatographs

and AAS instruments 55major components 658-659

Ion chromatography exclusion, separationin 662

Ion chromatography 658-667applications 658, 665-667calibration curves 666capabilities 181,649,663defined 675estimated analysis time 658exclusion 662general uses 658indirect 661of inorganic liquids and solutions, information

from 7of inorganic solids, types of information

from .4-6instrumentation 665introduction 658-659limitations 658modes of detection 659-662modes of separation 662-663of organic solids, information from 9related techniques 658reversed-phase 663sample preparation and

standardization 663-665samples 658, 663-667with spectrophotometric detection 661standard, separation mode 662

Ion detectionin gas mass spectrometers 153, 154-155methods 143-144methods, electrical and photometric .. 143-144

Ion exchangedefined 675principles of 658-659separation 66, 164-165, 170, 249

Ion-exchange chromatographydefined 675as separation

technique 168, 170, 653, 658-659Ion-exchange resins

core, materials for 662defined 675function in ion-exchange

chromatography 658-659as sampling substrates, x-ray spectrometry 94

Ion gunsaligned, by AES analysis 550for sputter removal of atoms, AES

analysis 554Ionic bond, defined 675Ionic charge, defined 675



Ionic crystals, ESR studied 263Ionic displacement

vs dilute acid, as digestion method 176in qualitative classical wet analysis 168as second-phase test method 177

Ion implantation. See also Implantation,AEM determination of microstructures

in .484-487damage, defect depth distribution for .....628heavy, depth distribution by Rutherford

backscattering spectrometry 628profile, phosphorus, in silicon 623-624Raman analysis 133SIMS phosphorus depth profiles 624

Ionizationelectron-impact, in gas mass

spectrometer 152-153inner-shell, as inelastic scattering process 433interferences 29, 33, 34limit, optical emission spectroscopy 22post-, EEL imaging .450potential, defined 153pre-, EEL imaging .450self-, of water 203suppressants, atomic absorption

spectrometry .48suppressed in flame emission sources 30

Ion microprobes 161,614Ion microscopes 614, 615Ion milling, as FIM sample preparation 584-585Ion neutralization, defined 675Ion-pair chromatography 653-654, 675Ion quadrupole mass filter, in gas mass

spectrometers 153-154Ions

beam, LEISS analysis 606-607bombardment, effects 611chloride, determining nickel in samples

containing 201common effect, in gravimetric analysis 163daughter, GC/MS scans of 646defined 675detection methods, spark source mass

spectrometry 143-144detectors, electron multiplier as 153-155dichromate, UVIVIS analysis of chromium

in 70effect of chelons on 164exchange principles 658-659exchange separation, classical wet chemical

analysis 164-165formation 142, 640fragment, in gas mass spectrometer 153hydrogen or hydroxyl, monitoring by

acid-base titration 172inorganic, determined by ion

chromatography 663interactions, determined by single-crystal

x-ray diffraction 344metal, separation and determination of 197,

200-201monitoring 153-154, 644negatively charged, or anions 659numbers for atom probe microanalysis 594optical aberrations, in atom probe

analysis 595parent, GClMS scans 646positively charged, or cations 659probe, defined 679quantitative determination by

electrogravimetry 197radical. 263, 265rate of flow to electrode, effects in

electrogravimetry 198removal, byelectrogravimetry 197,200sample, ion chromatography 658, 663-665secondary, defined 681separation, in constant current

electrogravimetry 198

solvated molecular, UVIVIS analyzed .....61as sources, mass

spectrometer 142-143, 152-153species of, defined 675transition-element, identification of valence

states of 253-266transition-metal, ESR analysis of 253, 254

Ion scatteringspectra 604-606, 675surface structure study by channelingl

blocking 633Ion scattering spectroscopy. See also Low-

energy ion-scattering spectroscopy.capabilities 549defined 675low-energy 603-609

Ion-selective electrode. See also Ion-selectivemembrane electrodes.

analysis of inorganic solids 6and direct and titrimetric potentiometry 204

Ion-selective membrane electrodes. See alsoIon selective electrodes.

determining selectivity 182-183membrane potential 182types of. 182

Ion sputtering 565, 575IR. See Infrared spectroscopy.IRE. See Internal reflection elements.Iridium

anomaly, at Cretaceous-Tertiaryboundary 240-241

concentration found as function of depth instrata 241

destructive TNAA for 239, 241determined by controlled-potential

coulometry 209field evaporation in 586, 587gravimetric finishes 171point defects observed by field ion

microscopy 588Iron. See also Iron alloys; Iron alloys, specific

types.age-hardened, FIMIAP study of precipitates

in 583in aluminum, extended solubility

of 294-295in aluminum matrix, x-ray maps of .448analysis in copper-beryllium alloys, by

thiocyanate method 68analysis, in lead alloys, by phenanthroline

method 66Auger chemical map for 557constant-current electrolysis 200in copper, analysis of phases of 294determined by controlled-potential

coulometry 209emission spectrum, spectral complexity

of. 22estimated volume of signals produced by

20-keV electron beam 500evaporation fields for 587ICP-determined in plant tissues .41iosotope composition and intensity 146K-absorption edge of .416Monte Carlo electron trajectory simulation,

for EPMA effects in 518neutron and x-ray scattering, and absorption,

compared .421nickel diffusion into, measurement of 243nonmetall ic elements determined in 178photometric analysis methods 64qualitative tests to identify 168quantitative determination of carbon and

sulfur 223-224redox titration 175species weighed in gravimetry 172in thermite, AAS analysis for 56TNAA of 236, 238volumetric procedures for 175

Index / 725

x-radiation, sulfur determination from .....94Iron alloys. See also Iron; Iron alloys, specific

types.analysis for copper in, neocuproine

method 65bee, EXAFS spectra above K-edges .416bee, helium implantation analysis .485diffraction techniques, elastic constants, and

bulk values for 382false silicon peak in EDS spectra of 520glow discharges for 28hydrogen peroxide dissolution medium

for 166sodium peroxide fusion 167steel, AAS analysis for trace metals 55sulfuric acid as sample dissolution

medium 165Iron alloys, specific types. See also Iron; Iron

alloys.17-4PH, diffraction techniques, elastic

constants, and bulk values for 382316, diffraction techniques, elastic constants,

and bulk values for 382410, diffraction techniques, elastic constants,


and bulk values for 3824340, local variations in residual stress from

surface grinding 390-39152100, diffraction techniques, elastic

constants, and bulk values for 3826260, diffraction techniques, elastic constants,


and bulk values for 382Fe-0.8C, TEM micrograph 509Fe-20Ni and Fe-25Ni, diffusion measurements

in .477Fe-Cr-Co permanent-magnet, FIM/AP

images 600Haynes 556, AEM-EDS two-phase

microanalysis of .447Incoloy 800, diffraction techniques, elastic

constants, and bulk values for 382Inconel 600 U-bend, residual stress 390Inconel 718, minimum and maximum

principal residual stress profiles 392Inconel 718, x-ray elastic constant

determination for 388Invar, diffraction techniques, elastic constants,

and bulk values for 382Kovar, elemental mapping 532M50, diffraction techniques, elastic constants,

and bulk values for 382M50 high-speed tool, diffraction-peak breadth

at half height 387Rene 95, diffraction-peak breadth at half

height, as function of percent coldwork 387

Iron-base magnet alloysFIMIAP analysis of. 597-599spinodal decomposition of. 598

Iron-base superalloysATEM image, spot diffraction pattern, and

indexed schematic diffraction patternfor. .438, 440

AEM analysis of "i-austenitematrix .453, 455

diffraction pattern and bright-field andcentered dark-field images of .442

two-phase microanalysis in .447Iron-carbon alloys, image analysis plots,

effects of detected area fraction 309Iron chip combustion accelerators 222Iron-chromium-cobalt alloys, composition

profiles for 600Iron ores, acid dissolution mediums 165Iron oxide films, composition

determined 135



726/ Index

Irradiance 675, 685Irradiated materials

ESR analysis 254, 263x-ray diffraction residual stress techniques 385

Irradiationof atoms, decay rate 235container, as contamination source 235epithermal vs thermal neutron 234gamma-ray spectrum of ores after. 235of sample, NAA analysis as 234TNAA detection limits for rock and soil

after 236-238IRRAS. See Infrared reflection-absorption

spectroscopy.ISE. See Ion-selective electrode.Isobar, defined 675Isocratic elution, defined 675Isokinetic sampling, devices for 16Isomers

determined by GC-IR 115identification and quantification by NMR 277shift, in Mossbauerspectroscopy .....288-290

Isomer shift, in Mossbauerspectroscopy 288-290, 292

Isothermsadsorption, Raman analysis as probe for .. 134phase transformation 317

Isotone, defined 675Isotope abundances, in mass spectra 641-642Isotope dilution analysis

capabilities 243by ICP-MS .40neutron activation analysis and,

compared 233Isotope factor, defined 236Isotopes

defined 675dilution .40, 145, 233, 243dry spike dilution, for spark source mass

spectrometry 146mass numbers of most stable per element 688multielement, for SSMS analysis ..... 145-146natural composition, iron, chromium, nickel,

and manganese 146naturally occurring, percent abundance and

atomic mass 643oxygen, determined in explosive

actuator 625-626radioactive 243, 244ratio measurement .40, 233as tracers or "spikes," 145

Isotopic analysis. See also Mass analysis.of inorganic gases, analytic methods for .... 8of inorganic liquids and solutions, analytic

methods for. 7of inorganic solids, analytical methods

for .4-6of organic solids and liquids, analytic methods

for 10of organic solids, analytic methods for. 9

Isotropic thermal motions, and crystal structuredetermination 352, 353

II' See Total diffracted intensity.

JJablonsky diagram, molecular absorption and

de-excitation processes, molecularfluorescence spectroscopy 73

Jacquinot's advantage, in Ff-IRspectroscopy 112

JCPDS card, x-ray powder diffraction data,mineral quartz 341

JCPDS Powder Diffraction File, use inelectron diffraction/EDS analysis .. .455-459

Jemez mountains, gamma-ray spectrum of oresfrom 235

Johnson noise. See Thermal noise.

Joints, integrity of, determined by opticalmetallography 299

Jominy bar, high-resolution analysis for. 508Jones reductor, for redox volumetric

methods 175-176Joule 685, 691Joule-Thomson effect, defined 675Joule-Thomson expansion, defined 675

KK~ aluminum or magnesium x-ray lines,

characteristic 570K~ doublet 385-386, 570K~ radiation, pure 326K-absorption

edge, pure nickel .408of nickel and iron .416

Karl Fischermethod for water determination 219reagent for surface oxides 177, 204titration 177

K-edgeabsorption spectrum, krypton gas .410aluminum, in light-element analysis by AEM

methods .461EXAFS of nickel metal .408EXAFS spectra .411fine structure .409iron and nickel, EXAFS spectra above

the 416of magnesium-, iron-, chromium-containing

compounds, EXAFS studies .408normalized nickel .417XANES, vanadium .415

Ketones, and aldehydes, determined 217k-factor, defined 675K-family x-ray lines, EPMA analysis 522Kikuchi diffraction patterns


defined 675deformed OFHC copper, dislocation cell

structure analysis .471Kikuchi lines. See Kikuchi diffraction patterns.Kinematical diffraction, in defect

imaging 367-370Kinematics

collision, in Rutherford backscatteringspectrometry 629

of diffraction 366Kinematic viscosity, SI derived unit and symbol

for 685Kinetic energy

AES and XPS measurement as functionof. 550

of Auger and photoemitted electrons ..569-570of bombarding electrons, effect in x-ray

emission 84converted to radiation 83defined 675of electrons, electron temperature for 24of heavy particles, gas kinetic temperature

for 24measurement, as basis of x-ray photoelectron

spectroscopy 85as pass energy 571Raman spectroscopy analysis 129range, Auger electron 551of styrene polymerization reaction 132

Kineticsabsorbance-subtraction studies of 116of cellular decomposition of martensite in

uranium alloy 316-318chemical reaction, potentiometric membrane

electrodes as detectors for 181crystal, by x-ray topography 376of crystals, and material transformations ..376

dispersive EXAFS analyses .418first-order, ESP study of free radicals 266GC-IR study of 115of growth, LEED analysis 536, 544NMR analysis 277of overlayer growth at submonolayer level

and above, LEED analysis 544of radical production and decay 265-266reaction, analyses 109, 628of texture development .424voltammetric analysis 188

Kinetic temperature, gas, and kinetic energyof heavy particles 24

Kjeldahl determinationapplications 214estimated analysis time 215in ion-selective electrode methods 186limitations 215for nitrogen 172-173, 214-215use with bromine and methyl acetate

dissolution 177KL2 ,3 transition, Auger electron emission

by 550K lines

fluorescent yield vs atomic number for 87intensity in titanium 97relative emission intensities of 86, 87

KLM markers, for qualitative x-rayspectrometric analysis 95-96

Klystron 255, 675K-matrix method, as IR multicomponent

analysis 117, 118Knight shift measurements 284KoirtyohanniPickett continuum-source

background correction system ....51, 52Kossel-Mollenstaedt (K-M) dilTraction

patterns .439, 441, 690Kossel pattern, as CBEDP .439, 442Kovar alloy, surface atomic values 579Kovar-glass seals, shear fraction studies

of 577-578K-photoelectron, germanium, backscattering

of. .408K-radiation, defined 675Kronecker Delta, use in ODF analysis 362KRS-S, as internal reflection element 113Krypton

continuous-wave gas lasers 128gas, EXAFS analysis .409, 410gas, K-edge absorption spectrum .410ionization potentials and imaging fields

for 586K-series, defined 675K-shell, defined 675Ku' See Uniaxial anisotropy.KulenkamplT expression, x-ray emission ....84Kunzl's law, energy/chemical shifts in EXAFS

analysis following .416Kurchatov, as synchrotron radiation

source .413Kurdjumov-Sachs orientation

relationship .438-439

LI. See Length.L2 ,3 transition, Auger electron emission

by , 550Laboratory animals, NAA analysis for

retention of toxic elements in 233Laboratory sample, defined 676Lachance-Trail equation, calibration curves for

x-ray spectrometry 98Ladder diagrams

in atom probe microscopy 594of nickel-base superalloy IN 939 598, 599

Lamb-Miissbauer factor. See Recoil-freefraction.



Langmuir-Blodgett depositiontechnique 119-120

Langmuir Torch atomizer, atomic absorptionspectrometry 54

Lang topographynear-surface analysis 377Pendellosiing fringes obtained by .368for polygonization of elastic strain

relaxation 370, 377Lanthanides

on periodic table 688species weighed in gravimetry 172use in flame atomizers .48weighed as the fluoride 171

Lanthanumadditions to flame AAS samples .48fluoride separation 169TNAA detection limits 237

Larmor frequency, defined 676Larmor period, defined 676Laser-induced fluorescence

spectroscopy 80-81Laser-induced resonance ionization mass

spectroscopy .141, 142Laser microprobe mass

analysis 142, 516, 583Lasers

ablation for solid-sample analysis 36broadband tunable dye 128continuous-wave gas 128in corrosion analysis 135exposure to preactivate Raman analysis

samples 130helium-neon, in Fr-IR spectroscopy 112irradiation, of 202 steel 623as light source in vibrational

spectroscopy 128low-powered, for Raman analysis of

graphites 132in molecular fluorescence

spectroscopy 76, 80-81neodymium-doped, yttrium-aluminum-garnet

(Nd:YAG), in spark source massspectrometry 142, 597

nitrogen gas, for atom probe analysis 597radiation, use in Raman spectroscopy 128in Raman analyses of polymers 131Raman molecular microprobe 129stability of 112treatment of stainless steel, SIMS surface

analysis of 622-623tunable infrared 112tunable radiation from 142welding by 156

Lateral resolution, atom probeanalysis 595-596

Lattice-parameter method, XRPDanalysis 339

Lattices. See also Crystal lattices; Superlattices.cubic, singular and vicinal surfaces of 537defects imaged by x-ray topography 365determining geometries of 327-328diffraction in 327distortion in 365, 368imaged by phase contrast. .445image of zinc oxide by combined beams . .446imaging, transmission electron

microscopy .445-446location in 628, 633-634MFS study of constituents 72modulations, in photoacoustic

spectroscopy . . . . . . . . . . . . . . . . . . . ....115-parameter and lattice-type determinations, by

XRPD analysis 333reciprocal, and Ewald construction 539space, in crystal systems 347spacing 384, 690strain measurement by dechanneling

in 634-635

strain measurement in 633-635vibrations 126, 130

Laue camera, for XRPD analysis 334-335Laue case

reflection topography 366synchrotron radiation with 374transmission patterns of aluminum 376

Laue zonesfirst-order (FOLZ) .439, 442higher-order (HOLZ) 439, 442zero-order (ZOLZ) .439

Layered structures, RBS analysis for 628Le. See Liquid chromatography.Leachates 7, 658Lead

-acid batteries 135air-acetylene flame atomizer for .48in blood, GFAAS analysis 55and cadmium separation, by internal

electrolysis 201deposition of. 20 Idetermined by 14-MeV FNAA 239determined by controlled-potential

coulometry 209determined in coal fly ash 147determined in plant tissues .41EDTA titration 173-174as electrode 185gaseous hydride, for ICP sample

introduction 36gravimetric finishes 171in iron-based alloys, AAS analysis

for. 55, 56LEISS segregated to surface of tin-lead

solder 607-608photometric analysis methods 64qualitative tests to identify 168quartz tube atomizers with .49recovery from brass 200species weighed in gravimetry 172in steel chips, GFAAS analysis 55sulfate ion separation 169sulfuric acid as dissolution medium 165surface corrosion, Raman analysis 135volumetric procedures for 175

Lead alloysanalysis for iron by phenanthroline

method 66Freiberger decomposition in 167sample dissolution medium 166

Lead oxide, in binary phosphate glasses 131Lead-tin alloys, eutectic, electropolished SEM

section 510Leak rate, tested in weld relays 156Least squares fit

curve fitting 118in EXAFS data analysis .414in surface stress measurement 386use in determining crystal structure ..351, 353for x-ray spectrometry 97-98

L-edges, of cesium to neodymium, EXAFSdetermined .408

LEED. See Low-energy electron diffraction.Leforte aqua regia, as dissolution medium for

sulfide minerals 166LEISS. See Low-energy ion-scattering

spectroscopy.Lengendre addition theorem 362Length 685, 686, 690Lenses

and deflector system, ECAP 597defined 676Einzel, in gas mass spectrometer 153electromagnetic, analytical transmission

electron microscopy .432Ray diagram .492SEM microscopes .492

Lensing action, scanning electronmicroscopy .492

Index / 727

Lerch and Bogue method, of free limecontent 179

Lewis acid sites, pyridine adsorption at, Ramanstudies 134

L-family x-ray lines, EPMA analysis 522Lifetimes, electronic excited-state, MFS

determined 72Ligands 70, 676Light

defined 676-element sensitivity, Auger emission and ..550path, through Czemy-Turner

monochromator. 23in UVIVIS analysis 61

Light-element analysiscombined EDS/EELS analysis .460-461with EDS and WDS systems, compared ..522by EDS/UTW-EDS/EELS .459-461for precipitate identification in stainless

steel .459-461results .461sensitivity, Auger emission and 550

Light elementsidentification of. .459-461metallographic identification 558-561

Light scatteringenergy-level diagram of. 127fundamentals 126-130

Lime, free, analysis in Portland cement .... 179Limestone

dissolution in hydrochloric acid 165flame emission sources for 30

Lineintensity 328pair, defined 676position 328profile 331-332scan, double-deflection system .493-495

Linear absorption coefficient, symbol for ..692Linear dispersion, defined 676Linear regression. See Least squares fit.Linear sweep voltammetry, vs DME

polarography 191Line blackening. See also Blackening;

Intensity,in spark source mass spectrometry 142

Line broadening. See also Broadening.analysis, and microbeam method 374analysis, factors controlling 331,332collisional, emission spectroscopy 22Doppler, in emission spectroscopy 22mechanisms, electron spin resonance 255stark, emission spectroscopy 22in x-ray diffraction residual stress

techniques 386-387Line gratings. See Gratings.Line pair, defined 676Lineshapes

absorption and dispersion, in nuclear magneticresonance 280

Auger spectra, and bonding changes 552changes, measurement 552Lorentzian and dispersion 281

Linewidth, as FMR resonantphenomenon 267, 268

Liquid alloys, NMR analysis of electronicstructure of 284

Liquid chromatographsand AAS instruments 55components 650UVIVIS detection of species in 60

Liquid chromatography 649-657applications 649, 655-657chromatographs, liquid 55, 650-651defined 676estimated analysis time 649fundamental concepts 651general uses 649introduction 649-650



728/ Index

Liquid chromatography (continued)limitations 649mobile phase programming 654modes of 651-654preparative 654qualitative and quantitative analysis by 654related techniques 649samples 649as separation tool 170

Liquid fire method, of wet washing organicsubstances 166

Liquid-liquid chromatography 652, 676Liquid membrane electrodes 182Liquid metals, NMR analysis of electronic

structure of 284Liquid organic compounds, ESR study of ..263Liquid-partition chromatography. See

Liquid-liquid chromatography.Liquids. See also Liquids. characterization of;

Solutions.immiscible, permeability 164inorganic, and solutions, analytic methods

for 7nonvolatile, as lR samples 112organic, analytic methods for 10organic volatile, analytic methods for 10RDF coordination numbers for 393as samples 95, 664SAS analysis of .402with suspended solids, sample

preparation 95volatile, analytical methods for 7

Liquids, characterization of. See also Liquids.atomic absorption spectrometry .43-59classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron spin resonance 253-266elemental and functional group


structure .. " .407-419gas analysis by mass spectrometry 151-157gas chromatography/mass


spectroscopy " 31-42infrared spectroscopy 109-125ion chromatography 658-667liquid chromatography 649-657molecular fluorescence spectrometry 72-81neutron activation analysis 233-242neutron diffraction .420-426nuclear magnetic resonance 277-286optical emission spectroscopy 21-30potentiometric membrane electrodes .. 181-187radial.distribution function analysis 393-401Raman spectroscopy 126-138ultraviolet/visible absorption

spectroscopy 60-71voltammetry 188-196x-ray spectrometry 82-101

Liquid-solid chromatography 651-652, 676Lithium

cations, in glasses, Raman analysis 131-doped germanium gamma-ray detector 235-drifted silicon detector 89, 90energy-level diagram, emission lines 22flame emission sources for 30species weighed in gravimetry 172in vacuum, as SERS metal 136

Lithium borate, glass-forming fusions 94Lithium carbonate

for acidic samples in flux 94as binding agent for samples, x-ray

spectrometry 94as fluxes 167

Lithium-doped germanium Ge(Li)detectors 235, 241

Lithium-doped silicondetectors 83, 89-91, 389, 519

Lithium fluoridefor base samples in flux 94as common analyzing crystal, in x-ray

spectrometry 88Lithium metaborate, as flux 167Lithium tetraborate

as flux 93, 167glass-forming fusions with 94

Live time, in x-ray spectrometry 92L lines 86, 87Local structure, determination by EXAFS

analysis .407Local thermodynamic equilibrium

abbreviation for 690emission source in 24

log. See Common logarithm (base 10).Log ratio scanning, analysis by 144Long-chain hydrocarbons, analytic methods

for '" 9Long-range order, analyses for 277,393Lorentzian absorption curve, ESR

spectrum 259Lorentzian absorption lineshape, and

dispersion lineshape 281Lorentz microscopy, for imaging magnetic

domain boundaries .446Lorentz polarization, and absorption, surface

stress measurement correction for ..385-386Lot, defined 676Lot sample, defined as gross sample 674Low-alloy steels, C, P, and S determined in ..29Low-carbon steels

influence of detection setting on detection areafraction 312

sheet, edge effects and etching influence,image analysis 316, 318

spheroidized cementite particles pinning arecrystallization front .471

Low-energy electron diffraction 536-545acronym 689applications 536, 543-544capabilities, FIMIAP and 583defined 676diffraction measurements 539-541estimated analysis time 536general uses 536introduction 537limitations 536, 542-543and multiple-scattering effects in EXAFS

analysis .410principles, diffractions from surfaces 538-539related techniques 536sample preparation 541-542samples 536, 541-542surface crystallography vocabulary ...537-538surface-sensitive electron diffraction,

limitations of 542-543use with Auger electron spectroscopy 554

Low-energy ion-scatteringspectroscopy 603-609

applications 603, 607-609Auger electron spectroscopy and 554basic elements of system 607capabilities 568capabilities, compared with Rutherford

backscattering spectrometry 628effect of improved mass resolution 605electrostatic analyzers for 607estimated analysis time 603general uses 603of inorganic solids, information from .4-6instrumentation 606-607introduction 603-604limitations 603of organic solids, information from 9

quantitative analysis 605-606related techniques 603samples 603, 607-609scattering principles 604spectra 604-606standards and correction factors '" 606

Lower limit of detection, of an element 96Low-pressure sputter chambers, atomic

absorption spectrometry 54Low-temperature fusion, sample

preparation 94Low-temperature storage, of samples 16Low-temperature techniques, in molecular

fluorescence spectroscopy 78-79LPCVD thin films. See also Films; Thin films.

quantitative impurity analysis in 624L-radiation, defined 675LSC. See Liquid-solid chromatography.L-series, defined 676L shell, defined 676LTE. See Local thermodynamic equilibrium.Lubricant coatings, measured 177Lubrication, AES analysis of 565Lucas-Tooth and Pyne model, calibration of

x-ray spectrometry 98Lunar surface

composition analysis by neutron activationanalysis 234

destructive TNAA analysis 239Lutetium, TNAA detection limits 237, 238L'vov platform .49, 55

Mm. See Molal solution.M. See Magnification; Magnetization; Molar

solution.Machined paris, as XRS samples 95Machining, determination of maximum residual

stress produced by 392Macroanalysis. See also Bulk analysis.

of inorganic gases, analytic methods for ....8of inorganic liquids and solutions, analytic

methods for. 7of inorganic liquids and solutions, analytic

methods for 7of inorganic solids, analytic methods for . .4-6macrograph, as-cast aluminum ingot 302optical metallography 301-303of organic solids and liquids, analytic methods

for 9,10Macroscopic stress, defined 676Macroscopy, of metallographic

sections 303-304Macro-SIMS instrument, for qualitative

analysis 613Macrostresses

measurement by x-ray diffraction residualstress techniques 380

states analyzed by neutron diffraction .424in x-ray diffraction residual stress

techniques 381Macroviewer, as input device on image

analyzers 310Magic-angle spinning nuclear magnetic

resonance, capabilities .407Magnesium

alloys, analysis for copper in, hydrobromicacid/phosphoric acid method 65

determined in plant tissues .41EDTA titration 173ion removal from 200ions, exchanged in water softeners 658-659in iron-base alloys, flame AAS analysis 56photoejection of electrons in 85photometric analysis methods 64precipitated as ternary phosphate 173species weighed in gravimetry 172



sum peaks in EDS spectrum of. 520TNAA detection limits 237volumetric procedures for 175weighed as the phosphate 171

Magnesium nitrate, as sample modifier,. GFAAS analysis 55

Magnesium oxide, in binary phosphateglasses 131

Magneticanisotropy, determined 272-273disordered materials, exotic effects in 276inhomogeneities, determined 274samples, ESR analysis 264separation 177states, identification 253, 267-structure analysis, Miissbauer

spectroscopy 287Magnetic anisotropy, determined 272-273Magnetic bubble material, backscattering

spectrum 631Magnetic contrast 506, 676Magnetic domain motion, studied by x-ray

topography with synchrotron radiation ..365Magnetic field

effect in ESR 254mass analyzers, in gas mass

spectrometers 153-154oscillating, wave theory of 83strength, in ESR analysis 253, 685structural changes as function of .420

Magnetic hyperfine interactions, transitionsand relative line intensities 293

Magnetic inhomogeneities 274-275Magnetic interaction, in Mossbauer effect. .293Magnetic materials, FlMIAP study of 583Magnetic methods, capabilities of. 380Magnetic phase diagrams, ferromagnetic

resonance 268Magnetic resonance. See also Electron spin

resonance; Resonance methods.defined 676field " 690linewidth, symbol for. 692principles of 254

Magnetic spectrometer, and detector, EELSanalysis .435

Magnetic structuredetermined by neutron diffraction .420refined by Rietveld method .423

Magnetic switching, use in spark source massspectrometry 144

Magnetism, conversion factors 686Magnetite, flame emission sources for 29-30Magnetization

abbreviation for 690determined 271-272effective 275, 690as ferromagnetic resonance

application 271-272FMR measurement of 267net nuclear 280saturation, as function of concentration 272temperature dependence 273

Magnetocrystalline aniosotropy, FMR studyof. " 267

Magnetometersdefined 676vibrating sample, abbreviation for 691

Magneton, defined 676Magnetostriction, defined 676Magnetostrictive alloy, SAM analyzed 510Magnetostrictive methods, capabilities of ..380Magnets

Chromidur ductile permanent, FIMIAPanalysis of 598-599

in gas mass spectrometers 153-154mass analyzer 153-154saturation 255in Zeeman-corrected spectrometer. 52

Magnificationabbreviation for 690defined 676effect, image analysis 313-314effect on inclusion volume fraction, image

analysis 314field ion microscope 588symbol for 692

Magnitude of strain, as x-ray diffractionanalysis 325

Major component analysisanalytical transmission electron

microscopy .429-489atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential

coulometry 202, 207-211electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis 516-535electron spin resonance 253-266elemental and functional group

analysis 212-220field ion microscopy 583-602gas analysis by mass spectroscopy 151-157gas chromatography/mass


spectroscopy 31-42infrared spectroscopy 109-125of inorganics .4-6, 7, 8ion chromatography 658-667liquid chromatography 649-657low-energy ion-scattering

spectroscopy 603-609molecular fluorescence spectrometry 72-81Mossbauer spectroscopy 287-295neutron diffraction .420-426optical emission spectroscopy 21-30of organics 9, 10particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187Raman spectroscopy 126-138Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627spark source mass spectrometry 141-150ultraviolet/visible absorption

spectroscopy 60-71voltammetry 188-196x-ray diffraction 325-332x-ray photoelectron spectroscopy 568-580x-ray powder diffraction 333-343x-ray spectrometry 82-101

Mandelic acid, as narrow-range precipitant 169Manganese

complexation titration for 174-copper alloys, isolation of manganese in 174determined by controlled-potential

coulometry 209determined in stainless steel 146evaporation fields for. 587ICP-determined in plant tissues .41interference with copper 201in iron-base alloys, flame AAS analysis

for 56isolation of ferromanganese in 174isotope composition and intensity 146photometric analysis methods 64redox titration 175segregation, in dual-phase steels .483species weighed in gravimetry 172TNAA detection limits 237volumetric procedures for 175weighed as the phosphate 171in zirconium alloys, by periodate method ..69

Index /729

Manganese dioxide, sulfur dioxide removal inhigh-temperature combustion by 222

Mapping. See also Dot mapping; Elementalmapping; X-ray maps.

analog 525-528chemical state, Auger electron

spectroscopy 555-556compositional, electron probe x-ray

microanalysis 516, 525-529two-dimensional topographic 372

Marion-Cohen technique, plane-stress elasticmodel 384

Martensite decomposition in uraniumalloys 316

Massconversion factors 686measurements, GC/MS analysis 642-643minimum detectable, abbreviation for 690numbers, isotopes 688resolution, LEISS analysis 605SI base unit and symbol for 685vs x-ray production, PIXE analysis 104

Mass absorptioncoefficients 85, 99, 676vs wavelength, absorption edges as

discontinuities in 85vs x-ray energy, copper 85, 87in x-ray spectrometry 84

Mass analysisanalytic methods .4-5, 7, 8, 9, 10gas analysis by 151-157

Mass analyzer, in gas massspectrometer 153-154

Mass density, SI derived unit and symbolfor 685

Mass discriminationcorrected by Einzel lens system 155in gas mass spectrometer. 153

Mass filter, quadrupole, in gas massspectrometer 153

Massmann graphite furnace atomizers .49Mass measurements

gas analysis by mass spectrometry ... 151-157gas chromatography/mass

spectrometry 639-648low-energy ion-scattering

spectroscopy 603-609Rutherford backscattering

spectrometry 628-636secondary ion mass spectroscopy 610-627spark source mass spectrometry 141-150

Mass memory, use in x-ray spectrometry ....92Mass peak, defined for gas mass

spectrometer 155Mass resolution. See also Resolution.

LEISS analysis 605Mass scale

atom probe, calibration of 592RBS energy scale as translated into 629

Mass spectraatom probe, of IN 939 599atom probe microanalysis,

interpretation 591-593Mass spectrometers

defined 151spark source 142time-of-flight 142

Mass spectrometrycapabilities 212, 226, 649capabilities, compared with IR

spectroscopy 109defined 676gas analysis by 151-157and high-performance liquid chromatography,

use with GC/MS " 645-646-isotope dilution, capabilities 243laser-induced resonance ionization 142and mass spectrometry, and gas

chromatography 646-647



730/ Index

Mass spectrometry (continued)for molecular structure 116spark source 141-150

Mass spectrometry/mass spectrometryblock diagram of spectrometer system

for 646nonvolatile compound analysis 639

Mass spectroscopy. See Mass spectrometry.Mass spectrum

atom probe 591, 592collision-activated dissociation 647complex, atom probe microanalysis ..591-592defined 676ethyl alcohol 640in gas analysis 151, 155naphthalene 643pentachlorobiphenyl 642scanning modes, gas mass spectrometers .. 154tabulated output, for GC/MS analysis of

extracted shale oil 643Match/search methods, for unknown phases or

particles .455-459Materials characterization

defined 1Handbook articles, organization of 1introduction 1qualitative chemical tests 168sampling for '" 12-18tandem methods of. 1

Materials sciencemicrobeam analysis strategy for. 529-530NAA application in 234PIXE studies in semiconductor industry 107

Material transformations 376, 566Matheson standard gas sample 155Matrix. See also Matrix effects.

absorption, as XRPD source of error 341complex, non trace components in 109defined 676methods, for quantitative IR analysis 117sample 83, 162, 168-170

Matrix effects. See also Interferences.in AFS .46!n e.mis.sion spectroscopy 33In tItamum .. '" 97in x-ray spectrometry 97

Matrix isolation, defined 676MAX, as synchrotron radiation source .413MAX-D index, use for unknown phase! particle

identification .456Maximum, abbreviation for 690MeA. See Multichannel analyzers.ME. See Mossbauer effect.Mean-free-path damping, EXAFS

analysis .410Mean linear intercept measure, grain

size 358Measure

angular, symbol for 691SI standardized 685units of 691

Measured cell potential, abbreviation for 690Measurements of film thickness. See Film

thickness measurements.Measurements of thickness. See Thickness

measurements.Mechanical deformation. See also

Deformation.effect on texturing 358

Mechanical polishing. See also Polishing.Raman analysis of 133

Medical analysiselemental content in toxicology,

epidemiology, PIXE analysis 102and materials characterization 1voltammetric monitoring of metals and

nonmetals in 188Mediums, for sample

dissolution 165, 166, 168

Merr• See Effective magnetization.Meinhard nebulizer, for analytic ICP

systems 35Meltable solids, as IR samples 112-113Membrane filters, for sample preparation ...94Membrane potential, ion-selective

electrode 182Membrane-type ion chromatography

suppressor 660Memory, mass " 92Memory effects

furnace atomizers .49ultrasonic and fritted disk nebulizers 36

Meniscus, reading level of 172Mercuric iodide detectors, capabilities 95Mercuric oxide, on mercury film electrode,

Raman spectroscopy 136Mercurous bromide and chloride, on mercury

film electrode, Raman analysis 136Mercury

anodic attack of 204cathodes, in electrogravimetry 199-200determined by controlled-potential

coulometry 209effect in dropping mercury electrode " 189as electrode in voltammetry 189, 191in furnace atomizers .49lamp sources, spectral output of 76quartz-tube atomizers for .49species weighed in gravimetry 172sulfuric acid as dissolution medium 165TNAA detection limits 238vapor detection, atomic absorption

spectrometry for .43volumetric procedures for 175weighed as the chloride 171weighed as the sulfide 171

Mercury cathodes 170, 199-200Mercury pump, Toepler pump as 152Mercury switch, analysis of surface films on

electrical contacts in 578-579Metabolites, GC/MS analysis of 639Metal alloys

composition determined by ICP-AESanalysis 31

microstructural changes studied by x-raytopography 366

Metal-bearing ores, photometric methods foranalysis 64

Metal/ceramic brazing assembly interface,molybdenum particles on .457

Metal coatings. See Coatings.Metal-gas interfaces 136Metal ions, determination of 197,200-201Metallic glasses

defined 676Knight shift measurements on 284SAS applications .405

Metallic nickel, partitioning oxidation statesin 178

Metallized ceramic, electron diffractioniEDSanalysis for unknown phases in ... .457-458

Metallochromic indicators, common ..... 174Metallographic identification

of cellular decomposition of martensite inuranium alloy 316

of light elements 549, 559-561optical metallography 299-308

Metallographic sections, macroscopyof 303-304

Metallography 517,676Metalloids, implantation of .485Metallo-organic chemical vapor

deposition 601,602,690Metalloproteins, EXAFS structural analysis

of. .407Metal oxides

particles, separation in high-temperaturecombustion 222

Raman analysis of 130-135surface films, XPS determined oxidation

states in 568Metal pipe, sampling trainload for percentage

of alloying element 15Metals. See also Metals and alloys,

characterization of.in alloys, electrogravimetric

determination 197analytic methods for. .4carbon in, determined by high-temperature

combustion 221-225controlled-potential coulometry for 202corrosion analysis of 134-135crystallographic texture measurement and

analysis 357-364deposition of small amounts 198detecting adsorbed monolayers on 114determined fluorimetrically by

complexation 74effect of oxygen on positive secondary ion

yields in 612FIMiAP study of point defects in 583finished, AAS analysis of .43fluorescent, MFS analysis 72-gas environments, SERS for 137high-purity, voltammetric analysis 188implantation of .485liquid, electronic structure of 284microgram amounts, electrogravimetric

measurement. 197multiphase, image analysis of 309non-, Raman analysis of surface species

of. 134perchloric acid as dissolution medium 166on periodic table 688photometric methods for analysis 64precious, SSMS analysis in geological

ores 141prompt gamma activation analysis of 240samples, treatment in mineral acids 165sampling of 12-18SAS applications .405SIMS analysis of surface layers 610SIMS phase distribution analysis in 610single-phase, image analysis of. 309small-angle scattering analysis .405in solutions, concentration range of 188spark source excitation for elemental analysis

of. '" 29sulfur in, determined by high-temperature

combustion 221-225surfaces, FIMiAP study of 583surfaces, IR study of monolayers adsorbed

on 118-120use of ICP-AES for trace impurities in .....31weighing as the, gravimetric

analysis 170-171x-ray diffraction residual stress techniques for

crystalline 381Metals and alloys, characterization of. See

also Alloys; Alloys, specific types; Metals.analytical transmission electron

microscopy .429-489atomic absorption spectrometry 43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211crystallographic texture measurement and

analysis 357-364electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis .. .516-535electron spin resonance 253-266extended x-ray absorption fine

structure .407-419ferromagnetic resonance 267-276field ion microscopy 583-602



inductively coupled plasma atomic emissionspectroscopy 31-42

inert gas fusion 226-232low-energy electron diffraction 536-545low-energy ion-scattering

spectroscopy 603-609Mossbauer spectroscopy 287-295neutron activation analysis 233-242neutron diffraction .420-426nuclear magnetic resonance 277-286optical emission spectroscopy 21-30particle-induced x-ray emission 102-108potentiometric membrane

electrodes 181-187radial distribution function

analysis 393-401radioanalysis 243-250Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627single-crystal x-ray diffraction 344-356small-angle x-ray and neutron


spectroscopy 60-71voltammetry 188-196x-ray diffraction residual stress

techniques 380-392x-ray diffraction 325-332x-ray photoelectron spectroscopy 568-580x-ray powder diffraction 333-343x-ray spectrometry 82-101x-ray topography 365-379

Metals Data File 355-356Metatorbernite, and turquoise, ESR

analysis 265Meter 685, 691Methane, analyzed in microcircuit fabrication

process 157Methanol

absolute, to isolate inclusions from steel .. 176and iodine, second-phase test methods .... 177

Methods based on sputtering or scatteringphenomena

atom probe microanalysis 583, 591-602field ion microscopy 583-.591, 598-602low-energy ion-scattering

spectroscopy 603-609Rutherford backscattering

spectrometry 628-636secondary ion mass spectroscopy 610-627

Methylene, stretching vibrations 111Methylisobutyl ketone, solvent extraction

with 169Methyl orange, as acid-base indicator. 172Methyl red, as acid-base indicator 172Methyl thymol blue, as metallochromic

indicator 174Metric conversion guide 685-687Metrology, image analysis use 316MFS. See Molecular fluorescence spectroscopy.Mica, grain size of silver film grown

on 543-544Micelle, defined 676Michelson interferometer 39, 112Microabsorptions, as XRPD source of

error 341Microanalysis. See also Microanalysis, methods

for.atomic probe '" 583,591-602basic concepts, EPMA analysis 517-518chemical analysis and microscopy in 517chemical, at atomic level, FIMJAP for 583of crystal structure, inorganic solids,

analytical methods for .4-6of defects, inorganic solids, analytical

methods for .4-6

defined 676elemental, of inorganic solids, analytical

methods for .4-6for inhomogeneous compositional

structures 529of inorganic solids, analytical methods

for .4-6of morphology, inorganic solids, analytical

methods for .4-6of phase distribution, inorganic solids,

analytical methods for .4-6of phase identification, inorganic solids,

analytical methods for .4-6spatial resolution in 525x-ray, in analytical electron

microscopy .446-449x-ray, of diffraction-induced grain-boundary

migration .462Microanalysis, methods for. See also

Microanalysis.analytical transmission electron

microscopy .429-489Auger electron spectroscopy 549-567crystallographic texture measurement and

analysis 357-364electron probe x-ray microanalysis 516-535field ion microscopy 583-602image analysis 309-322low-energy electron diffraction 536-545optical emission spectroscopy 21-30optical metallography 299-308particle-induced x-ray emission 102-108radial distribution function analysis 393-401Raman spectroscopy 126-138scanning electron microscopy .490-515x-ray powder diffraction 333-343x-ray topography 365-379

Microballoons, glass, ion chromatographyanalysis of 665-667

Microbeam analysis. See also Electron probex-ray microanalysis.

applicability 529applying, electron probe x-ray

microanalysis 529-530compositional gradients 530and line broadening analysis 374multiphase samples 529-530sample preparation 529-530sampling strategy 529-530

Microcircuit process gas, analyzed 156-157Microcomputers

-based data systems, for Ramanspectrometers 128

effect on x-ray spectrometry 83Microdensitometer

spark source mass spectrometry 143for topographic intensity profiles 372

MicroditTraction, defined 438-439MicroditTractometer 338Microelectrogravimetry, conduction of 200Microelectronics, AES in-depth surface

analyses for 549Micrograph 302, 676Microphase separation, SAS techniques

for .405Micropolishing. See also Polishing.

as FIM sample preparation 584Microprobe

analysis, NBS standards for 530Auger, of gold-plated stainless steel lead

frame 560electron, capabilities 161ion, capabilities 161laser Raman molecular 129proton, and PIXE analysis 107

Microsampling, infrared 116Microscopes. See also Scanning electron

microscopes; Transmission electronmicroscopes.

Index /731

analytical electron .430-432defined 676detectors and image formation in .492direct-imaging ion 613field ion 584infrared 116ion 614SEM .491-494upright, with image analyzers 310

Microscopic stress. See also Microstresses.defined 676

Microscopydefined 676residue analysis by 177

Microsecond, symbol for 692Microsiemen, as common ion chromatography

unit 659Microstresses

associated with cold working 386determined 380, 386-387states analyzed .424in x-ray diffraction residual stress

techniques 380, 381Microstructural AEM analysis of ion

implanted alloysimplantation of two species: ternary

alloys .486inert elements, implantation of .485-486metalloids, implantation of .485metals, implantation of .485precipitation .485-486radiation-induced changes .484sample preparation .484thermal treatments .486-487

Microstructural analysisin atomic detail. 583EPMA compositional analysis of phases

at 516field ion microscopy and atom probe 583of ion-implanted alloys .484use of stereological relationships 309x-ray topography 366

Microstructurecrystallographic texture measurement and

analysis for 358of ion-implanted alloys, AEM

determined .484-487and magnetic properties, FlM/AP analysis of

relationship 599stereological parameters to determine

influence of processing on 316surface, LEED analysis of. 536weld metal, AEM interpretation .478-481

Microtomes, for specimen preparation, ATEManalysis .452

Microwaveabsorption intensity, in ESR analysis 253losses, FMR determination of 267radiation, defined 676-677spectrometers, in FMAR measurements in

transmission 272spectroscopy, capabilities 253

Microwave radiation, defined 676-677Microwave-resonant cavity

modes 256power reflected, as function of frequency 256

Middle-infrared radiation, defined 677Migration

diffusion-induced grain-boundary, EDS/CBEDanalysis of. .461-464

electrical, in voltammetry .. " 189Miller index

of crystallographic direction 359single-crystal analysis 346unit meshes and two-dimensional 537

Millingsample, for chemical surface studies ..... 177as wet chemical technique for subdividing

solids 165



732/lndex

Milliprobe, for historical studies, PIXEanalysis 107

Mineral acids, sample dissolution in 165Mineral quartz, XRPD analysis 341Minerals. See also Minerals. characterization

of.analytic methods applicable 6crystallinity characterized by electron spin

resonance 253with defects, ESR studied 264effects of composition on mass

absorption 97EXAFS analysis of. .407sample dissolution mediums 166sampling of 12-18

Minerals, characterization of. See alsoMinerals.

analytical transmission electronmicroscopy 429-489

atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis 516-535electron spin resonance 253-266extended x-ray absorption fine



spectroscopy 603-609molecular fluorescence spectrometry 72-81Mossbauer spectroscopy 287-295neutron activation analysis 233-242neutron diffraction .420-426optical emission spectroscopy 21-30particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187radial distribution function analysis 393-401radioanalysis 243-250Raman spectroscopy 126-138scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627single-crystal x-ray diffraction 344-356spark source mass spectrometry 141-150ultraviolet/visible absorption

spectroscopy 60-71voltammetry 188-196x-ray diffraction 325-332x-ray powder diffraction 333-343x-ray spectrometry 82-101

Miniboat. See L'vov platform.Minicomputers, for image analysis 310Minitorches, for the ICP 37Minor component analysis

analytical transmission electronmicroscopy '" .429-489

atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis 516-535electron spin resonance 253-266elemental and functional group

analysis 212-220field ion microscopy 583-602gas analysis by mass spectrometry 151-157gas chromatography/mass


spectroscopy 31-42

infrared spectroscopy 109-125of inorganic gases, analytical methods for ...8of inorganic liquids and solutions, analytical


for .4-6ion chromatography 658-667liquid chromatography 649-657low-energy ion-scattering

spectroscopy 603-609molecular fluorescence spectrometry 72-81neutron activation analysis 233-242neutron diffraction .420-426optical emission spectroscopy 21-30of organic solids and liquids, analytic methods

for 10of organic solids, analytical methods for 9particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187Raman spectroscopy 126-138Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627spark source mass spectrometry 141-150ultraviolet/visible absorption


Mirror plane, defined in crystal symmetry ..346Miscibility, SAS techniques for .405Misorientation determination, in dislocation

cell structure analysis .471-472Mixtures

acid, nonoxidizing, sample dissolutionby 165

composition determined 213determination of molecular components

in 109interpreting spectra of 116liquid chromatography isolation of pure

compounds from 649matrix methods to analyze complex 117organic and inorganic, gas analysis of 151oxidizing acids, sample dissolution by 166separation and component analysis by liquid

chromatography 649of volatile compounds, GC/MS analysis

of. 639M lines, emission 86Mobile carbon, determined in iron and

steels 178Mobile nitrogen, determined in steels 178Mobile phase, defined 677Mobile phase programming, functional group

analysis 654MOCVD. See Metallo-organic chemical vapor

deposition.Modulation

in ESR spectrometer 255polarization 114-115

Modulus of elasticityabbreviation for 690anisotropic 358defined 677in stress measurement 382variance with preferred orientation 358

Mohr's circle for stress 381Mohr titration

for chloride 173defined 164

Moietydefined 677multielement, classical wet analysis of. 162

Moire fringes 371, 677Moire pattern, defined 677

Moistureas contaminant in microcircuit process

gases 156-157removal in high-temperature combustion ..222and sampling 16

Molality, defined 677Molar absorptivity, in UVIVIS analysis ..62-63Molar extinction coefficients .47Molarity

defined 162, 677and titrant standardization 172

Molds, use in solid sample preparation 93MOLE. See Molecular optical laser examiner.Mole 677, 685, 690Molecular absorption

Jablonsky diagram indicating 73as requirement for fluorescence 73-74

Molecular analysesof bulk inorganic solids, analytical methods

for 6of inorganic gases, analytical methods for 8of inorganic liquids and solutions, analytical

methods for. 7IR quantitative determination, in

mixtures 109of organic solids and liquids, analytical

methods for. 10of organic solids, analytical methods for 9Raman spectroscopy 126-138

Molecular bandsin emission spectroscopy 23in flame emissions 29

Molecular-cage effect, XANESanalysis .415-416

Molecular conformation, and stereochemistry,IR determination of 109

Molecular emissionminimizing 23in optical emission spectroscopy 22-23

Molecular flow, defined 152Molecular fluorescence spectroscopy 72-81

applications 72, 79-81capabilities, compared with UVIVIS

analysis 60defined 677detection limits and dynamic range 76estimated analysis time 72excitation and emission spectra, qualitative

analysis 74-75fluorescent molecules 73-74general uses 72indirect, of nonfluorescing atoms,

molecules 76of inorganic and organic materials .. .4-5, 7-10instrumentation 76-77introduction and theory 73lasers 76, 80-81limitations 72, 76monochromators 76-77possible errors 77-78practical considerations 77-78quantitative analysis 75radiation sources 76related techniques 72, 78-79samples " 72,76,79-81special techniques 78-79

Molecular hydrogen lamp, for continuous-source background correction 51

Molecular light-scattering processes, energy-level diagram for 127

Molecular optical laser examinerinstrument layout for 130for Raman spectroscopy 129-130use in glasses 131

Molecular orientationin drawn polymer films 120IR determination of 109

Molecular reorientation, as NMR kineticprocess 277



Molecular scattering, by Ramanspectroscopy 126-130

Molecular species, as adsorbed onsurfaces 109

Molecular spectrum, defined 677Molecular structure

balls and massless springs model 110, 111compound, IR spectroscopy for 109defined 677determined by single-crystal analysis 345mass spectrometry for 116nuclear magnetic resonance 116in UVIVIS analysis 61

Molecular vibrationsof diatomic molecule 111group frequencies as 111in infrared spectroscopy 111normal-coordinate analysis 110-111with Raman spectroscopy 126-138

Molecular weight, defined 677Molecules

adsorbed, on smooth metal surfaces, SERSanalysis of 137

adsorbed, orientation on single crystals .. .407aggregate, in complexometric titrations 164aromatic, in ESR analysis 259chemisorbed, EXAFS geometry of .407defined 677diatomic, molecular vibrations 111electronic structure, UVIVIS analysis 60and emission spectroscopy 22-23functional groups in 109gas, three-dimensional structure of 393inorganic, MFS analysis 74interactions between, determined by single-

crystal x-ray diffraction 344odd electron, ESR analysis of 254organic and inorganic fluorescent " 72-74organic, UVIVIS analysis of functional

groups in 60with overlapping fluorescence spectra 75polarization of 127polymer, SAS applications .405surfactant, in water, structural changes

in 118symmetry of 348

Mole, equivalence of. 162Molten salts, analysis 131Molybdena catalysts, analyses 134Molybdenum

crystal, x-ray fractography for fracture surfaceof. 377


determined in molybdenum-tungstenalloys 207

epithermal neutron activation analysis 239evaporation fields for. 587gravimetric finishes 171implanted in aluminum .484interfacial segregation studies in 599-60Iin iron-base alloys, flame AAS analysis

of. '" 56Jones reductor for. 176neutron and x-ray scattering, and absorption,

compared " .421particles, on metal/ceramic brazing assembly

interface " .457photometric analysis methods 64qualitative tests to identify 168with sodium samples, epithermal neutron

activation analysis of 239species weighed in gravimetry 172TNAA detection limits .. '" 237volumetric procedures for 175

Molybdenum alloys, FIM sample preparationof. 586

Molybdenum carbides, quantitative effect ofcarbon KVV spectra in 553

Molybdenum oxide catalysts, Ramananalysis 133

Molybdenum-rhenium alloys, polycrystalline,bend contours in .445

Monochromatic beams, single-crystaldiffraction methods 329-330

Monochromatic, defined 677Monochromatic reflection topography 366Monochromators

for atomic absorption spectrometry and relatedtechniques .44, 50-52

crystal, for neutron diffraction .422Czerny-Turner design 23, 38defined 677dispersive infrared IIIand flame emission sources 30grating, as wavelength sorting device 23ICP-AES analysis 34for molecular fluorescence

spectroscopy 76-77with molecular optical laser

examiners 129-130scanning 38, 128stray light rejection for single, double,

triple 129Monoclinic unit cells 346-348Monolayers

adsorbed on metal surfaces, examinationof 118-120

Langmuir-Blodgett 120sub-, effect of adsorbed oxygen on

metals .. " " 552top, AES chemical analysis " 551

Monomer, defined 677Monoperoxydodecanedioic acid, ATR, DRS,

and PAS granular analysis of 120Monosubstituted benzene derivatives,

substituent effects on fluorescence quantumyields for. 74

Monte Carlo electron trajectory simulation,of EPMA effects 518

Monte Carlo techniquesfor 20-keV electrons .499defined 677

Morphologyof crystal structure, organic solids, analyses

for " 9grain, topographic methods for 368image analysis for 309-322of inorganic solids, analytical methods

for .4-6molecular structure of organic solids, analyses

for " " 9optical microscope and SEM imaging for 521of organic solids, analytical methods for ....9phase distribution of organic solids, analyses

for " '" 9Mosaic crystal structure, defined 351Mosely's law, representation of .433Miissbauer effect. See also Mossbauer

spectroscopy.abbreviation for 690capabilities 277defined 677as method 287-295sources, principal methods used for

producing 291-292Miissbauer spectroscopy. See also Mossbauer

effect.absorption spectra 294applications 287, 293-295capabilities 253,267,277capabilities, compared with classical wet

analytical chemistry 161defined 677estimated analysis time 287experimental arrangement 293general uses 287introduction and principles 287-293

Index /733

limitations 287for partitioning oxidation states, iron 178related techniques 287selection rules 288sources, principal methods for

producing 291-292spectra components 293transitions, properties of. 289-290

Miissbauer spectrum, defined 677Miissbauer transitions, some properties

of 289-290Mounting

angle 576optical metallography sample, in

Bakelite 300powders, for XPS analysis 575specimens for optical metallography 300

M shell, defined 676Mume furnaces, for sinters and fusions 166Mull preparation, for IR samples 113Multichannel analyzers

defined 677effect in EPMA analysis 519

Multichannel detectorsFellgett's advantage and 129Raman spectrometer with 128

Multielement analysisenergy-dispersive x-ray spectrometry ..82-101simultaneous, ICP-AES as 32, 33

Multielement isotopes, for spark source massspectrometry 145

Multiphase ceramics, SIMS phase distributionanalysis 610

Multiphase materialsimage analysis of 309neutron diffraction analysis .420XRPD-determined weight fraction or

crystalline phases in 333Multiple-expansion volume introduction

system, gas mass spectrometer 152Multiple scattering

effects, in EXAFS analysis .415event, defined 677

Multiplet splitting, in XPS analysis 572Multiplex advantage

in FT-IR spectroscopy 112in Raman spectroscopy 129

Multiplier phototube. See Photomultipliertube.

Murexide, as metallochromic indicator 174Mylar, transmission by 100

Nn. See Refractive index.N. See Normal solution.N-I00, as synchrotron radiation source .... .413NAA. See Neutron activation analysis.Nanocoulomb, abbreviation for 691Nanogram, abbreviation for 691Nanometer, abbreviation for 691Nanosecond, abbreviation for 691Naphthalene 78, 643Narrowing exchange, as ESR line-broadening

mechanism 255National Bureau of Standards

SRM, microprobe analysis 530Standard Reference Material (NBS SRM) 147

Natural abundance, of isotopes 643Natural gas, analytic method for 11Natural logarithm (base e), abbreviation

for 690Naturally occurring substances, as system

favorable to ESR analysis 263Natural waters. See also Water.

analysis of. .41N-benzoyl-N-phenylhydroxylamine (BPA), as

precipitant. 169



734/ Index

NBS. See National Bureau of Standards.ND. See Normal direction (of a sheet).N(E). See Electron energy distribution.Near-edge structure, determined . .407, 415-416Nearest layer model, Raman vibrational

behavior of intercalated graphites 133Near-infrared

abbreviation for 690radiation, defined 677regions of spectrum, Fr-IR analysis 114

Near-perfect crystal, diffraction in 365-367Near-surface

analysis 126, 133-137defects, single crystals 633stresses, effect of stress gradient correction of

measurement of 388Nebulizers

for AAS and related techniques .44-50for analytical ICP systems 34-36argon gas flow as 34Babington 36concentric 34, 35conductive solids 36, 690corrosion-resistant 35crossflow 34, 35defined 677effects in flame spectroscopy 29efficiency of, defined 35fritted disk 36, 55for ICP-MS .40pneumatic 34-36, 47ultrasonic 36, 55

Needle tissue biopsy, GFAAS detection ofmetals in 55

Neel point. See Neel temperatureNeel temperature, defined 677Negative absorption, fluorescent enhancement

as 98Negative glow, in glow discharges 27Negative ion charge, symbol for 692Negative logarithm of hydrogen-ion activity.

See pH.Neocuproine method, analysis for copper in

iron and steel alloys by 65Neodymium

and praseodymium, separation of 249-250TNAA detection limits 238-YAG lasers 142,597,601

Neodymium-doped yttrium-aluminum-garnet(Nd:YAG) laser 142,597,601

Neonadsorbed, effects of 588as image gas, for FIM analysis of

semiconductor 601,602as imaging gas, FIMJAP analysis of

permanent magnet alloy 599ionization potentials and imaging fields

for 586Neptunium, determined by controlled-potential

coulometry 209Nernst equations 197, 208Nessler tubes, in UVIVIS absorption

analysis 66Neutral filter, defined 677Neutral loss scans, gas chromatography/mass

spectrometry 646-647Neutron absorber, defined 677Neutron absorption, defined 677Neutron activation analysis 233-242

14-MeV fast neutron activation analysisas 239

applications 233, 240-241basic principles and introduction 234capabilities, compared with PIXE 102defined 677epithermal neutron activation analysis as ..239estimated analysis time 233of inorganic liquids and solutions, information

from 7

of inorganic solids, information from .4-6limitations 233neutron sources 234nondestructive thermal neutron activation

analysis as 234-238of organic liquids and solutions, information

from 10of organic solids, information from 9prompt gamma activation analysis

as 239-240radiochemical (destructive) TNAA

as ~ ~38-239related techniques v- .' ••• ',' : '.••233samples 233<2,36, 240-241as trace-element assay ,,:, ";\~i" ,,," ..233uranium assay by delayed-neutron'<-,' \'. I

counting 238,239Neutron capture. See also Neutron

absorption.prompt "(-ray activation analysis 239~:240

prompt "V-rays ,.. ,234slow or thermal ;,.\ ~34

Neutron cross section, defined. : ' ~Z8Neutron detector, defined 6/8Neutron diffraction .420-426

applications .420, 425-426capabilities 333, 365,407defined 678detection for .422general uses , . .420introduction .421limitations '.. .420monochromators .413neutron powder diffraction .422-423neutron production .421-422pole figure .423-424related techniques 420residual stress .424Rietveld method .423samples .420, 422-423single-crystal .424-425single-crystal capabilities 344texture measurements 357,423-424two modes of .422

Neutron flux, defined 678Neutron powder diffraction. See also Neutron

diffraction.data, Rietveld refinement of 344instrumentation .422Rietveld method .423samples .422-423

Neutron powder diffractometers, schematic,with multidetector bank .422

Neutrons. See also Neutron diffraction.14-MeV, for FNAA 239capture, slow or thermal, in NAA 234cross section, defined 678defined 677delayed 238detector for, defined 678effect of low absorption .423epithermal 234high-energy, use for assay measurement ..234-irradiated ores, "V-ray spectrum of 235production for neutron diffraction .421-422reactions, in NAA 234sources for NAA 234sources, radial distribution function

analysis 395spallation sources .421

Neutron scattering, and x-ray scattering,compared .421

Neutron spectroscopy, defined 678Neutron spectrum, defined 678Neutron topography, capabilities 365Newton 685, 691NGR. See Nuclear gamma-ray resonanceNibbling, as wet chemical technique for

subdividing solids 165

Nickel. See also Nickel-base alloys; Nickel-basealloys, specific types.

bismuth in, GFAAS analysis 57and cobalt, corrosion in aqueous alkaline

media 135concentration vs intensity plot for. 99controlled-potential electrogravimetry of ..200in copper alloys, by dimethylglyoxime

method 66determined by controlled-potential

coulometry 209determined in samples containing chloride

ions 201determined in stainless steel 146diffusion into iron, measurement of 243direct-current and differential pulse

polarograms of 194dominant texture orientations 359electronic, analysis for aluminum in 65epithermal neutron activation analysis 239evaporation fields for. 587EXAFS scan using synchrotron radiation . .408gravimetric finishes 171high-purity, "V-ray spectrum 240hydride-generation AAS system for 50ICP-determined in silver scrap metal .41-implanted aluminum .485impurities determined in 240intensity vs concentration, x-ray

spectrometry 99in iron-base alloys, flame AAS analysis 56isolation in high-temperature alloys 174isotope composition and intensity 146K-edge .414, 416metallic, partitioning oxidation states in ... 178neutron and x-ray scattering, and absorption,

compared ....................•.... .421-nickel pair, phase and envelope function

for .414normalized, K-edge EXAFS plotted .417organic precipitant for 169-phosphorus film, extent of coverage on

platinum substrate 608photometric analysis methods 64qualitative tests to identify 168as sample modifier, GFAAS analysis 55support of SERS in vacuum 136titration, with cyanide 174trace-element concentrations 194, 240volumetric procedures for 175weighed as the dimethylglyoxime

complex 171x-rays, effects of absorption/enhancement

on 97Nickel-base alloys. See also Nickel; Nickel-base

alloys, specific typesAAS furnace atomizer for trace analysis

in , 55AEM determined orientation relationships

in .454age-hardened, FIMJAP study of precipitates

in 583amorphous, NMR Knight shifts 284bulk composition of 562dendritic solidification structure in 306diffraction techniques, elastic constants, and

bulk values for 382FIM sample preparation of 586grain-boundary compositions 562hydrogen peroxide dissolution medium 166isothermal section, AEM determined .475LEISS depth profile 609ordered, effect of antiphase boundaries on

FIM image 589, 590ordered Ni-Mo, effects of antiphase

boundaries on FIM image 589-590pulse-fraction curves for atom probe

analysis 595trace analysis for aluminum in 66



Nickel-base alloys, specific types. See alsoNickel; Nickel-base alloys.

Hastelloy C-22, AEM-determined orientationrelationships .454

Hastelloy C-22, weld soundness in .. .478-481Incoloy 901, diffraction techniques, elastic

constants, and bulk values for 382Inconel 600, 'chromium sensitization in .. .483Inconel 600, diffraction techniques, elastic

constants, and bulk values for. 382Inconel 600 tubing, residual stress and percent

cold work distributions 390Inconel 600 tubing, residual stress and cold

work distribution 390Inconel 625, chemical composition as function

of etching time 559Inconel 625, corrosion rate 558Inconel 718, diffraction techniques, elastic

constants, and bulk values for 382Inconel 718, x-ray elastic constant

determination for 388Inconel X-750, diffraction technique, elastic

constants, and bulk values for. 382Rene 96, diffraction techniques, elastic

constants, and bulk values for. 382U-700, continuous grain-boundary precipitate

in 308Nickel-base superalloys

high-resolution energy-compensated atomprobe analysis of 597

phase chemistry and stability in 598pulse-fraction curves 594, 595

Nickel-base superalloys, specific typesIN 939, atom probe mass spectra of 'Y matrix

and primary 'Yprecipitates 598IN 939, chemical analysis of ultrafine

secondary preciptates 598IN 939, composition of 598IN 939, FIM and TEM images of 598IN 939, FIMIAP analysis of 598IN 939, four-stage heat treatment of. 598IN 939, 'Y phase analysis 598IN 939, ladder diagrams 599Nimonic 90, lAP study of 596

Nickel-phosphorus film, LEISS determinationof coverage on platinum substrate 608

Nicol prism, defined 678Nier-type ion source, in gas mass

spectrometer 153Niobium

evaporation fields for. 587gravimetric finishes 171ores, fusion flux for 167ores, hydrofluoric acid as dissolution

medium 165NIR. See Near-infrared.Nital

as etchant 316, 318and picral, etchants compared 302

Nitratesanions, separation by ion

chromatography 659as electrodes 185

Nitric acidwith hydrochloric acid, as sample dissolution

medium 166as oxidizing sample dissolution medium .. 166residue isolation using 176as sample modifier, GFAAS analysis 55solution, as eluent for suppressed

chromatography 660volatility 166

Nitric oxide, SERS analysis of. 136Nitrides, as inclusions 176Nitriding surface, chemical studies of 177Nitriloacetic acid, detected by ion

chromatography 661Nitrite anions, separation by ion

chromatography •...................659

Nitrogenanalyzed in microcircuit fabrication

process 156-157chemistry at surfaces, AES analysis of. ...553combustion method for elemental analysis

of. 214determined by combustion 214determined by potentiometric membrane

electrodes 181exclusion in de arc sources 25-fired fracture surface, XPS survey of 577gas mass analysis of. 155in high-purity metals, biamperometric analysis

for 205inert gas fusion system for

detecting 226, 228-231in inorganic solids, applicable analytical

methods .4, 6Kjeldahl determination of 172, 214mobile or interstitial, determined in

steels 178in organic substances, ISE analysis 186photometric analysis methods 64prompt gamma activation analysis of 240volumetric procedures for 175in weld relay, gas mass spectroscopy of .. 156

Nitrogen dioxide, SERS analysis of 136Nitrogen peroxide, SERS analysis of 136Nitrous oxide-acetylene names 29, 48NMR. See Nuclear magnetic resonance.Noise

defined 678elimination, ESR spectrometers 257thermal, defined 683

Nondestructive analysisneutron activation analysis 233-242surface residual stress measurement, for

quality control 380thermal neutron activation 234-238thin/thick samples, PIXE as 102uranium assay by DNC as 238by voltammetry 188x-ray topography 365-379

Nondestructive thermal neutron activationanalysis, as common NAAanalysis 234-238

Nonferrous alloysdiffraction techniques, elastic constants, and

bulk values for 382glow discharges for 28

Nonmetallic elements, partitioning oxidationstates in 178

Nonmetalsanalysis of surface species 134concentration range of voltammetric

analysis 188on periodic table 688Raman analysis of surface species on 134

Nonoxidizing acids, sample dissolutionby 165-166

Nonrefractory metals, effects of lowered SIVin 588

Nontarnishing ammonia solution, brass alloySCC environment tested in 563-564

Nontransparent samples, surfacescharacterized 70-71

Nonvolatile liquids, as IR samples 112Normal-coordinate analysis

diatomic molecule 111infrared spectroscopy 110-111results 111

Normal direction (of a sheet), abbreviationfor 690

Normalityin analytical chemistry 162defined 678and titrant standardization 172

Normal phase chromatograms, liquidchromatography 652

Index /735

Normal-phase chromatography 652defined 678

Normal pulse polarography, as improvedvoltammetry " .193

Normal solution, abbreviation for 690Notation, x-ray and spectroscopic 569N-phenylbenzo-hydroxamic acid, as solvent

extractant 170N-phenyl carbazole, absorption and

fluorescence emission spectra 75NQR. See Nuclear quadrupole resonance.N shell, defined 677NSLS, as synchrotron radiation source .413Nuclear charge. See Atomic number.Nuclear cross section (IT), defined 678Nuclear fuels, assays of 207Nuclear gamma-ray resonance, acronym ..689Nuclear magnetic resonance 277-286

applications 277, 282-286basic equation of 279Bloch equations (T, and Tz) 280capabilities 287, 649capabilities, compared with infrared

spectroscopy 109defined 678ESR, IR, and UV, compared with 265estimated analysis time 277experimental arrangement. 281-282ferromagnetic nuclear resonance 281general uses 277inorganic applications 7, 282-283introduction and principles 277-281Knight shift measurements, metallic

glass 284magic-angle spinning, capabilities .407for molecular structure 116nuclear quadrupole resonance 281organic applications 9, 10, 285-286polyimide resin analysis 285pulse-echo method 281related techniques 277samples 277,282-286sensitivity 281

Nuclear materials, radioactive elementsdetermined in 243

Nuclear-polarization techniques, and doubleresonance 258

Nuclear properties, of elements 278-279Nuclear quadrupole resonance 281, 689Nuclear reactors 233, 459Nuclear structure, defined 678Nuclear waste ceramic forms, EPMA study

of 532-534Nucleation

in age-hardening materials, FIMIAP studyof. 583

in metals, by SAXSISANSISAS .402SAS techniques for .405theories, and isothermal phase

transformations 317Nucleic acids, ESR studies of 264Nuclei, properties of. 277-278Nuclide, defined 678Numerical aperture, defined 678

oOak Ridge Thermal Ellipsoid Program

(ORTEP), to illustrate crystalstructure 352, 354

Objective, defined 678Ocular. See Eyepiece.OD. See Outside diameterODF. See Orientation distribution functionODMR. See Optical double magnetic

resonance.OES. See Optical emission spectroscopy.



736/ Index

Ohm, as SI derived unit, symbol for 685Ohmic resistance energy loss 199Oils

detection limits of minor elements in 101sulfur determination in 101vegetable, olefinic unsaturarion 205wear metal analysis, optical emission

spectroscopy 21Oil shale, GC/MS analysis of volatile

compounds in 639Oil spills, MFS identification of. 72Olefinic unsaturation in vegetable oils,

electrometric titration determined 205OM. See Optical metal/ographyOne-dimensional analysis, of

defects .465-466Operator fatigue, minimized by image

analysis 309Optical aberrations, ion, in atom probe

analysis 595Optical and x-ray spectroscopy

atomic absorption spectrometry .43-59inductively coupled plasma atomic emission

spectroscopy 31-42infrared spectroscopy 109-125molecular fluorescence spectrometry 72-81optical emission spectroscopy 21-30particle-induced x-ray emission 102-108Raman spectroscopy 126-138ultraviolet/visible absorption

spectroscopy 60-71x-ray spectrometry 82-101

Optical axis, defined 678Optical cells, selection for UVIVIS absorption

analysis 68Optical density, in ion detection 143Optical diagram, Ff-IR spectrometer 112Optical diffraction, and single-crystal x-ray

diffraction, compared 345-346Optical double magnetic resonance, as ESR

supplemental technique 258, 689Optical emission spectroscopy 21-30

applications 21, 29-30and atomic absorption spectroscopy 21Boltzman equation 24capabilities, compared with UVIVIS

absorption spectroscopy 60, 226, 253capabilities, compared with classical wet

analytical chemistry 161defined : 678and direct-current plasma emission

spectroscopy 21electronic structure 21-22electronic transitions 22emission sources 24-26estimated time analysis 21excitation spectra 22general principles 21-23and ICP-AES 21of inorganic solids .4-6introduction 21monochromator 23-24optical systems 23-24polychromator 23-24related techniques 21samples 21of stainless alloy 178-179and x-ray fluorescence 21

Optical laser examiner. See Molecular opticallaser examiner (MOLE).

Optical mask, for echelle spectrometer ..... .41Optical metallography See also Metal/ographic

identification 299-308applications 299capabilities 287,365,429defects observable using 307estimated analysis time 299general uses 299image analysis for morphology 309

of inorganic solids, types of informationfrom .4-6

introduction 299-300limitations 299macroanalysis 301-303microanalysis 304-308of organic solids, information from 9related techniques 299samples 299, 300-301and SEMffEM, compared 299specimen preparation 300-301structure-property relationships established

by 299-300Optical methods. See also Electron optical

methods; Optical and x-ray spectroscopy.capabilities 102

Optical microscopesdepth of field .497with image analyzers 310resolution limits .495-496with SEM imaging, for morphology

studies 521Optical microscopy. See also Electron optical

methods; Optical and x-ray spectroscopy.capabilities .490SAM, SEM, and, compared 509-510

Optical systems. See also Electron opticalmethods; Optical and x-ray spectroscopy.

collection optics 24emission spectroscopy 23-24wavelength sorters 23-24

Opticsbeam-condensing 113collection 24, 128electron, of electron probe

microanalyzer. .432, 517inverted, in wavelength-dispersive x-ray

spectrometers 88Optimum absorbance, in UVIVIS analysis ..68Optoelectronic devices, microanalysis

of 601-602Orange, methyl, as acid-base indicator 172Order

long- and short-range, EXAFSstudied .407, 408

long-range, intermetallic compounds, NMRanalysis 277

long-range, RDF, in amorphousmaterials .393

-order transitions 544Order-disorder

analysis, NMR, in ferromagnetic alloys ...284in ferromagnetic alloys 284-285transitions, LEED analyzed 544

Ordered alloyseffect of antiphase boundaries on FIM

images 589ladder diagrams of 594

Ordered structure .407, 678Ordered systems, EXAFS analysis of ..... .407Ordering

composition profile for 593ferri-, ferro-, antiferro-, or complex magnetic,

by neutron diffraction .420long- and short-range, by neutron

diffraction .420sublattice, in interrnetallic

compounds 283-284Ores

analytic methods applicable 6direct AAS analysis of. .43effects of composition on mass absorption ..97mineral, potentiometric membrane electrode

analysis 181powder or briquet sample preparation, x-ray

spectroscopy 93samples, crushed 165samples, resource evaluations by NAA 233settling, and sampling 14

sodium peroxide fusion for 167treatment in mineral acids 165

Organic acidsconductometric titration of. 203in isopropanolic medium, determined by

electrometric titration 205Organic coatings. See Coatings.Organic complexing agents, determined

fluorimetrically 74Organic composites. See also Composites;

Organic materials; Organic materials.characterization of.

analytic methods for. 9Organic compounds. See also Compounds;

Organic materials; Organic materials,characterization of.

containing nitro groups, assayed bycontrolled-potential coulometry 207

determination of empirical formula of 212direct method for determining crystal

structure of 351EFG analysis for 212elemental analysis 181gas analysis of 151hyperfine splitting in ESR analysis 260identified 213MFS analysis of 73-74NMR analysis of 277UVIVIS analysis of 60

Organic contaminants, removal from XPSsamples 575

Organic gases. See also Gases; Organicmaterials. characterization of.

analytic methods for. 11Organic liquids. See also Liquids; Liquids.

characterization of; Organic materials,characterization of.

analytic methods for. 10Organic materials. See also Organic materials,

characterization of.carbon and sulfur in 221-225characterized 1deer hair follicles, determination of sulfur

in 224determining inorganic materials in 167fusion techniques for 167identified, and structure determined in 109liquid fire method of wet washing 166microanalytical elemental analysis 186single-crystal, Raman analysis of 129

Organic materials, characterization ofanalytical transmission electron

microscopy .429-489Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron spin resonance 253-266elemental and functional group


structure .407-419gas analysis by mass spectrometry 151-157gas chromatography/mass

spectrometry 639-648infrared spectroscopy 109-125liquid chromatography 649-659low-energy ion-scattering

spectroscopy 603-609molecular fluorescence spectrometry 72-81neutron activation analysis 233-242neutron diffraction .420-426nuclear magnetic resonance 277-286particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187radial distribution function analysis 393-401Raman spectroscopy 126-138



secondary ion mass spectroscopy 610-627single-crystal x-ray diffraction 344-356ultraviolet/visible absorption


Organic mixtures. See also Mixtures; Organicmaterials; Organic materials.characterization of.

liquid chromatography of 649Organic polysulfides, recrystallized, single-

crystal analysis of. 353Organic single crystals. See also Crystals;

Single crystals; Organic materials; Organicmaterials, characterization of.

ESR studied 263Organic solutions. See also Organic materials;

Organic materials, characterization of;Solutions.

analytic methods for. 10Organic solvents. See also Organic materials;

Organic materials, characterization of;Solvents.

flame atomic absorption spectrometry for . .47in ICP sample introduction 35

Organometallicsanalytic methods for. 9silicate film, positive SIMS spectra for 617

Organosulfur compounds, collision-activateddissociation mass spectra 647

Orientationeffect. 119molecular, determined in drawn polymer

films 120molecular, IR determination of 109

Orientation distribution functionalong fiber lines as function of rolling

reduction 363-364analysis. series method of 361-363coefficient, determining 362for copper tubing, Euler plots method 361defined 360and Euler plots 360-361series representations 361-362

Orientation relationshipscrystallographic, SEM evaluated .490determined .453in dislocation cell structure analysis . .470-473as fine structure effect .438and habit plane .453-455Kurdjumov-Sachs, for fcc/bee

materials .438-439and misorientation determination .471-472as x-ray diffraction analysis 325

Oriented surfaces, structural information byEXAFS .407

Orthorhombic unit cells 346-348Oscillating electric field, wave theory of ....83Oscillating magnetic field, wave theory of. ..83Oscillometric (high-frequency) titration, as

electrometric 203-204Osmium

distillation 169gravimetric finishes " 171

Outlier, defined 678Overaging, kinetics of 317Overcorrection, of signal, AAS

spectrometers 5 IOverlayer growth, LEED kinetic

analysis 544Overload failure, of quench-cracked AISI 4340

steel threaded rod 511-513Overpotential, in electrogravimetry 198Overscanning, field of mixed phases, errors

observed by 529Overvoltage, effects in EDS 523

Oxidation. See also Oxidation-reduction;Redox; Reduction.

chemical reaction products identified 549of copper films, using oxygen 609effect on FMR in single-crystal iron

whisker 274internal, SIMS analysis of second-phase

distribution 610iron, partitioning states in 178LEISS analysis of 603, 609molecular structure and orientation determined

in '" " '" 109-reduction reactions, classical wet

chemistry 163-164SERS studies of 136of silver electrodes in alkaline

environments 135SIMS tracer studies 610species, analysis of 201of species soluble in solution 208states, of elements 688states of metal atoms in metal oxide surface

films, XPS for 568states, partitioning 178surface, F1M1AP study of 583in voltammetry 189and x-ray spectrometry 82

Oxidation-reduction (redox). See alsoClassical wet analytical chemistry;Oxidation; Redox; Reduction.

of potential contaminant ions, in gravimetricsamples 163

reactions, as classical wet chemicalanalysis 163-164

Oxidesdeposition 201formation, as interfering elements in high

temperature combustion 222hydrated, precipitation for 169as inclusions 176pulsed laser atom probe analysis for. 597sample dissolution in hydrochloric acid 165surface layers, SIMS analysis 610surface, measuring 177vanadium K-edge XANES spectra in .415weighing as the, gravimetric analysis 170

Oxidizing acids, sample dissolution by 166Oxygen

analysis by inert gas fusion, for aluminum-killed steel 231

analyzed in microcircuit fabricationprocess 156-157

Auger chemical map for 557bombardment, SIMS spectra for 615-616chemistry at surfaces, AES analyis of 553determined by 14-MeV FNAA 239effect on positive secondary ion yields 612-fired fracture surface, XPS survey 577gas mass analysis of. 155high-energy neutron irradiation of 234inert gas fusion systems for

detecting 226,228-229,231injection 221in inorganic solids, applicable analytical

methods .4, 6isotopes, determination in explosive

actuator 625-626isotopes in explosive actuator, SIMS

determined 625-626oxidation of copper films using 609quenching of fluorescence 79-80in silicon wafers, quantitative analysis

of '" " 122-123in titanium, determined 231ultrahigh-purity 224use in high-temperature

combustion 221-222, 224Oxygen-flask combustion. See Schoniger flask

method.

Index / 737

Oxygen plasma dry ashing, for sampledissolution 167

Oxygen quenching of fluorescence 79-80

p

P. See Phosphorescence.P. See Polarization.Paint

14 KRS-5 ATR spectrum 121adherence, effect of surface carbons on 224automobile, NAA forensic studies of 233dissolved in methylene chloride solvent, ATR

analysis 121potassium, calcium, and titanium

determination in 98Pair distribution functions, separation of RDF

into 397-398Palladium


evaporation fields for. 587gravimetric finishes 171organic precipitant for 169photometric analysis methods 64support of SERS in vacuum 136weighed as the dimethylglyoxime

complex 171PAN, as metallochromic indicator 174Paper, acidity-basicity measured in 172Paper chromatography, as qualitative

separation technique 168Parabens

as antimicrobial agents 655liquid chromatography analysis in baby

lotion 655-656Parabolic peak location method, x-ray

diffraction residual stresstechniques 386

Paramagnetic centers and properties, ESRcharacterized 253, 263

Paramagnetic resonance. See Electron spinresonance.

Paramagnetism 257, 678Parameters

defining background, RDF analysis 396short distance, RDF analysis 351

Parasitic peaks. See Escape peaks.PAR, as metallochromic indicator 174Parent-daughter relationship, radioactive

isotope decay 244Parent ion scans, gas chromatography/mass

spectrometry 646Parent population, defined 12Parr oxygen bombs, use in ion

chromatography 664Particle absorption, as XRPD source of

error 341Particle accelerator, defined 678Particle growth, effect in gravimetric

analysis 163Particle-induced x-ray emission. " 102-108

and other elemental analyses, compared ... 106applications 102, 106-107Binary Encounter Model 104calibration 105capabilities, compared with Rutherford

backscattering spectrometry 628characteristic x-rays 103data reduction 105defined 678detection limits 104estimated analysis time '" 102general uses 102introduction and principles 103-105limitations 102and milliprobe and historical studies 107



738/ Index

Particle-induced x-ray emission (continued)and neutron activation analysis, compared 233Plane Wave Born Approximation 104and proton microprobe 107quality assurance protocols 105RACE code 105related techniques 102samples 102sensitivity 104-105stopping distance 103typical set-up for 103x-ray cross section 104and x-ray fluorescence, compared 105-106

Particles. See also Particle size; Particle sizedistribution.

absorption of 341accelerator, defined 678atmospheric, analysis of 106charged, detectors for 245-246combined geometric and elemental

analysis 318-320of elemental categories, data and statistical

summaries 320-322energy-dispersive spectrum from 319gold, scan line across .496growth of 163heavy, kinetic energy of 24located, image analysis for 319PIXE analysis 102-108produced by explosive detonation, image

analysis of. 318-320scanning electron micrograph 319shape, geometric and elemental analysis

of 318-320small, examination by ATEM .452small, single-stage extraction replicas for

ATEM analysis .452suspended, PIXE analysis 102unknown, identification by electron

diffractionlEDS .455-459Particle size. See also Particles; Particle size

distribution.effect in gravimetric analysis 163effects, and sample preparation for x-ray

spectrometry 93geometric and elemental analysis 318-320PIXE analysis of atmospheric aerosols

by , 102typical, PIXE analysis , .. 0' ••••••• 103

Particle size distribution. See also Particles;Particle size.

as analysis, in second-phase testing 177image analysis 309-322optical metallography 299-308in powders, image analysis of. 309as residue analysis 177scanning electron microscopy .490-515

ParticulatesPIXE phase analysis of 102removal 664

Partitioningin gas chromatography/mass

spectrometry 641oxidation states 178in solvent extraction 164

PAS. See Photoacoustic spectroscopy.Pascal 685, 691Paschen-Runge polychromators, for ICP ., .37Pass energy, as kinetic energy 571Passive films. See also Films; Thick films; Thin

films,composition vs depth, on tin-nickel

substrate 608-609study of 557-558

Path length, in UVIVIS absorptionspectroscopy 62

PDA. See Photodiode arrays.Peak broadening

in EPMA measurement , 519

as XRPD source of error 341Peak overlap

defined 678major component analysis with 530spectral, AES 556

Peaksartifact, as AEM-EDS microanalytic

limitation .448Auger electron 551breadth and position, micro- and

macrostresses from 387broadening 341, 519diffraction, in surface stress

measurement. 385EPMA, gold-copper alloys 530escape or parasitic 520false silicon or internal fluorescence 520identification, EDS 522-523internal fluorescence, EDS spectra 520sum, defined 92, 520switching 144well-resolved, and high concentrations 530width, liquid chromatography 651in x-ray spectrometer detectors 92

Peak switching technique, for ion currentsignals 144

Pearlitegrowth 508SEM resolution of .494

Pearson VII distribution functions, in surfacestress measurement. 386

PelletsKBr, as IR samples 113as samples, x-ray spectrometry 93

PEM. See Photoelastic modulators.Pendellosung fringes 368, 370Penetration, depth of, in ATR

spectroscopy 113Pentachlorobiphenyl, mass spectrum for 642Pentaerythritol, as common crystal analyzing

crystal 88PEP, as synchrotron radiation source .413Percent cold work

diffraction-peak breadth at half height asfunction of 387

gradient, and maximum residual stress 380and residual stress caused by stress-relieving

heat treatment and forming, measured ..380and residual stress distribution 390surface or subsurface, by x-ray diffraction

residual stress techniques 380, 390Perchlorate, as electrode 185Perchloric acid

as oxidant and sample dissolutionmedium 166

residue isolation using 176Periodate method, analysis for manganese in

zirconium alloys by 69Periodic table

for analytic sensitivities of AAS .46of the elements 688

Peristaltic pumps, use with concentricnebulizers 35

Permalloy, on ceramic substrate, x-rayspectrometry 100-10 I

Permanganate titration, for chromium andvanadium 176

Permeabilityof immiscible liquids 164SI derived unit and symbol for 685

Permittivity, SI derived unit and symbolfor 685

Perovskite, in ceramic waste form simulant,EPMA analysis for 532-535

Peroxidesdetermined 218functional group analysis of 218

PesticidesGC/MS analysis 639

liquid chromatography analysis of thermallyunstable 649

residues, detected in plant and animaltissues 188

PETRA, as synchrotron radiation source .413Petrography, residue analysis by 177Petroleum. See also Petroleum products.

analytic methods for. 10derivatives, analytic methods for 10oil, GClMS analysis of volatile compounds

in 639voltammetric monitoring of metals and

nonmetals in 188Petroleum products. See also Petroleum.

acidity-basicity measured in 172analysis of 100-10 Isulfur determination by XRS 82

PGAA. See Prompt gamma activation analysis.pH

change, effect in analyte extraction 164constant, maintained by electrometric

titration 202control, in EDTA titration 173determination by glass electrode 203effect in chelometric titration 164effect in inorganic precipitation 169effect of overpotential in

electrogravimetry 198and equilibrium, in classical wet analysis 163meters, vs acid-base indicators 173negative logarithm of hydrogen-ion activity

as 690Pharmaceutical mixtures

liquid chromatography of 649voltarnmetric analysis of metals in 188

Phase analysisof hydrided TiFe, Miissbauer effect, .293-294by Mossbauer spectroscopy 287-295nuclear magnetic resonance 277-286

Phase boundariesdetermined .474effect on lateral resolution, atom probe

analysis 595Phase contrast

analytical electron microscopy .445, 446defined 678microscopy, Lorentz microscopy as .446

Phase diagram determinationequilibrium verification .475-476experimental procedure .474phase boundaries .474-475traditional and modern probe-forming

transmission electron method ..... .473-474Phase diagrams

determination of .473-476magnetic 268XRPD determined 333

Phase distributionof inorganic solids, methods for analysis . .4-6of organic solids, methods for analysis 9SIMS analysis 610

Phase/grain size and distributionimage analysis 309-322optical metallography 299-308scanning electron microscopy .490-515

Phase identificationof inorganic solids, applicable analytical

methods .4-6second-phase testing, classical wet

chemistry 176-177surface, LEED analysis 536unknown, by electron diffractionlEDS

analysis .455-459Phase or compound identification


electron probe x-ray microanalysis 516-535elemental and functional group

analysis 212-220



field ion microscopy 583-602gas analysis by mass spectrometry 151-157gas chromatography/mass

spectrometry 639-648infrared spectroscopy 109-125liquid chromatography 649-659molecular fluorescence spectrometry 72-81Mossbauer spectroscopy 287-295neutron diffraction .420-426nuclear magnetic resonance 277-286optical metallography 299-308Raman spectroscopy 126-138single-crystal x-ray diffraction 344-356small-angle x-ray and neutron

scattering .402-406ultraviolet/visible absorption

spectroscopy 60-71x-ray diffraction 325-332x-ray powder diffraction 333-343

Phase problem, in single-crystal x-raydiffraction 349-351

Phases. See also Phase or compoundindentification; Phase transformations;Phase transitions.

amorphous, TEM bright-field images ofceramic containing .445

amount of, as x-ray diffraction analysis 325changes detected in 277, 282-283changes, using single-crystal x-ray diffraction

for 354chemistry of .445, 446, 678compositional analysis, EPMA 516crystalline, XRPD analysis 333defined, for inclusion and second-phase

testing 176differences in scattering from different

electrons within an atom 328precipitate, SEM analysis .490problem in single-crystal x-ray

diffraction 349-351separation of .402, 405stability of 598structure, characterization by optical

metallography 299unknown, identification of. .455

Phase transformationseffect of temperature on 318pressure- or temperature-induced, XRPD

analysis 333solid-state, XRPD analysis 333studied by FIMlAP '" ..583studied by x-ray topography 365, 376

Phase transitionscrystallographic, variable-temperature ESR

studies of 257observing by neutron diffraction .420

Phenanthroline method, for iron in leadalloys 66

Phenoformaldehyde resins, formation of 132Phenolphthalein, as acid-base indicator 172Phenol red, as acid-base indicator 172Phenols

determined 218-219electropolymerization of, SERS study of .. 136in isopropanolic medium, determined by

electrometric titration 205Phenyl groups

in polymers, Raman analysis 131in silicone, Raman analysis 132

Phenylhydrazine, as precipitant. 169Phenylthiohydantoic acid, as precipitant 169Philips PW-1410 sequential x-ray

spectrometer, spectrum from 88Phonons, excitation, as inelastic scattering

process .434Phosphates

anions, separation by ion chromatography 659rock, nitric acid as dissolution medium

for 166

weighing as the, gravimetry analysis ..... 17lPhosphorescence 679, 690Phosphoric acid

derivatives, as solvent extractant 169-170as sample dissolution medium 165as sample modifier, GFAAS analysis 55

Phosphorusback-titration determination 173determined by 14-MeV FNAA 239glow discharge sources for 29glow discharge to detemine, in low-alloy

steels and cast iron 29high-energy neutron irradiation of. 234ICP-determined in natural waters .41ion chromatography analysis in organic

solids 664ion-implantation profile in silicon, SIMS

analysis 623-624photometric analysis methods 64radiochemical, destructive TNAA of 238species weighed in gravimetry 172surface segregation during heating 564-565volumetric procedures for 175

Phosphorus-doped silicon substrate, high-resolution SIMS spectra 623

Photoacoustic spectroscopyapplications 115depth profiling a granular sample using 120and FT-IR, compared 115

Photochemical systems, ESR analysis of 256Photoconductors, ESR studied 263Photodetectors, for echelle spectrometer. .41Photodiode arrays, in ICP spectrometers 38,

690Photoejection of electrons, by

x-radiation 84-85Photoelastic modulators 114, 115, 690Photoelectric absorption, in EXAFS

analysis .409Photoelectric effect

absorption and 97defined 679and radiationless transitions 568in x-ray spectrometry 84

Photoelectric electron multiplier. SeePhotomultiplier lithe.

Photoelectric penetration distance, effect indefect imaging 367

Photoelectronsand Auger electrons 550K-, backscattering of .408

Photoemission, principles andnomenclature 569

Photographic filmas detectors 326dot maps recorded on 527

Photoionization, x-ray detectors 90Photoluminescence, defined 679Photolytic systems, ESR analysis for 256Photometers

defined 679filter 67

Photometric methodsfor analysis of metals and metal-bearing

ores 64ion detection technique 143-144

Photomultiplier tubefor AAS and related techniques .44abbreviation for 691defined 679for molecular fluorescence spectroscopy 77use in ICP polychromator 38for UVIVIS analysis 66in x-ray spectrometers 89

Photon detectors 246, 326Photon factory, as synchrotron radiation

source .413Photons. See also X-ray photon emission.

absorbed or scattered 84-85

Index /739

absorption of. 61colliding, in Raman spectroscopy 127defined 679detectors for 246EDS measurement of 519-520effect in EDS detectors 90emission 61and fluorescent yield 86infrared light as 109numbers for dot mapping 527scattering of 84

Photoplate blackening and ion exposure forSSMS, relationship between 143

Photosynthesis, ESR studied 264Phthalic acid salts, as ion chromatography

eluents 660Physical adsorption. See Physisorption.Physics, atmospheric, PIXE studies in ..... 106Physisorption

as contamination in gravimetric samples .. 163defined 679of pyridine, Raman analysis 134

Pibonding, defined 679electron, defined 679

Picometer, abbreviation for 691Picral and nital, etchants compared 302Picture element. See Pixels.Picture points, IA scanners 310Piezoelectric effect, in deposition,

electrogravimetry 198Pinhole cameras, for XRPD analysis 334-335Pipe, metal, sampling trainload of. 15Pipet, defined 679Pitting, effect in surface stress

measurement. 387PIXE. See Particle-induced x-ray emission.Pixels

density, in elemental mapping of high-temperature solder 532

in dot mapping 526-527image analysis scanners 310picture elements as 690

Plain carbon steels, effect of disturbed metal onmetallographic appearance of 301

Planck's constantabbreviation for 690defined 679in electromagnetic radiation 83in ESR analysis 254

Plane angle, SI supplementary unit and symbolfor 685

Plane grating, defined 679Plane strain, defined 679Plane stress, defined 679Plane-stress elastic model

full-tensor determination 384Marion-Cohen technique 384sin2 <I> technique 384single-angle technique 383-384two-angle technique 384of x-ray diffraction stress

measurement 382-384Plant tissues

AAS analysis of trace metals 55analysis of .41ICP-sequential monochromator analysis of . .41powdered, PIXE analysis 102voltammetric detection of herbicides/pesticides

in " 188Plasmajet .40, 679Plasma-polymerized hexamethyldisiloxane,

structure and degradation of. 285-286Plasmas

defined 679mixed gas 37

Plasma torchICP, structure of. 32use in ICP-AES 31



740/ Index

Plasmondefined 679excitation, as inelastic scattering

process .434loss, Auger electron 551loss, peak structures, alumina and

aluminum 552Plastic deformation. See also Deformation.

effect on fringe patterns 368Plasticizers

GC/MS analysis of 639infrared spectrum 124and polymer materials, identified in vinyl

film 123-124Plastics

acidity-basicity measured in 172analytic methods for 9EFG composition analysis 212GC/MS analysis of volatile compounds

in 639Plastic strain, topographic methods for. 368Platelets, inclined through foil, AEM

analysis .453, 455Plating baths

acidity-basicity measured 172potentiometric membrane electrode analysis

of. 181solution analysis, by ion chromatography 658wet chemical analysis of 165

Platinumalloys, FIM sample preparation of 586determined in silver scrap metal .41electrodes, in biamperometric titration 204evaporation fields for 587gravimetric finishes 171nitric/hydrochloric acid dissolution

medium 166substrate, extent of coverage of nickel-

phosphorus film on 608in vacuum, as SERS metal 136

Plutonium-beryllium reactions, as neutron source for

NAA 234determined by controlled-potential

coulometry 209diffusion into thorium 249

PMT. See Photomultiplier tube.Pneumatic nebulizers 34-36, 47Point analysis

beryllium-copper alloy 559cold-rolled steel. 556-558

Point defectsFIM images in pure metals 588-589internal grain structure 358observed using FIM 588in radiation damage, FIMIAP study of. 583

Poisson's ratiodefined 679or frequency, symbol for 692in stress measurement 382

Polar crystals, LEISS identification offaces 603

Polarizability, molecular, effect in Ramanspectroscopy 127

Polarizationof a molecule, abbreviation for 690analyzer, in Raman spectrometer 128"f-ray, Mossbauer spectroscopy 288modes, dynamic diffraction 367modulation 114-115molecular 127potentiostatic, curve for Inconel 558, 625prevention by stirring in

electrogravimetry 200scrambler, in Raman spectrometer 128in voltammetry 189

Polarization modulation, as infraredspectroscopic method 114-115

Polarizing element, defined 679

Polarograms, de and differential pulse, ofnickel in cobalt nitrate 194

Polarographic wave, defined 190Polarography

capabilities 207current-sampled 193defined 189, 679differential pulse 193electrometric titration and, compared 202potentiostat for 199pulse 193

Pole figures(ill) from copper tubing 363defined 679determining, in crystallographic measurement

and analysis 360-361expected orientations 360from inside wall, copper tubing 363measured (ill) for Cu-3Zn 360from midwall, copper tubing 362neutron diffraction .423thick-sample reflection measurement 360

Polishingautomatic equipment 313chemical, as FIM sample preparation 584damage 301mechanical, Raman analysis 133microbeam analysis samples 529-530rough and fine, optical metallography

specimen preparation 301of samples, x-ray spectrometry 93

Pollution. See also Effluents.environmental, GFAAS analysis of 58studies, by NAA 233

Polyacrylamide, percent conversion topoly(N-dimethylaminomethylacrylamide),Raman analysis for. 132

Polychromatic radiationbeams, single-crystal diffraction

methods 329interelement effects 97

Polychromatic reflection topography 366Polychromators

computerized 24defined 679ICP-AES 34, 37-38Paschen-Runge 37as wavelength sorting device 23-24

Polycrystalline diffraction methods 331-332Polycrystalline materials

described 358double-crystal diffractometry for 372, 373engineering, residual stress and texture

determined by neutron diffraction .420EXAFS analysis .410measurement and analysis 357-364preferred orientation in 358RDF-determined interatomic distance

distributions and coordinationnumbers 393

texture as measure of average grainorientation in 358

x-ray topography of aggregates of 365Polycrystal rocking curve analysis 371-373Polycrystals, Berg-Barrett reflection topographic

method for 369Polycrystal scattering topography

basic principle 374Soller slit arrangements for 375

Polyethylenecrystallization, Raman analysis of. 132high-density, for irradiation containers 236

Polygonization, Lang topography for 377Polyimide resin, NMR analysis of curing

mechanism of 285Polymer blend system, factor analysis and

curve fitting applied 118Polymer-curing reactions, ATR

monitoring 120-121

Polymer films. See also Films.drawn, infrared dichroism spectroscopy to

determine molecular orientation in ..... 120stretched, infrared determination of molecular

orientation in 109Polymer glasses, SAS applications .405Polymerization

of butadiene and styrene, Ramananalysis 132

of phenols, SERS studies of 136Raman analysis 131x-ray topography and synchrotron radiation

studies 365Polymer membrane electrodes 182Polymers

analysis of 9, 131-132, 639, 647-648blends 118, 405block, SAS applications .405curing, ATR monitoring of 115,120-121drawn films, molecular orientation

determined 120EFG determination of unsaturation in 212ESR analysis 263identification in vinyl film 123-124infrared spectrum 123liquid chromatography monitoring of stability

during aging 649and plasticizers identified in vinyl film 123pyrolysis GC/MS analysis of 647-648Raman analysis 131-132resins, use in ion exchange separation 164SAXS/SANS analysis of .405

Polymorph, defined 679Polymorphism, defined 679Polynomial regressions, use in x-ray

spectrometry calibration 97Polynuclidic elements, SSMS analysis 145Polyphosphates, detected by ion

chromatography 661Polyphosphonates, detected by ion

chromatography 661Polypropylene

isostatic, infrared linear dichroismspectroscopy of. 120

transmission by 100Polystyrene blend, analysis of. 118Polytetrafluoroethylene vessels, for sample

dissolution treatment 165, 166Polythioethers, terminal mercapto groups in,

Raman analysis 132Polyvinyl alcohol, as sample binding

agent 94Polyvinylchloride, determined in vinyl

film 123-124Pontachrome Black TA. See Eriochrome Black

T.Population

defined 679of excited nuclear level, Mossbauer

spectroscopy 288target and parent, in random sampling 12

Portland cementanalysis of free lime 179flame emission sources for 30

Poschenrieder analyzer, in ECAPanalysis 597

Position-sensitive detectorabbreviation for 691effect in double-crystal

spectrometry 372-374, 377neutron diffraction .422

Positive eyepiece, defined 679Positive ion charge, symbol for. 692Positive secondary ion yields, effect of oxygen

on 612Positron emission, and electron capture, as

radioactive decay mode 245Postionization structure, typical K-shell

edge .450



Potassiumacid-base titration 173additions to flame AAS samples .48cations, in glasses, Raman analysis 131determination in paint, absorption and

enhancement effects 98flame emission sources for 30as flux 167organic precipitant for 169Raman vibrational behavior. 133species weighed in gravimetry 172TNAA detection limits 237in vacuum, as SERS metal 136

Potassium benzyl penicillin, three-dimensionalelectron density map of 350

Potassium bromidepellets, as IR samples 113pellets, as Raman samples 131sample, for Raman spectroscopy 129

Potassium hydrogen difluoride, as fusionflux 167

Potassium hydroxide fusion, crucibles for .. 167Potassium pyrosulfate

as acidic flux 167for low-temperature fusions 94

Potentialbetween working and reference

electrodes 661half-wave, as polarographic wave

parameter 190membrane, ion-selective membrane

electrode 182standard, in controlled-potential

electrolysis 208vs time, potentiometric membrane

electrodes 186use in voltammetry " 189

Potential buffers, use in electrogravimetry ..200Potential difference, SI derived unit and

symbol for 685Potential energy diagrams 586Potentiometric gas-sensing

electrodes 183-185Potentiometric membrane electrodes. See also

Classical. electrochemical andradiochemical analysis;Potentiometry 181-187

additional techniques used with 183advantages 181analysis methods 183applications 181, 186calibration curves 183capabilities, compared with voltammetry .. 188defined 679estimated analysis time 181experimental arrangement for 186general uses 181introduction 181ion-selective membrane electrodes 181-183limitations 181possible errors 185-186potentiometric gas-sensing electrodes 183-185related techniques 181samples 181, 186subtraction techniques used with 183titration methods 183

Potentiometric titration 183, 203, 204Potentiometry. See also Potentiometric

membrane electrodes.capabilities, compared with voltammetry .. 188

Potentiostatautomatic, for controlled-potential

analysis 200galvanostat, power. 199

Pourbaix (potential-pH) diagramsand corrosion on lead surfaces 135defined 679

Powdercompacts, preferred orientations in 358

diffraction, geometry and detectionmethods 331

metallurgy, abbreviation for 691pattern 262, 265samples, ESR analysis of 262x-ray diffraction of 333-343

Powder Diffraction File (PDF) 327Powdered biological materials, analysis

of '" 106-107Powders

hjtlage analysis of particle size distributionsin 309

mounting, for XPS analysis 575pure, Raman analysis 129for sample dissolution 165samples, fluxes for fusing of. 167as samples for x-ray spectrometry 93-94as samples, Raman analyses 130SIMS analysis of surface layers 610XPS samples ground to 575

Powerconversion factors 686density, conversion factors 686radiant flux, SI derived unit and symbol

for 685supplies, electrogravimetry 200

Power density, conversion factors 686Praseodymium and neodymium, separation by

radioanalysis 249-250Preamplifiers

and amplifiers, in x-ray spectrometerdetectors 91

field effect transistor, for EPMA 519pulsed optical 91

Prearc period, defined 679Precession camera, diffraction pattern

photographs by 345-346Precession method

net nuclear magnetization 280single-crystal diffraction 330

Precious metals, SSMS analysis in geologicalores 141

Precipitatesdiscrete, along grain boundaries in nickel-base

alloy 307FIMIAP study of nucleation, growth, and

coarsening of 583in gravimetric analysis 163identification in stainless steels, by light-

element analysis .459-461lost, in gravimetric analysis 163measurement of persistence depth, as FIM

application 590optical micrograph, in stainless steel

tube .459particles, growth in gravimetric analysis .. 163phases, SEM analysis .490pure, quantitative removal for weighing,

gravimetry as 163ultrafine secondary, atom probe analysis

of IN 939 598Precipitation

ammonium hydroxide 168atom probe composition profile of 593of chemical compound, as chemical

equilibrium 163coherent, effect on diffraction

pattern .438, 440CO°, in gravimetric analysis 163by cupferron 169efficiency measured 243grain-boundary, AES analysis 549by hydrolysis to oxides 169of implanted alloys .485-486inorganic 169of R203 group, by ammonium hydroxide .. 168separations 168SIMS analysis of second-phase distribution

due to 610

Index /741

sodium hydroxide 168sulfide ion 169techniques 168-170titrations 173

Precipitation titrationsof industrial materials 173Volhard, of silver. 173

Precisionand accuracy, compared 524-525analysis and automation,

electrogravimetry 199analysis, electrogravimetry as 197defined 679high-, electro metric titration for 202of radioanalysis 246-247of single-crystal analysis 352in UVIVIS absorption spectroscopy 70

Pre-edge absorption, oxide series .415Preferred crystallographic growth, SACP use

to establish 509Preferred orientation

crystallographic, measurement and analysisof 357-364

Euler plots and orientationdistribution 360-361

in stereographic projection 358metallurgical specification of 359-360pole figures 360polycrystalline, and property behavior 358RD-TD-ND system " 358,359specifying 359in stereographic projection 358-359as XRPD source of error 340-341

Prefixes, of SI units, names and symbols ...687Prehistoric materials, radioanalytic dating

of. 243Preionization structure, in typical K-shell

ionization edge .450Premix burners

defined 679for flame source emission 28temperature of flames 29

Premix chamber, AAS flame atomizers . .47,48Preparative liquid chromatography, for

obtaining purified compounds 654Prepolishing. See also Polishing.

chemical or electrolytic, as FIM samplepreparation 585

Preservation sample 15, 16Prespark period, defined 679Pressed briquet XRS samples 93Pressure

controlled in gas mass spectrometer .. 151-152fluid, conversion factors 686stress, SI derived unit and symbol for 685structural changes as function of .420

Pressure-induced phase transformations,XRPD analysis 333

Primary excitation. See also Excitation.AES, electron beams for 550

Primary extinctioneffect, in dynamic theory of

diffraction 366-367as XRPD source of error 341

Primary ion bombardment, effects of 611Primary standards, assay by electrometric

titration 202Primary x-rays, See also X-rays.

defined 679Principal stresses, and stress distribution 382Prism, defined 679Probe ion, defined 679Probes. See also Electron probe x-ray

microanalysis; Pulsed laser atom probe.electroanalytical, for process control ..... 197

Process control. See also Quality control.electrometric titration for 202on-line, electrogravimetry 199of solid samples, XRS for 83



7421 Index

Process control (continued)use of ICP-AES in 31

Process gas. See also Gases.analytic methods for 8, 11inorganic, analytic methods for 8microcircuit, analyzed 156-157microcircuit, gas mass spectrometry

for , 156-157organic, analytic methods for 11

Process monitoring, Ff-IR spectroscopyfor 112

Process reagents. See also Reagents.trace impurities analysis in .43

Process streams, UV/VIS on-line monitoringof species in 60

Process waters. See also Rinse waters; Water.wet chemical analysis , 165

Profiles. See also Composition profiles; Depthprofiles; Depth profiling.

damage depth, RBS analysis for 632-633depth-composition, stainless steel 555depth, FIMIAP surface analysis 583impurity. RBS analysis for 632

Progressive field evaporation, in the atomprobe , 591

Projection topography, for defect imaging ofcrystals 369

Prompt gamma activationanalysis 239-240, 689

Prompt neutron-capture 'V-rays, inNAA 234

Proportional limit, defined 679Protactinium, M lines use for 86Protein

dynamics, MFS analysis for 72surface, IR analysis 1l9-120

Protocol, sampling 13, 15-16Proton energy, abbreviation for. 690Proton microprobes

of biological samples, compared 107capabilities 102particle-induced x-ray emission and 107

Proton milliprobes, capabilities 102Protons, defined 680PSD. See Position-sensitive detector.Pseudo-Kossel llnes, in divergent-beam

topography 371PST. See Polycrystal scattering topography.PTB, as synchrotron radiation sourc,e .413Pulsed laser atom probe

facilities built into ECAP 598schematic 5.97of ternary 3:5 semiconductor 601-602

Pulsed optical preamplifier, x-rayspectrometers 91

Pulsed spectrometers, in acoustic ESR 258Pulse-echo method, nuclear magnetic

resonance 281Pulse fraction curves, for atom probe

microanalysis 594-595Pulse generator, high-voltage, for atom probe

microanalysis 591Pulse-inspection circuitry, energy-dispersive

spectrometer 519-520Pulse method, of measuring relaxation

times 258Pulse NMR spectrometer 283Pulse polarography

differential 193as improved voltarnmetry 193normal. 193

Pumping system, vacuum, SEMmicroscope .491

Pumpsperistaltic, in ICP concentric nebulizers ....35rotary and diffusion vacuum, in gas mass

spectrometer .. , 151-152sampling 16Toepler 152

Punching technique for subdividingsolids 165

Punctual illumination, MOLE/Ramananalysis 129-130

Pure aluminum, K-M CBEDP from , . .441Pure materials, as primary standards 162Pure metals, FIM images of defects

in 588-589Pure nickel, K-absorption edge .408Purity

determined by EFG 212of materials, NAA analysis for 233of solvents and reagents, UVIVIS analysis .68

Pyrene monomer, fluorescence emissionspectra 76

Pyridineadsorbed, vibrational behavior 134SERS of 136

Pyridylazonaphthaol, as metallochromicindicator 174

Pyridylazorescorcinol, as metallochromicindicator 174

Pyrocatechol violet, as metallochromicindicator 174

Pyrochlore, in waste form simulant, EPMAanalysis for 532-535

Pyroelectric device, infrared detector as ....223Pyrolysis gas chromatography/mass

spectroscopyanalysis of rubber sheaths by 648polymer analysis by 647-648

Pyrolysis products, analytic methods for .... 11Pyrophosphate, zirconium weighed as, in

gravimetric analysis 171Pyrotechnic actuators, corrosion in 510-511Pyrotechnic materials, SEM analyses ..510-511

Q

Q-band microwave frequency, use in ESR 255Quadrupole interaction, in Miissbauer

effect 290-293Quadrupole mass filter, schematic, of gas mass

spectrometer 153Quadrupole resonance, capabilities 253Qualitative analysis. See also Qualitative

analysis, methods for.of anions and cations, organic and

inorganic 658and Auger emission probabilities 550classical wet chemistry 167-168defined 680direct-current plasma .40electrographic 202electrometric titration 202-206electron energy loss spectroscopy .450energy-dispersive spectrometry 522-523energy-dispersive x-ray spectrometry ..82-101functional group 654of inorganic gases, analytic methods for 8of inorganic liquids and solutions, analytic


for .4-6infrared, factor analysis for 116LEISS spectra in 604-605of major components, analytic methods for . .4micro-, AEM-EDS for .446-447of minor components, analytic methods for . .4of organic solids and liquids, analytic

methods for 9-10resolution enhancement methods 1l6-117search/match methods as .455of surface phase on silicon 341-342of trace elements, analytic methods for .... .4of ultratrace components, analytic methods

for .4wavelength-dispersive spectrometry 523-524

Qualitative analysis, methods for. See alsoQualitative analysis.


Auger electron spectroscopy 549-567electron probe x-ray microanalysis 516-535electron spin resonance 253-266field ion microscopy 583-602gas analysis by mass spectrometry 151-157gas chromatography/mass

spectrometry 639-648infrared spectroscopy 109-125ion chromatography 658-667liquid chromatography 649-659low-energy ion-scattering

spectroscopy 603-609molecular fluorescence spectrometry 72-81Miissbauer spectroscopy 287-295neutron diffraction .420-426optical emission spectroscopy 21-30particle-induced x-ray emission 102-108Raman spectroscopy 126-138scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627spark source mass spectrometry 141-150ultraviolet/visible absorption

spectroscopy 60-71x-ray diffraction 325-332x-ray photoelectron spectroscopy 568-580x-ray powder diffraction 333-343x-ray spectrometry 82-101

Qualitative elemental analysiscrystallographic texture measurement and

analysis 357-364de arc emission spectroscopy 25

Quality assurance. See also Quality control;Process control.

for sampling , 17Quality control. See also Process control.

by image analysis 309, 316of integrated circuits 122-123of metallurgical products 200nondestructive surface residual stress

measurement for. 380for purity or composition, NAA analysis

as 233of raw materials, sampling in 12in sampling 17of semiconductor devices, by SEM .490x-ray spectrometry of solid samples as 83

Quantitative analysis. See also Quantitativeanalysis, methods for.

AEM-EDS micro- .447atom probe microanalysis, requirements

for 594-595defined 680electron energy loss spectroscopy .450elemental, of industrial materials 162-179electron probe x-ray microanalysis, standards,

accuracy, and precision 524-525of field ion microscopy images 590-591of four titanate phases, waste form

simulant 534functional group 654of hydroxyl and boron content in

glass 121-122for impurities in LPCVD thin films 624of inorganic gases, analytic methods for 8of inorganic liquids and solutions, analytic

methods for. 7of inorganic solids, analytic methods for . .4-6of major components, analytic methods for . .4of minor components, analytic methods for . .4of organic liquids and solutions, analytic

methods for. 10of organic solids, analytic methods for. 9of oxygen in silicon wafers 122-123of phosphorus ion-implantation profile in

silicon 623-624



and separation, of metal ions 200-201stripping analysis 202of trace components, analytic methods for .. .4ultrasensitive destructive 233of ultratrace components, analytic methods

for '" .4x-ray powder diffraction 339-340of ZnO in calcite 342

Quantitative analysis, methods for. See alsoQuantitative analysis.


atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrochemical analysis 181-211electrogravimetry 197-20 Ielectrometric titration 202-206electron probe x-ray microanalysis 516-535electron spin resonance 253-266elemental and functional group

analysis 212-220gas analysis by mass spectrometry 151-157inductively coupled plasma atomic emission

spectroscopy 31-42infrared spectroscopy 109-125ion chromatography 658-667liquid chromatography 649-659low-energy ion-scattering

spectroscopy 603-609molecular fluorescence spectrometry 72-81M6ssbauer spectroscopy 287-295neutron activation analysis 233-242neutron diffraction .420-426optical emission spectroscopy '" 21-30particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187Rutherford backscattering

spectrometry 628-636spark source mass spectrometry 141-150ultraviolet/visible absorption

spectroscopy 60-71voltammetry 188-196x-ray diffraction '" 325-332x-ray photoelectron spectroscopy 568-580x-ray spectrometry 82-101

Quantitative metallography. See Imageanalysis

Quantity of electricity, SI derived unit andsymbol for 685

Quantity of heat, SI derived unit and symbolfor 685

Quantity, symbol for change in 692Quantum mechanical tunneling process, field

ionization as 584Quantum mechanics

defined 680of electron spin resonance 254

Quantum number, defined 680Quantum theory. See also Quantum

mechanics.of scattered radiation 126-127

Quantum yields, fluorescence, structuraleffects on 74

Quartering, of samples 17, 165Quartz

hydrofluoric acid as dissolution medium .. 165as internal reflection element. 113JCPDS data for. 341sintering agent for 166

Quartz refractor plate, in polychromators 38Quartz tube atomizer, characteristics .48Quench-cracked AISI 4340 steel threaded

rod, overload failure of 511-513Quenching

defined, in atomic fluorescencespectrometry .46

of fluorescence 73, 79-80

RR. See Rare earths.R. See Radius of curvature.R203 group, elements precipitated in 168Rachinger correction 386Radial distribution function analysis 393-401

applications 393,398-401data reduction 396-398defined 680diffraction data 394-395estimated analysis time 393general uses 393instrumentation 395-396interpretation 398introduction 393-394limitations 393in liquid and amorphous materials .420related techniques 393samples 393, 398-401x-ray sources 395

Radian 685, 691Radiance, SI derived unit and symbol for ...685Radiant energy 62, 680Radiant intensity 680, 685Radiant power

exponential decay, as function ofconcentration 62

flux, defined 680intensity as 62as transfer of radiant energy '" .62

Radiation. See also Bremsstrahlung radiation;Synchrotron radiation; X-rays.

absorption and scatter, in x-rayspectrometry 84

continuum or bremsstrahlung, defined 83copper 326damage 253, 365, 583, 588defined 83electromagnetic 83electromagnetic, in x-ray spectrometry 83energy, absorbance vs 85-86as environmental health hazard 247in ESR analysis 254far-infrared, defined 673-induced changes, ion-implantation .484infrared 109, 114K« 326molecular polarization as source of 127monochromatic, in reflection

topography 366penetration into stress gradient, and

measurement errors 388polychromatic 97, 366in Raman spectroscopy 126-130sources, MFS 76sources, synchrotron radiation .413from tunable lasers 142ultraviolet, defined 683UVIVIS, molecular absorption as requirement

for fluorescence 73wavelength and energy theories of 83white, defined 325-326in x-ray range 85-86

Radiationless transition, and photoelectriceffect, in XPS development 568

Radical. See Free radicals.Radical ions 263, 265Radical production and decay, kinetics

of 265-266Radioactive decay

half-life, defined 244modes 244-245principles of 244scheme 292

Radioactive decay spectrometry 246Radioactive isotopes

radioanalysis of 243specific activity of 244

Index /743

Radioactive materialsnaturally occurring, radioanalysis of. 243requirements for 247

Radioactivitydecay modes 244-245defined . . . . . . . . . . . . . . . . . . . . . . . . . . . . .680detection and measurement 245-246of NAA samples 233remote analysis by electrometric titration

for " 202Radioanalysis 243-250

accuracy, precision, and sensitivity 246-247analytical procedure 247-249apparatus for, schematic 247applications 243, 249-250background and coincidence corrections 248chemical preparations 247defined 680detection and measurement of

radioactivity 245-246equipment 247-248estimated analysis time 243general uses 243half-life 244introduction 244limitations 243radioactive decay modes 244-245radioactive measurement 247-248related techniques 243sample preparation 248samples 243, 248-250

Radiochemical (destructive) TNAA elementalassay 233, 238-239

for iridium determination in Cretaceous-Tertiary boundary 240-241

Radio frequencyabbreviation for 691defined 680generators, analytic ICP systems 34, 37spectrometers, defined 680

Radio-frequency spectroscopy, defined 680Radioisotopes

analysis for 233decay rate 235defined 234, 680

Radionuclides. See also Radiosiotopes.activity of, SI unit and symbol for 685

Railroad rail head, residual stress distributionacross a flash-butt welded 391

Rainwater. See also Water.GFAAS analysis for silver 55

Raman band, defined 680Raman effect

experimental considerations 128-129fundamentals 126-128sampling 129-130

Raman line, defined 680Raman microprobe analysis

capabilities 516of pyridine adsorbed on metal oxide

surfaces 134Raman scattering, surface-enhanced 135-136Raman shift, defined 680Raman spectrometer

conventional 128with multichannel detector. 128

Raman spectroscopy 126-138anti-Stokes radiation 127applications 131-133bulk materials analysis by 126, 130-133capabilities 333capabilities, compared with infrared

spectroscopy 109defined 680estimated analysis time '" .126experimental utility 127-128and gas analysis by mass spectrometry,

compared 151information obtainable from 130



744/ Index

Raman spectroscopy (continued)for graphites 132-133and infrared spectroscopy, compared 127of inorganic liquids and solutions 7of inorganic solids .4-6in situ, laser excitation sources for 135introduction 126laser Raman microprobe 129lasers 129limitations 126, 135, 136for metal corrosion 134-135for metal oxides 130-131molecular optical laser examiner

(MOLE) 129molecular vibration 127monochromator-detector assembly

of. 128-129of organic gases 11of organic liquids and solutions 10of organic solids 9polarization 127for polymers 131-132Pourbaix diagram 135Raman effect. 126-130related techniques 126sampling 126, 129-130selection rules 127spectrometers for 128Stokes radiation in 127surface-enhanced Raman scattering 135-137

Raman spectrum, defined 680Random access memory (RAM) 92Random alloys, EXAFS analysis .407Random errors, in sampling 12Random samples, defined 12Rare earths

copper oxide, for carbon monoxide, carbondioxide removal 222

electron spin resonance and 262elements, laser-induced resonance ionization

mass spectrometry for 142ESR analysis of 262fluoride separations 169ICP-MS analysis of .40

Rasberry-Heinrich model, calibration of x-rayspectrometry 98

Rasterswith Auger spectrometer 554formation, and scan coils, SEM

microscopes .493image analysis scanners 310

Ratiometric instruments, MFS analysis 77Raw materials, industrial, sampling of 12-18Ray diagram, for lensing action .492Rayleigh scattering

and Compton scatter, x-rays 85defined 127, 680energy-level diagram 127in Raman spectroscopy 126-128from x-ray absorption 84

Rb z, single-crystal analysis of 355RBS. See Rutherford backscattering

spectrometry .RDF. See Radial distribution function

analysis.Reaction kinetics, analyses 109, 628Reaction products, identified 212, 628Read camera

as glancing angle 336schematic 336

Reagent chemicals, defined 680Reagents. See also Chemical reagents.

analytic methods for. 10chemical, analytic methods for 6-10chemical, defined 680contaminated, controlling for 12defined 680effect on analyte extraction 164elimination by NAA use 234

Karl Fischer 204process, AAS for trace impurities in .43pure, use in SSMS 144purity, in UVIVIS analysis 68-69as solvent extractants 170suitability, classical wet analysis 163trace impurities analyzed 31use of excess, for UVIVIS interferences 66

Real time, in x-ray spectrometers 92Reciprocal lattice, defined 680Reciprocal linear dispersion, defined 680Recoil-free fraction, as basis of Mossbauer

spectroscopy 287-288Reconstruction

LEED analysis 536surfaces, FIM/AP study of 583

Recovery, analysis of. .468-470Recrystallization

front, cementite particles pinning .471measurement and analysis by crystallographic

texture 357-364structures, analysis of .468-472studied by x-ray topography 365, 376textures, orientation relationships in 358

Red, methyl, as acid-base indicator. 172Redox. See also Oxidation; Oxidation-reduction

(redox); Reduction.completeness of reaction 164endpoint detection 164titrations 174-176

Red shift, defined 680Reducing agents, precipitation by 169Reduction

defined 680-oxidation reactions, classical wet chemistry

analysis of 163-164polarographic 191reversible, completeness of reaction as

function of potential for 209of species soluble in solution 208in voltammetry 189

Reductor, Jones 175Reed's vortex stabilization technique, use in

ICP-AES 32Reentrant, abbreviation for 691Reference electrodes

defined 680for ISE 185schematic of 186

Reference materials, defined 680Reference sphere, in stereographic projection,

grain orientation 358Reflectance

-absorption attachment, IRRASspectroscopy 114

defined 680specular infrared, for chemical surface

studies 177Reflection, wave theory of 83Reflection EXAFS detection technique .. .418Reflection grating, defined 680Reflection high-energy electron diffraction

acronym 689with Auger electron spectroscopy 554capabilities 536effect of grazing incidence 540instrumentation 539-540introduction 537measurements 539-540

Reflection spectrometers, FMR 270Reflection technique, thick-sample, for pole

determination 360Reflection topography

applications 366asymmetric 371Bragg case 366camera for 369Laue case .366polychromatic and monochromatic .366

Schulz and Berg-Barrett methods of ..368-369Reflux, defined 680Refraction, wave theory of. 83Refractive index 680, 690Refractory compounds, nitrous oxide-acetylene

flame atomizer for .48Refractory materials, high-silica, dissolution

medium for 165Refractory metals

field evaporation of 586grain-boundary embrittlement in, lAP

studies 599-600nitric/hydrofluoric acid as dissolution

medium 166powder or briquet sample preparation 93radiation-damaged, FIM studies of 588sodium peroxide fusion 167

Reinforcement, in x-ray spectrometers 88Relative sensitivity factor

abbreviation for 691LEISS 606use in SSMS 145

Relative standard deviation, defined 681Relative transmittance, defined 681Relaxation

parameter, ferromagnetic materials .. 275, 276pulse method of measuring times of 258saturation method of measuring times of ..258spin, rates of 275-276spin-spin 257in stress, due to layer removal 388as supplemental ESR technique 257-258surface atom, in single crystal. 628times, saturation and pulse methods of

measuring 258vibrational, abbreviation for 691

Relaxation parameter, as ferromagneticresonance application 275-276

Relaxation-time experiments, effects oftemperature on 257

Relay weld integrity, as gas analysisspectroscopy application 156

Reliability of measurements, and samplequality 12

Repeatability, in quantitative EPMA 525Replicas, extraction for TEM .452Replication, in sampling 12Reprecipitation and dissolution, as gravimetric

sample preparation 163Representative sample, defined 13Reproducibility, of electrode materials,

voltammetric monitoring for 189Research reactor, as common source for

low-energy TNAA neutrons 234Residual stress

arithmetically defined 385associated with failures caused by fatigue or

stress corrosion 380'defined 681determined by neutron diffraction .420distribution, longitudinal, in welded railroad

rail 391-392ferromagnetic resonance ' 267-276local variations produced by surface

grinding 390-391maximum, magnitude and direction produced

by machining 392measurement of. .425-426neutron diffraction analysis of. . .424, 425-426and percent cold work distributions caused by

stress-relieving heat treatment orforming . . . . . . . . . . . . . . . . . . . . . . . . . . .380

and percent cold work distribution intubing 390

and percent cold work distribution in beltpolished and formed Inconel 600tubing 390

profiles, minimum and maximumprincipal 392



Rutherford backscattering analysis ....628-636subsurface, and hardness distribution in

induction-hardened steel shaft 389-390subsurface, in steels 389-390surface, and hardness, on raceway of ball and

roller bearings 380surface compressive, uniformity

determined 380surface, nondestructive measurement for

quality control 380x-ray diffraction techniques 380-392

Residuesanalytical techniques for 177metal and alloy, isolation of 176refinement of. 176-177volatilization during ignition 163

Resinsanalytic methods for. 9ion-exchange, as sampling substrates 94ion-exchange, defined 675polyimide, curing mechanism 285polymer. 164

Resistance furnaces, high-frequency ..221-222Resolution

defined 681depth, AES 556depth, atom probe analysis 595detector (peak broadening) 519enhancement, methods for 116-117of features, SEM .490field ion microscope 588Ff-IR spectrometers 112high SEM, use in Jominy bar analysis 508lateral, atom probe analysis 595-596limits, SEM and optical microscopes,

compared .495liquid chromatography 651mass, LEISS analysis 605neutron diffraction .422SEM .494spatial. .448, 525, 595-596spectral, EOS and WOS compared 521-522of x-ray spectrometers 91

Resolution enhancement methods, lRqualitative analysis 116-117

Resonance. See also Electron spin resonance.complex, appearance of 255effect, RBS analysis 635equations, for single crystals 269field, defined 267

Resonance methodselectron spin resonance 253-266ferromagnetic resonance 267-276Mossbauer spectroscopy 287-295nuclear magnetic resonance 277-286

Resonance transitions, optical emissionspectroscopy 22

Restoration, substructure due to .469-470Retarding field analyzers, for AES

analyses 554Retention

parameters for defining 65Itime, defined 681

Retrofitting spark, imaging detectors for 144Reversed-phase chromatography

defined 681as LC mode 652-653separation of cations and anions 663

Reversed-phase ion chromatography,separation mode 663

Reversible electrode reactions, involtammetry 190-191

RF. See Radio frequency.RF generator, ICP systems 34, 37RHEED. See Reflection high-energy electron

diffraction.Rhenium

evaporation fields for. 587filament, gas mass spectrometer 153

highest oxide, titration of 173species weighed in gravimetry 172sulfuric acid as dissolution medium 165

Rhodiumdetermined by controlled-potential

coulometry 209evaporation fields for. 587gravimetric finishes 171as tube anode material, x-ray

spectrometers 90tube, from iron and plastic, Compton scatter

for 99Rhombohedral unit cells 346-348Ribbons, abraded, FMR study of 274Riboflavin, ESR studied 264Rietveld method

Nd2(Coo.•Feo.9)14B analysis by ..... .425-426in neutron powder diffraction .. .423, 425-426of x-ray or neutron diffraction data 344

Rimers, as blenders for samples 17Riming, of particulate samples 165Rimmed steels, sample dissolution for 176Ring diffraction patterns,

SAO/ATEM " " .. .436-437Rinse waters, acidity-basicity measured .... 172Rocking curves

defined 681gold single crystal 373grains, polycrystalline sample 374as intensity profiles 372polycrystal analysis 371-373profiles, for epitaxial films, differing

thicknesses 375Rock, TNAA detection limits for 237-238Rockwell hardness

abbreviation for 690diffraction-peak breadth at half height as

function of 387Rods

fiber textures in 359preferred orientation in 359

Roe formalismand Bunge formalism, compared 362complete set of angles for 359notation, Euler space in 361OOF coefficient determined 362for specifying orientation in crystallographic

measurement 359-361Roentgen, abbreviation for 691Rolled copper, lX- and l3-fibers in 363Rolled fcc materials, textures in 363-364Rolled sheet materials

expected pole orientations of preferredorientations 360

grain orientation 358preferred orientation in 359

Rollingreduction, OOF along fiber lines as function

of. 364textures, features in fcc materials 363-364

Rotary pumps, gas mass spectrometry 151-152Rotating platinum microelectrode ...204, 691Rotating sample cell, Raman analysis of

graphites 132Rotation axis, defined in crystal symmetry ..346Rotation, molecular, in Raman

spectroscopy 127Rotation pattern, single-crystal diffraction ..330Rowland circle mount, polychromators

with 23RPE. See Rotating platinum microelectrode.RS. See Raman spectroscopy.RSF. See Relative sensitivity factor.r space, Fourier transform to .412-413Rubber

analysis, nitrile sheath vs neoprene sheath 648ESR for. 263

Rubidiumcations, in glasses, Raman analysis 131

Index / 745

epithermal neutron activation analysis 239in insect eggs, GFAAS analysis 55organic precipitant for 169Raman vibrational behavior. 133species weighed in gravimetry 172TNAA detection limits 238

RubyESR studied 264fusion with acidic fluxes 167

Rutheniumdetermined by controlled-potential

coulometry 209distillation 169evaporation fields for 587gravimetric finishes 171

Rutherford backscatteringspectrometry '" 628-636

applications 628,631-636backscattering , 629capabilities 610capabilities, and FIM/AP 583channeling effect in 630-631collision kinematics 629defined 681energy loss 630equipment for. 631estimated analysis time 628general uses 628of inorganic solids .4-6introduction and principles 629limitations 628related techniques 628resonance effect 635samples 628, 632-636scattering cross section 629-630sensitivity 630

Rutilebright-field and dark-field images of

annealing twin in .443in ceramic waste form simulant, EPMA

analysis for 532-535sintering agent for 166

5(J' phase, orientation relationship in ... .453-454SACP. See Selected-area channeling pattern.SAD. See Selected-area diffraction.SADP. See Selected-area diffraction pattern.Safety

in hydrogen sulfide use 169in sample dissolution 165-167

Saha equation 24Salting, as AAS flame modification 54Salting up

with concentric nebulizers 35with total consumption burners 28

Saltsnonstoichiometric, single-crystal analysis ..355in sinters and fusions 166

SAM. See Scanning Auger microscopy.Samarium

epithermal neutron activation analysis(ENAA) 239

TNAA detection limits 237Sample cavity, ESR spectrometer 256Sample cell, rotating 132Sample dissolution. See also Dissolution.

mediums for 165, 166, 168Sample matrix 83, 162, 168-170Sample preparation. See also Samples;

Sampling.analytical electron microscopy .450-453for classical wet analytical

chemistry " 165-167elemental and functional group analysis ...213field ion microscopy 584-586for image analysis 309-310,313-314



746/ Index

Sample preparation (continued)gas chromatography/mass

spectrometry 644-645microbeam analysis 529for microstructural analysis of ion-implanted

alloys .484techniques for selected materials 586x-ray diffraction residual stress

techniques 384-385x-ray photoelectron spectroscopy 574-576for x-ray spectrometry 93-95as XRPD source of error 341

Samples. See also Sample preparation;Sampling.

aciditylbasicity measured in 172aqueous, optical emission spectroscopy

for 21briquets, for x-ray spectrometry 93-94bulk, Rutherford backscattering

spectrometry 631charging, AES 556composite 13defined . . . . . . . . . . . . . . . . . . . . . . . . . . 681dissolution ..... , ... .4,56-57, 163, 165-167as error source in image analysis 313fluorescence of 387fusion of 94geometry, effect on XRD analysis 388gross, defined 674high vapor pressure, AES 556holders, MFS analysis , 76-77identification 17infinitely thick/thin, x-ray spectrometry 93labeling and recording of 13laboratory, defined 676matrix 83, 162, 168-170mechanical strength of. 587metallurgical, precision analysis by

electrogravimetry 197minimum number. 14minimum size 14multiphase 516, 529-530NAA, radioactive contamination of 236particulate, preparation of 165positioning, XRD analysis 385powder, fluxes for fusing 167powders, for x-ray spectrometry 93-94preservation 12, 15, 16pretreatment : 12, 15quality of 12radioactive, remote analysis by electrometric

titration 202representative 13rotation of 130, 132sectioning, for OM analysis 300size and form, importance in classical wet

chemistry 162size and homogeneity of 13small diameter, surface stress measurement

of. 385solid, for x-ray spectrometry 93storage 12, 15systematic 12-13temperature control of 257thin-film, x-ray spectrometry 95types of 12-13unknown, AAS for. .46variability of. 12

Sample tube, pure quartz, in ESRanalysis 256

Sampling. See also Sample preparation;Samples , 12-18

accessories, infrared spectroscopy 112of bulk materials 13-14composite samples 13costs of 15in de arc 25defined 12, 681and excitation, in emission sources 25

field sampling 16filter, applications 94by Grimm glow discharge source 27isokinetic, devices for 16materials in discrete units 14model of operation for 13plan 13-15practical aspects of 15-16preliminary considerations 12protocol. 13, 15-16quality assurance for 17and the Raman effect 129-130random 12representative samples 13resources, optimizing 15sample contamination 16sample damage 15-17sample discrimination 16sample preservation 16sampling protocol 15-16segregated (stratified) materials 14specific materials 17by sputtering 27statistics 12-15strategy, microbeam analysis 529-530subsampling 13, 15substrates, for x-ray spectrometry 94techniques, infrared spectroscopy 112-116uncertainty 12, IS, 17volume, by neutron diffraction .423

Sampling boat, for flame AAS .49SANS. See Small-angle neutron scattering.Sapphire

fusion with acidic fluxes 167as internal reflection element. 113

SAS. See Small-angle scattering.Satellites, shake-up 572Satellite spots, as fine structure effect .438Satellite lines 86, 521Saturated calomel electrode

in amperometric titration 204defined 681as reference electrode 189

Saturation and relaxation, in ESR 257-258Saws, as sampling tools 16SAXS. See Small-angle x-ray scattering.S-band microwave frequency, use in ESR

analysis 255Scan coils and raster formation, SEM

microscopes .493Scandium

fluoride separation 169species weighed in gravimetry 172TNAA detection limits 238weighed as the fluoride 171

Scan lines, image analysis scanners 310Scanners, image analyzers 310-311Scanning Auger microscopes

with secondary electron or x-raydetectors 501

and SEM, compared 509-510Scanning Auger microscopy

defined 681magnetostrictive alloy analysis by 510

Scanning electron beam instrumentscompared 501sample volume .499-500signals generated by .497-499

Scanning electron microscopesarea channeling analysis with 357basic components .491depth of field .496-497detectors and image formation in .493-494double-deflection system .493electron column .431electron gun for. .491-492electron optical column, compared with TEM

column , .431with electron probe microanalyzer 517

image contrast in 500-504as input devices for image analyzers 310lenses .492for particle image analyses 318resolution limits .495-496and SAM, compared 509-510scan coils and raster formation .493with secondary electron and x-ray

detectors 501vacuum pumping system .491

Scanning electron microscopy .490-515advantages .494-497of aluminum/iron and aluminumlbrass

interfaces 531-532applications .490, 508-514capabilities 309, 365, 402, 429, 536capabilities, and FlM/AP 583capabilities, compared with optical

metallography 299cathodoluminescence 507defined 681electron beam induced current. 507electron channeling patterns and

contrast 504-506general uses .490image contrast. 500-504image morphology 309of inorganic solids, types of information

from 6integrated circuit problems solved

by 513-514introduction .491limitations .490microscope for .491-494of organic solids, information from 9related techniques .490and SAM 509-510samples .490, 508-514scanning electron beam instruments . .497-500special techniques with 506-508voltage contrast. 506-507

Scanning log ratio, analysis by 144Scanning monochromators, radiation

detection 38Scanning transmission electron

microscopes 501Scanning transmission electron microscopy

capabilities .490defect analysis by .464-468defined 681lenses for .432profiles, diffusion interfaces .478

Scansdaughter ion 646in ESR spectrometers 255natural loss, GC/MS 646-647parent ion 646

ScatterCompton 84ratio of Compton-to-Rayleigh 84wave theory of 83x-ray, defined 84

Scattering. See also Backscattering; Scatter.in AFS atomizer .46anti-Stokes 126-128atomic absorption spectrometry 51-52binary collisions 604contributions to scattered intensities 604conversion electron Mossbauer 293-294cross section, in Rutherford backscattering

spectrometry 629cross section, symbol for 692defined 681effect in MFS analysis 77-78elastic, ATEM .432-433electron, defined 672electron, volume of .434factor, of atom 349inelastic .433, 540, 674



infrared 117light- 126-130molecular 126-130rnultiple-, in EXAFS .410neutron and x-ray, compared .421pathological electron, effects in microbearn

analysis 530phase differences from different electrons

within an atom 328photoelectron, in EPMA energy-dispersive

spectrometer 518principles, LEISS 604process, in Auger electron production 550Raman 135-136Rayleigh " 126-128small-angle x-ray and neutron .402-406Stokes 126-128types of curves .404x-ray anomalous .407

Scattering cross section, symbol for 692Scavenging, chemical .46SCC. See Stress corrosion cracking.SCE. See Saturated calomel electrode.Scheelite, sintering agent for 166Schlapfer and Bukowski method, for free lime

content 179Schiiniger combustion 167, 681Schiiniger flask method

for common elements 215for elemental analysis 215estimated analysis time 215limitations 215for sample dissolution 167use in ion chromatography 664

Schottky barrier technique, EBIC arrangementusing '" " 507

Schulz method, reflection topography ..368-369Scintillation

counter, diffractometers 351detectors 88-89

Scoops, plastic, as sampling devices 16Scott spray chamber, for analytic rep

systems 35Scraping, of samples 575Scrap metal, silver, analysis of .41SE. See Secondary electrons.Seals, shear fracture studies of

Kovar-glass 577-578Search/match methods, for unknown phases or

particles .455-459Seawater, boron determined in 205Secondary electron detectors

for AES analysis 554image contrast with SEM 501-502sample configurations .495with scanning electron beam instruments ..501types of electrons detected 502

Secondary electron emissionas low-energy .433-434surface, AES analysis for 549

Secondary electrons. See also Electrons.abbreviation for 691Auger ejection 86and backscattered electrons, yields for 502defined 681emission .433-434, 549images of 554, 558measuring instruments 554micrographs, beryllium copper alloy 559peak intensity .498-499production and x-ray photon emission 86signal generation 500STEM mode, signal detector .435

Secondary iondefined 681imaging, schematic diagrams 622

Secondary ion mass spectroscopy 610-627applications 610, 622-626artifacts, effects of 619

with Auger electron spectroscopy 554capabilities 516, 517, 549, 568, 603capabilities, and FIM/AP 583capabilities, compared with classical wet

analytical chemistry 161defined 681depth profiles 617-620detection limits 622elemental in-depth concentration profiling

by 610and EPMA, compared 516,517estimated analysis time 610general uses 610hydrogen analysis by 610images, schematic diagrams 622of inorganic solids .4-6instrumentation 613introduction 611ion imaging 621isotope abundances by 610limitations 610principles, schematic 611quantitative analysis 620-621related techniques 610samples 610, 622-626secondary ion emission 612secondary ion mass spectra 615-617sensitivity enhanced 618sputtering 611-612surface compositional analysis by 610system components 613-615

Secondary-target excitation, x-rayspectrometers 89

Secondary x-rays, defined 681Second, as sr base unit, symbol for. 685Second-order polynomial, fit of intensity vs

concentration 97Second-phase distribution, SIMS

analysis 610Second-phase imaging 309, 490Second-phase inclusions


electron probe x-ray microanalysis 516-535field ion microscopy; 583-602scanning electron microscopy .490-515small-angle x-ray and neutron

scattering .402-406x-ray diffraction 325-332

Second-phase particlesand field evaporation 587volume fraction, by autocorrelational

analysis 594Second-phase testing

isolation 176-177methods 177purification 177residue refinement and analysis 176-177

Sections, for metallographic analysis 300, 303Sector analyzers, AES analysis 554Seeman-Bohlin x-ray diffractometer 337Segment, defined 681Segregated (stratified) materials, sampling .. 14Segregation

of alloy and compound constituents tosurface 603

of alloy elements and impurities todislocations and interfaces 583

of binary/ternary trace elements in solids ..544effect in creep strengthening 598grain-boundary .481-484, 610interfacial, in molybdenum 599in uranium isotopes, radioanalytic

measurement. 243of lead to surface of tin-lead solder 607-608LEED analysis of. 536manganese, dual phase steel .483solute, AES analysis 549surface 564-566, 583, 593

Index /141

Selected-area channeling patternsarrangement for 506for pearlite growth 508-509for preferred crystallographic growth 509as SEM technique 505-506

Selected-area diffraction pattern,defined 681

Selected-area diffractiondefined 681Kikuchi patterns .437-438patterns, and CBEDP, compared .439, 441ring patterns .436-437spot patterns '" .437,438,440TEM .436-438

Selected complexation 65-66Selection rules

effect on x-radiation K lines 86Mossbauer spectroscopy 288

Selective combustion 223-224Selective vaporization, in arc sources 25Selectivity

coefficient, defined 165in controlled-potential coulometry

analysis . . . . . . . . . . . . . . . . . . . . . . . . . . .208defined 681determining electrode 182-183of fluorescence analysis 76UVIVIS 68of x-ray spectrometry 96

Selectivity coefficient, defined 165Selenium

determined in natural waters .41distillation 169epithermal neutron activation analysis 239gaseous hydride, for ICP sample

introduction 36gravimetric finishes 171quartz tube atomizers for .49redox titration 174, 175reduction, by iodimetric titration 174sample modification, GFAAS analysis 55in semiconductor alloys, electrometric titration

for " '" .206sulfuric acid as dissolution medium 165TNAA detection limits 238volatilizing 166

Self-absorptiondefined 681emission profile of 22in glow discharges 28

Self-deconvolution, Fourier, as method ofresolution enhancement 116

Self-electrode, defined 681Self-ionization, of water 203Self-reversal

defined 681in emission spectroscopy 22, 25

SEM. See Scanning electron microscopy.Semiautomatic digital image analyzer '" .310Semiconductor devices, defect analysis and

quality control .490Semiconductor materials. See also

Semiconductors; Semiconductors.characterization of.

diffused or ion-implanted, SIMS analysisof. 610

interdiffusion analyzed 583metallization 583oxidation, FIMiAP study of 583prXE analysis of 102pulsed laser atomic probe analysis of 597reconstruction of surfaces 536selenium and tellurium in, by electrometric

titration 206SSMS analysis of high-purity silicon for .. 141

Semiconductors. See also Semiconductormaterials; Semiconductors,characterization of.

analytic methods for. .4



748/ Index

Semiconductors (continued)compound, ECAP/PLAP analysis

of. 598, 601-602field evaporation for. 590FIM images of 589-590intrinsic, sample preparation for FIM 584rocking curve analyses of 371ternary 3:5, local composition fluctuations

in 601-602x-ray topographic analysis 366

Semiconductors, characterization of. See alsoSemiconductor materials; Semiconductors.


atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis 516-535electron spin resonance 253-266extended x-ray absorption fine

structure .407-419field ion microscopy 583-602inductively coupled plasma atomic emission

spectroscopy 31-42infrared spectroscopy 109-125low-energy electron diffraction 536-545low-energy ion-scattering

spectroscopy 603-609neutron activation analysis 233-242neutron diffraction .420-426optical emission spectroscopy 21-30particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187Raman spectroscopy 126-138Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-5 ISsecondary ion mass spectroscopy 610-627single-crystal x-ray diffraction 344-356spark source mass spectrometry 141-150ultraviolet/visible absorption

spectroscopy 60-71voltammetry 188-196x-ray diffraction 325-332x-ray photoelectron spectroscopy 568-580x-ray powder diffraction 333-343x-ray spectrometry 82-101x-ray topography 365-379

Semikilled steels, sample dissolution for. ... 176Semimetallic elements, partitioning oxidation

states in 178Semiquantitative analysis. See also

Semiquantitative analysis. methods for.dc arc emission spectroscopy 25electrographic 202of inorganic gases 8of inorganic liquids and solutions, methods

for 7of inorganic solids, applicable analytical

methods .4-6of organic solids and liquids, techniques

for. 9, 10Semiquantitative analysis, methods for. See

also Semiquantitative analysis.analytical transmission electron

microscopy .429-489Auger electron spectroscopy 549-567electron probe x-ray microanalysis 516-535electron spin resonance 253-266field ion microscopy 583-602gas analysis by mass spectrometry 151-157gas chromatography/mass

spectrometry 639-648infrared spectroscopy 109-125ion chromatography 658-667

liquid chromatography 649-659low-energy ion-scattering

spectroscopy 603-609molecular fluorescence spectrometry 72-81Mossbauer spectroscopy 287-295neutron diffraction .420-426optical emission spectroscopy 21-30particle-induced x-ray emission 102-108scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627spark source mass spectrometry 141-1 SOultraviolet/visible absorption

spectroscopy 60-71x-ray diffraction 325-332x-ray photoelectron spectroscopy 568-580x-ray powder diffraction 333-343x-ray spectrometry 82-101

SEM microscopes. See Scanning electronmicroscopes.

SEM special techniquescathodoluminescence 507electron beam induced current. 507magnetic contrast 506signal processing 507-508specimen current detectors 506voltage contrast. 506-507

Sensitivityatomic, empirical factors 574detection, AES 556and detection limits, UVIVIS 70elemental, LEISS analysis 605-606of radioanalysis 246-247ofRBS 630relative, LEISS 606of SIMS, enhanced by oxygen primary ion

beam 618surface, LEISS 605surface, XPS analysis 569-570wavelength-dispersive spectrometer 521

Sensitization, chromium, in Inconel . .483, 600Separation

automated 199of cadmium and lead, by internal

electrolysis 201by complexation, for UVIVIS

interferences 65cupferron 169direct chemical, for UVIVIS

interferences 65by distillation 169effectiveness, measure of. 164efficiency measured by radioanalysis 243of interfering elements, in high-temperature

combustion 222ion exchange 164-165of metals in electrogravimetry, emf conditions

for 197-198of praseodymium and neodymium 249-250precipitation 168principles, ion chromatography 658-659and quantitative determination of metal

ions 200-201of RDF into pair distribution

functions 397-398sink/float density 177techniques, classical wet

chemistry 165, 168-170Separation science, defined 164Separation techniques

classical wet chemistry 162, 165, 168-170hydroxide 168ion-exchange chromatography 168magnetic 177paper chromatography 168for solids 165

Sequential multielement analysisdirect-current plasma .40monochromators for 37, 38scanning monochromator for 38

and simultaneous multielement analysis,combined 38

Sequential wavelength-dispersive x-rayspectrometers, automated 87

SERS. See Surface-enhanced Raman scattering.Serum glutamate pyruvate transaminase,

reaction rate analysis 70Sewage, potentiometric membrane electrode

analysis of 181SFC. See Supercritical fluid chromatography.SG. See Spin glass.Shake-up satellites, in XPS analysis 572Shear fracture, of Kovar-glass seals 577-578Sheet, normal direction, abbreviation for. ...690Sheet metal materials

determining pole figures in 360diffraction in 360effects of steel surface carbons on paint

adherence 224texture of 363

Short distances, RDF parametersdefining 396-397

Short-range order .407, 691Shot peening

compressive residual stresses 380surface stresses 383

Siemensabbreviation for 691defined 681as IC unit of conductance 659as SI derived unit, symbol for 685

Sievingof particulate samples 165in sampling 16

Sigma bonding, defined 681Sigma phase, orientation relationship

in .453-454Signal '.

averaging, for fluorescence noise 130detectors .434-435generation, electron beam .498-500processing 507-508, 631scanning electron beam instrument 501-to-noise ratios 68, 409, 413, 681

Signal detectorsanalytical transmission electron

microscopy .434-436positioning, in AEM microscope column . .434secondary electrons (STEM mode) .435transmitted and scattered electrons (TEM

mode) .434-435transmitted and scattered electrons (STEM

mode) .435Signal-to-noise ratio

defined 681EXAFS .409, 413UV/VIS 68

Silica-aluminas 130background fluorescence of. 130platinized, for removal of carbon

monoxide/dioxide in high-temperaturecombustion 222

Silica glassRDF analysis 395-399x-ray diffraction patterns for 395, 398-399

Silicatesfluoboric acid as dissolution medium 165glasses, bonding topologies in 393hydrofluoric acid as dissolution medium

for 165sintering 166

Silicide formation, RBS analysis 628Silicon

[111) single-crystal, Kikuchi diffractionpatterns from .438

analysis of phosphorus ion-implantationprofile in 623-624

with arsenic, ESR studies 263



boule, alignment for cutting alongcrystallographic planes 342

crystal, lithium-doped, for EPMA 519crystals, spin-dependent recombination

analysis of. 258depth profiles for LPCVD thin films on 624determined by l4-MeV FNAA 239evaporation fields for. 587AM sample preparation of 586Ff-IR spectra of. 123high-energy neutron irradiation of. 233high-purity, under oxygen bombardment, ion

microscope 615as internal reflection element. 113photometric analysis methods 64prompt gamma activation analysis of 240qualitative analysis of surface phase

on 341-342RBS profiles of arsenic in 632in simple steels, partitioning oxidation states

in 178SIMS analysis of phosphorus ion-implantation

profile in 623species weighed in gravimetry 172SSMS analysis of impurities in

high-purity 141surface segregation, temperature dependence

of. 565wafers, analysis of oxygen in 122

Silicon carbides, effect of carbon KVVlineshapes on 553

Silicon wafers, oxygen determined in .. 122-123Si(Li) detectors. See Lithium-drifted silicon

detectors.Silver

anode x-ray tube 90in cloud-seeded rainwater, GFAAS

analysis 55Compton-scattered 84current-time curves in coulometric

determinations of 210deposition 199determined by controlled-potential

coulometry 209electrodes, oxidation in alkaline

environments 135evaporation fields for. 587film, grown on mica, analysis of grain size

in .. '" '" 543-544film grown on mica, grain size of 543-544gravimetric finishes 171high-purity, SSMS analysis 144internal electrolysis of 200powders, catalytic oxidation by SERS

analysis 136scrap metal .41as SERS metal 136species weighed in gravimetry 172texture orientations 360TNAA detection limits 238Volhard titration of 173volumetric procedures for 175weighed as the chloride 171x-ray tube emission, spectrum of 90

Silver bromide, as internal reflectionelement 113

Silver chloride, as internal reflectionelement 113

Silver scrap metal, analysis of .41Simple-SIMS instrument, for qualitative

analysis 613Simplified impulse and inductive inert gas

fusion furnaces 228SIMS. See Secondary ion mass

spectroscopy.Simultaneous multielement analysis

direct-current plasma .40direct-current plasma atomic emission

spectroscopy .43

inductively coupled plasma atomic emissionspectroscopy 31-42, 43

neutron activation analysis 233-242and sequential multielement analysis,

combined 38Sin2

'" techniqueplane-stress elastic model 384six-angle, residual stress pattern 386

Single-angle technique, plane-stress elasticmodel. 383-384

Single-column chromatography anion, forsuppression of backgroundconductivity 660

Single-column chromatography ion, withconductivity detection 660-661

Single-crystal diffraction, basic principlesof. 350

Single crystalline graphite, Ramananalysis 132

Single-crystal neutron diffraction .424-425Single crystals. See also Crystals.

of aluminum, spot diffraction patternfrom .437

defined 681diffraction experiments with 330for ESR study 256EXAFS analysis .410experiment with monochromatic beams 330lattice location of impurities in 628NaC!, rotation pattern for 330neutron diffraction .424orientation by XRPD analysis 333orientations determined 357resonance equations for 269study of near-surface defects in 633surface, density of steps determined 544surfaces, EXAFS for orientation adsorbed

molecules on .407unit mesh size and shape of overlayer

adsorbed on 544Single-crystal topography, as x-ray diffraction

radiography 330-331Single-crystal x-ray diffraction 344-356

accuracy and precision 352applications 344, 353-355assumptions of 352capabilities 333, 393crystal diffraction 346crystallographic problems 352-353crystal structure definition 348crystal symmetry 346diffraction intensities 348-349estimated analysis time 344experimental procedure 351-352general uses 344introduction and principles 345-346limitations 344, 352-353phase problem 349-351related techniques 344samples 344, 351, 353-355space groups 347unit cells 346-347

Single-exposure technique, plane-stress elasticmodel 383

Single monochromators, stray light rejectionfor 129

Single-phase materialsEPMA compositional analysis 516image analysis 309

Single scattering approximation, in EXAFSanalysis .409-410

Single scattering formalism, in EXAFSanalysis .407, 417

Single-stage extraction replicas, for small-particle analysis .452

Sink/float density separations, for high-carbonsteels 177

Sinters, solid sample digestion by 166-167Siphon, use in electrogravimetry 200

Index /749

Site symmetry, determined .407SI units

base, supplementary, and derived 685guide for 685-687prefixes, names and symbols 687

Size. See also Particle size.of crystal, as x-ray diffraction analysis 325measurements with image analysis 315

Size-exclusion chromatography 654, 681Sizing, of particulate samples 165Slags

analysis of oxidation states in 162analytic methods applicable 6partitioning oxidation states in 178sodium peroxide fusion for 167

Sliding, material transfer during 566Slip

effect on texturing 358in FIM samples 587lines, topographic methods 368

Slit width, UVlVlS 68Slow neutron capture 234Sludge treatment, constant conditions

maintained by electrometric titration....202Slurries, solid-sample Babington-style

nebulizers for 36Small-angle neutron scattering. See also

Small-angle x-ray and neutronscattering .402-406

analysis of ceramics .405analysis of glasses .405analysis of metals .405analysis of polymers .405

Small-angle scattering. See Small-angle x-rayand neutron scattering.

Small-angle x-ray and neutronscattering .402-406

applications .402, 405estimated analysis time .402experimental aspects .402-403general uses .402introduction .402related techniques .402samples .402theoretical aspects .403-405

Small-angle x-ray scattering .402-406analysis of ceramics .405analysis of glasses .405analysis of metals .405analysis of polymers .405of organic solids, information from 9

Small-particle examination, samplepreparation, ATEM .452

Smearing, cause from line source .403Smith/Hieftje system, AAS spectrometers 52Snell's law, of light refraction 113Sodium

acid-base titration 173cations, in glasses, Raman analysis 131flame emission sources for 30as flux 167fusion, crucibles for. 167ions, exchanged in water softeners 658-659as sample contaminant. 236species weighed in gravimetry 172TNAA detection limits 237

Sodium bisulfate, as acidic flux 167Sodium borohydride, as reductant .49Sodium chloride, as analyzing crystal. 88Sodium diethyldithiocarbamate, as

extractant 170Sodium hydroxide, as precipitate 168-169Sodium oxide, in binary phosphate glasses .. 131Sodium peroxide

fusions 166-167as sintering agent 166

Sodium tetrabnrateas flux 167glass-forming fusions with 94



750/ Index

Sodium tetrahydroborate, for hydridegeneration 36

Sodium tetraphenylborate, as narrow-rangeprecipitant. 169

Softwarefor calibration, x-ray spectrometers 98empirical correction, x-ray spectrometry .. 100for ICP-AES computer systems 39

Soft x-rays, defined 83Soils

molecular structure and orientation determinedin 109

potentiometric membrane electrodeanalysis 181

TNAA detection limits for. 237Solar spectrum, and AAS .43Solder

analysis of. 179high-temperature, elemental mapping of ..532segregation of lead to surface 607-608

Solid angle, SI base unit and symbol for 685Solid crystalline membrane electrodes 182Solid-electrode voltammetry, capabilities ..207Solidification, studies of. 365Solids. See also Solids. characterization of.

acid mediums for digesting 166EPMA elemental analysis 516IC analysis of 663-664inorganic, analytic methods for .4meltable, as IR samples 112-113organic compounds, ESR studied 263phase composition determined 126in production and quality control, XRS

analysis for 83pure , 129subdividing, wet chemical analysis techniques

for 165transition series elements identified 253-266XRS analysis of 93

Solids, characterization of. See also Solids.analytical transmission electron

microscopy .429-489atomic absorption spectrometry .43-59Auger electron spectroscopy 549-567classical wet analytical chemistry 161-180controlled-potential coulometry 208-211crystallographic texture measurement and

analysis 357-364electrochemical analysis , 181-211electrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis 516-535electron spin resonance 253-266elemental and functional group


structure .407-419ferromagnetic resonance 267-276field ion microscopy 583-602gas chromatography/mass


spectroscopy .. , 31-42infrared spectroscopy 109-125ion chromatography 658-667liquid chromatography 649-659low-energy electron diffraction 536-545low-energy ion-scattering

spectroscopy 603-609molecular fluorescence spectrometry 72-81Mossbauer spectroscopy 287-295neutron activation analysis 233-242neutron diffraction .420-426nuclear magnetic resonance 277-286optical emission spectroscopy 21-30optical metallography 299-308particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187radial distribution function analysis ...393-401

Raman spectroscopy 126-138Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515secondary ion mass spectroscopy 610-627single-crystal x-ray diffraction 344-356spark source mass spectrometry 141-150ultraviolet/visible absorption

spectroscopy 60-71voltammetry 188-196x-ray diffraction 325-332x-ray photoelectron spectroscopy 568-580x-ray powder diffraction 333-343x-ray spectrometry 82-101x-ray topography 365-379

Solid sample analysis 36, 113Solid-state electronic device materials, x-ray

topographic studies of 365, 376Solid-state infrared detection system .....223Solid-state phase transformations,

characterized 333Soller collimator, WDS spectrometers 87Soller slit, use in topographic

methods 370, 374, 375Solubility

extended, of iron in aluminum 294-295in gravimetric analysis 163

Solutes. See also Solution analysis; Solutions.defined 682elemental PIXE analysis 102segregation in 549-solute equilibria 188

Solute-solvent equilibria, voltammetricanalysis 188

Solution analysis. See also Solutes; Solutions.ATR spectroscopy 113chemical, by controlled-potential

coulometry 207to determine bonding distance, coordination,

neighbors .407electrometric titration 202-206elemental, AAS as .44element transition series identified

by 253-266gravimetric, of reagents 163ICP-AES as 34of structure 188

Solutionsaqueous, containing nickel and cobalt ions,

spectra compared 65aqueous, use in ion chromatography ..658-667colored, electrometric titration analysis

of. 202defined 682inorganic, analytic methods for 7liquid, analytic methods for. 7molal, abbreviation for 690normal, abbreviation for 690organic, analytic methods for 10preparation of known 162turbid, electro metric titration for 202very dilute, electrometric titration for 202

Solvent extractionclassical wet chemical analyses 164by methylisobutyl ketone 169separations, common 170techniques 170using ethyl ether. 169

Solventsanalytic methods for. 10defined 682effect in MFS 77effects in flame emission spectroscopy 29evaporation, as IR sample 112ICP-AES for trace impurities in 31for ion chromatography sample

preparation 663liquid chromatography analysis for low-level

organic contaminants 649

nonpolar, effect in extraction 164purity, in UVIVIS analysis 68-69sample preparation, x-ray spectrometry 95-solute equilibria, voltammetric analysis .. 188

SOR Ring, as synchrotron radiation source . .413Space groups

230, relation to crystal symmetry and crystalsystems 348

and atomic symmetry 347atoms residing in 348for defining crystal structure 348identification for single-crystal analysis 351of recrystallized organic polysulfide 353

Spallation neutron sources, for neutrondiffraction .421

Sparging, dissolved oxygen removal by 204Spark, defined 682Sparking off 26Spark source mass spectrometry 141-150

applications 141, 146-150basis of technique 141-142defined 682depth profiling 142electric and magnetic sectors 143estimated analysis time 141general elemental surveys 144-145general uses 141of inorganic solids .4-6instrumentation 142-143internal standardization techniques 145introduction 141ion detection methods 143-144isotope dilutions 145-146limitations 141mass spectra 144neutron activation analysis and,

compared 233quantitative elemental measurement :'. 145-146related techniques 141, 142samples 141, 146-150

Spark sourcesapplications 29controlled waveform 25, 26high-voltage, defined 25parameters 26

Spark spectrometer, calibration 26Spark volatilization, for solid sample

analysis 36Spatial distribution

of constituents, EPMA mapping of ...525-529of elemental species, SIMS analysis for. ..610

Spatial resolutionatom probe analysis 595-596quantitative EMPA 525x-ray, effect in microanalysis .448

SPEAR. See Stanford Position ElectronAccelerator Ring

Speciationof inorganic gases, analytic methods

for 8of inorganic solids, analytic methods to

determine 5-6of organic solids and liquids, techniques

for. 9, 10population, in sampling 13

Specification compliance, image analysisfor 309

Specific energy, SI derived unit and symbolfor 685

Specific gravityof gases, defined 682of solids and liquids, defined 682

Specific heatconversion factors 686SI derived unit and symbol for 685

Specific volume, SI derived unit and symbolfor 685

Specimen current detectors, as SEM specialtechnique 506-508



Spectra. See also Spectrum.characteristic 325-326corrected, for MFS 77electromagnetic, x-radiation in high-energy

region of 83energy-dispersive, sum and escape peaks

in 520ESR absorption 260excitation and emission, MFS analysis ..74-75gamma-ray 235infrared, defined 674LEISS, in qualitative analysis 604-605Raman accessibility to low-frequency regions

of. 133resonance 254of silver x-ray tube emission 90wavelength-dispersive, stainless

steel 87, 88x-ray, EPMA measurement 518-522

Spectral background, defined 682Spectral distribution curve, defined 682

of synchrotron radiation from SPEAR .41ISpectral interferences. See also Interferences.

with flame emission sources 30in flame spectroscopy 29in ICP-AES 33-34

Spectral line, defined 682Spectrallineshapes, in infrared spectra 116Spectral order, defined 682Spectral peak overlap

Auger electron spectroscopy 556optical emission spectroscopy 22

Spectral resolution, EDS and WDS,compared 521

Spectral-stripping techniques, as lR qualitativeanalysis 116

Spectrochemical analysisatomic absorption spectrometry as .43atomic emission as .44defined 682

Spectrofluorometer, double-beam 77Spectrogram, defined 682Spectrograph, defined 682Spectrographic analysis, of residues 177Spectrometers

AAS double-beam 50atomic absorption .43, 45, 50-52Auger, cylindrical mirror analyzer in 554continuous-wave NMR 283curved crystal, x-ray spectrum of '" ..517defined 682defocusing, effects of 527dispersive and Ff-lR, infrared reflection-

absorption by 114echelle, for direct-current plasma .40electron, for AES analysis " 554for elemental mapping 527-528emission, defined 673energy-dispersive x-ray 89-93,519-520ferromagnetic antiresonance 271Fourier transform 38-39Ff-IR 112gas mass 151-156high-resolution, and spectral interferences ..33inert gas-purged 37infrared . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117magnetic and detector, for EELS .435microwave 254-255, 270-271monochromators 38-39photodiode arrays 38polychromators 37-38pulse NMR 283Raman 128reflection, for FMR 270scanning monochromator 38simultaneous x-ray fluorescence 162spark source mass 142time-of-flight mass 142, 591with Triplemate device 129

vacuum 29, 41wavelength-dispersive

x-ray 87, 89-93, 527-528WDS vs EDS 527-528Zeeman-corrected 52zero-dispersion double 129

Spectrometrygas analysis by mass. " 151-157gas chromatography/mass 639-648molecular fluorescence 72-81Rutherford backscattering 628-636spark source mass 141-150x-ray 82-101

Spectrophotometersdefined 682dispersive single-beam 67double-beam, block diagram 67dual-beam dispersive 67-68

Spectrophotometric detection 661, 663ion chromatography with 661

Spectrophotometric titrations 70Spectrophotometry, indirect 70Spectroscopes, defined 682Spectroscopy

attenuated total reflectance 113-114Auger electron 549-567categories of. 264diffuse reflectance 114electron or x-ray methods of 549-580inductively coupled plasma atomic

emission " 31-42infrared 109-125low-energy ion-scattering 603-609mass 141-157Mossbauer 287-295optical and x-ray 21-138optical emission 21-30Raman 126-138secondary ion mass 610-627ultraviolet/visible absorption 60-71x-ray photoelectron 568-580

Spectrum. See also Spectra.defined . . . . . . . . . . . . . . . . . . . . . . . . . . . . .68 I-fitting programs, x-ray spectrometers 91

Spectrum shifter, in polychromators 38Specular reflectance

defined . . . . . . . . . . . . . . . . . . . . . . . . . . . . . I 15infrared instruments 177as IR technique 115

Specular transmittance, defined 682Spherical aberration, defined 682Spherical harmonics, in series ODF

method 362-363Spider cracks, in macrostructure of continuous-

cast copper ingot 302Spiking method, XRPD analysis 340Spin decouplers, in ESR analysis 258Spin-dependent recombination, for analysis of

change in photo-induced conductivity ...258Spin echo

schematic 282spectra of Ni., room-temperature zero-

field 285technique 258

Spin glassabbreviation for 69Idefined 682identification of magnetic states in 253

Spin lattice relaxation time, in ESRanalysis 257

Spinodal decompositioncomposition profile of 593of Fe-base magnet alloy 598-600SAS techniques for .405

Spin relaxation rates, determined 275-276Spin-spin relaxation, ESR 257Spin wave

defined 682NMR studies in ferromagnetic materials ..277

Index /751

resonance 268, 273, 275Split mull, for IR samples 113Splitting, multiplet 572Spodumene, flame emission sources for ..29-30Spontaneous fission, as neutron source for

NAA 234Spot diffraction patterns .437, 438, 440Spot test kits, for alloy identification and

sorting 168Spray chambers

corrosion-resistant 35for ICP-MS 35, 40

Sputter chambers, low-pressure 54Sputter etching 556, 558Sputtering

artifacts, AES 556differential, as artifact 556as effect of primary ion bombardment 611as glow discharge effect 27inert gas ion, use with LEISS 603ion beam, for AES analysis 550sampling by 27species, schematic diagram 612

Sputter ion gun 554SRM. See Standard Reference Materials.SRO. See Short-range order.SRS, as synchrotron radiation source .413SSMS. See Spark source mass spectrometry.Stability constants, as voltammetric

information 193Stable free radical hydrazyl, ESR analysis

of. 265Stacking faults

effect in topographs 369-370in fcc cobalt-base alloy .466FlMlAP study of point defects in 583imaged by x-ray topography 365

Staining techniques, for lA samples 313Stainless steels. See also Stainless steels.

specific types.absorption/enhancement effects in 97austenitic, dislocation interaction .469determination of Cr, Ni, and Mn in .. 146-147electrolytic inclusion and phase isolation

in 176ion-implanted, AEM analysis .484nitric/hydrochloric acid as dissolution

medium 166precipitate identification by light-element

analysis .459-46ISIMS analysis of surface composition effects

in 622-623spark source mass spectrometry for. .. 146-147surface composition effects during laser

treatment of. 622-623texture orientations 360tube, optical micrograph with precipitates and

cracks .459umpire analysis of. 178-179weld metal, measurement of 8-ferrite in 287x-ray spectrometry of. 100

Stainless steels, specific types. See alsoStainless steels.

18Cr-12Ni high-purity austenitic, atom probeanalysis 595

300/400 series, analysis of 100300/400 series, data reduction and

standardization in x-ray spectrometry in 100304, depth-composition profiles 555304 foil, surface segregation in 564-566304, hot-rolled and recrystallized .470309, x-ray spectrometric results 100316, conventional SADP and ZOLZ-CBEDP

in " .441347, wavelength-dispersive spectrum

of 87,88416, examples of preferential detection, image

analysis 311NBS SRM-442 standard 147



752/ Index

Stains, surface, LEISS determined 603Standard addition

defined 682method, XRPD analysis 340

Standard deviationand random error 12relative, defined 681

Standard electrode potential, defined 682Standardization

of common titrants 172defined 682by ion chromatography 664techniques, internal, in SSMS 145

Standardless method, XRPD analysis 340Standardless ratio (Cliff-Lorimer)

microanalytic technique .447Standard reference materials

abbreviation for 691defined , 682for environmentallindustrial effluent

waters , 95Standards

for EPMA 524, 530primary, assay by electrometric titration ..202pure-element, x-ray scan across 527quantitative LEISS analysis 606of units and measures, SI 685verification by controlled-potential

coulometry 207Stanford Position Electron Accelerator Ring

(SPEAR), spectral of synchrotron radiationfrom .411

Stanford Synchrotron RadiationLaboratory

EXAFS experimental apparatus at 521as EXAFS radiation source .411-413

Stannous chloride, as reducing agent 169Starch, as binding agent for samples 94Stark effect

defined 682splittings 264

Stark line broadening, in emissionspectroscopy 22

State, change of, as x-ray diffractionanalysis 325

State movement, automated 310Static magnetic parameters, FMR quantitative

determination of 267Stationary phase, defined .' 682Statistical precision, assumptions of 525Statistics

for image analysis 313sampling 12-15

Steam distillation, in determination ofnitrogen" 173

Stearic acid, as binding agent for samples,x-ray spectrometry 94

Steel alloys. See also Steel alloys. specifictypes; Steels.

analysis for copper in, neocuproinemethod 65

analysis for oxide inclusions in 162atom probe composition profile, for heat-

treatment responses in 594optical emission spectroscopy ".21

Steel alloys, specific types. See also Steelalloys; Steels.

202, SIMS depth profiles 6231010, effect of improper polishing 3011070 shaft, residual stress and correction for

surface removal 3894140 steel hook, flow lines in forged 3034340 ground, effect of stress gradient

correction on measurement of near-surfacestresses for 388

4340, optical micrograph of fracturesurface 512

4340, overload failure of quench-crackedthreaded rod ..511-513

52100 bearing, high-resolution Jominy baranalysis 508-509

commercial chromium-molybdenum, atomprobe mass spectrum for 592

NBS reference, positive SIMS spectra underoxygen bombardment. 616

tempered 2.25Cr-Mo, atom probe massspectrum, carbide particle 592

Steel chips, analysis for silver, lead, andcadmium in 55

Steels. See also Steel alloys; Steel alloys,specific types.

AI-killed, analysis of 231alloying element partitioning in, FIM/AP

study of. 583alloying elements in 56analysis, as ratioed with the intensity of

iron , ..26carburizing 380chromium-molybdenum, atom probe

analysis 592cold-rolled, corrosion resistance 556-557determination of alloying elements by flame

AAS 56EPMA analysis of inclusions 516FIM sample preparation of 586fully-killed, cleanliness assayed 176high-resolution energy-compensated atom

probe analysis of 597induction-hardened shaft, subsurface residual

stress and hardness distributionsin 389-390

iron-based, AAS analysis of 55isolation of inclusions in 176Miissbauer measurement of retained austenite

in 287nonmetallic elements determined in 178optical emission spectroscopy 21pearlitic, atom probe composition profile

of. 593phase stability in 583phase transformation in 583quantitative determination of carbon and

sulfur by high-temperature combustionin 223-224

semikilled and rimmed, sample dissolutionof. 176

simple, partitioning silicon oxidation statesin 178

simulated, range of Kn doublet blendingfor 385

spark emission sources for. 29trace metals AAS analysis of 55weathering, Raman analysis 135

Steradian, as SI supplementary unit, symbolfor 685

Stereochemistry, and conformation,molecular 109

Stereographic projectionconstruction 358crystal axes using 359preferred crystallographic orientations

in 358-359by XRPD 333

Stereology 310, 316Stirring, effect in electrogravimetry 197, 200Stoichiometry, in basic chemical equilibria and

analytical chemistry 162Stokes radiation. See Stokes scattering.Stokes Raman line, defined 682Stokes scattering

energy-level diagram " 127in Raman spectroscopy 126-128

Stop cock, use in electrogravimetry 200Stopping distance, PIXE analysis 103Strained-layer superlattices, RBS analysis

of. 634Strains

ferromagnetic resonance analysis 275

fields of. 365frozen-in 268interfacial, evaluated by x-ray

topography 365magnitude of. v- •••••••••••325measurement, in lattices 633-635measurement of 275relaxation of, stress measurement 385surface, and corrosion. products 607

Stratified material, sampling 14Stress. See also Residual stress; Stress-

corrosion cracking.distribution, defined 382force per unit area, conversion factors 686gradients, subsurface, effects on

measurement 388-389grain interaction, neutron diffraction

analysis .424macroscopic, defined 676measurement, by x-ray diffraction 381-382micro- 380, 386-387microscopic, defined 676Mohr's circle for, x-ray diffraction stress

measurement. 381as not directly measurable 381principal 382symbol for 692total 385

Stress-annealed pyrolytic graphite, Ramananalysis 132-133

Stress corrosion 380Stress corrosion cracking

effect of boundary precipitation and solutesegregation in 549

fracture surfaces 562-564near-crack tensile sample geometry for ...563three brass alloy environment for 563-564

Stress distribution, defined 382Stress-strain diagram, defined 682Stripping analysis, electrometric titration and,

compared 202Stripping voltammetry 192-193Strontium

epithermal neutron activation analysis 239species weighed in gravimetry 172sulfate ion separation 169sulfuric acid as dissolution medium 165TNAA detection limits 237

Strontium oxide, in binary phosphateglasses 131

Structural analysis. See also Structure;Structure determinations; Substructure;Surface structure.

by CBED , .461-464of change, by neutron diffraction .420crystal, applicable analytical methods .4of defects, applicable analytical methods .4electronic : 60, 277elemental, applicable analytical methods ... .4extended x-ray absorption fine

structure .407-419inert gas fusion, in titanium 231of inorganic solids, applicable analytical

methods .4-6in situ, of active sites in catalysts .407in vivo, of active sites in metalloproteins . .407phase distribution, applicable analytical

methods .4phase identification, applicable analytical

methods .4in solutions, voltammetric analysis 188substructure, due to cold .468-469substructure, due to hot deformation and

restoration .469-470Structural evolution, EXAFS described ... .407Structure. See also Structural analysis;

Structure determinations; Substructure;Surface structure.

atomic-scale, FIMIAP for 584



crystal, of organic solids, analytic methodsfor 9

and degradation, of plasma-polymerizedhexamethyldisiloxane 285-286

of inorganic liquids and solutions, analyticmethods '" 7

of inorganic solids, analytic methodsapplicable 6

layered, RBS analysis of 628of materials, and materials

characterization 1molecular, of organic solids, analytic methods

for '" 9of organic solids and liquids, techniques

for 10of organic solids, methods for 9phase distribution/morphology, of organic

solids, analytic methods for. 9SAS techniques for '" .405

Structure determinations. See also Structuralanalysis; Structure; Substructure; Surfacestructure.



electron spin resonance 253-266extended x-ray absorption fine

structure .407-419ferromagnetic resonance 267-276field ion microscopy 583-602infrared spectroscopy 109-125Mossbauer spectroscopy 287-295neutron diffraction .420-426nuclear magnetic resonance 277-286Raman spectroscopy 126-138single-crystal x-ray diffraction 344-356small-angle x-ray and neutron

scattering .402-406x-ray diffraction 325-332x-ray powder diffraction 333-343

Structure factorcomplete equation for 352defined 349, 682-683equation, cells, and diffraction in unit

cell 329F, derivation of 350

Styrene, polymerization of 132Subgrains

size and shape 365topographic methods for 368

Sublattice ordering in intermetalliccompounds, NMR analysis 283-284

Submonolayers, effect of oxygen adsorbed onmetal surfaces 552

Subsample, defined 683Subsampling 13, 15-17Substance, amount of, SI base unit and symbol

for 685Substrate

effects of grain size on surface kinetics ... 560heavily TaC-coated WC + cobalt, XPS

analysis of 576-577high-resolution SIMS spectra for phosphorus-

doped silicon 623high-surface-area, infrared-transparent, DRS

for 114light, diffusion in 628lighter elements, surface impurities of heavy

elements on 628perfection of 375platinum, extent of coverage, Ni-P film

on '" " ..608platinum, LEISS spectra from Ni-P film

on " ..609rocking curve analyses of 371semiconductor, topographic methods for ..368silicon, organometallic silicate film deposited

on 617

tin-nickel, composition vs depth of passivefilm on 608-609

WC-Co tool, vapor-deposited multilayerstructure, by AES 561

Substrate intensity attenuation method, forthin-film samples 95

Substructuredue to cold deformation .468-469due to hot deformation and

restoration .469-470Subsurface

residual stress and hardness distributions ininduction-hardened steel shaft .....389-390

Subsurface residual stressdistributions 380, 388-390

Subsurface stress gradients, effect onsubsurface measurement 388

Subtraction techniques 183Sulfate ions, as narrow-range precipitant. 169Sulfates

anions, separation by ionchromatography 659

calibration curve for glass micro balloons ..667ion chromatography analysis of geological

waters for 665-666weighing as the, gravimetric analysis 171

Sulfide ionselements precipitated by 168ion chromatography analysis of. 661

Sulfide ores, nitric acid as dissolution mediumfor 166

Sulfidesas electrode 185as inclusions 176Leforte aqua regia as dissolution medium 166sintering agents for. 166weighing as the, gravimetry analysis 171

Sulfurchemistry at surfaces, AES analysis of....553determination by high-temperature

combustion 221-225determination from iron x-radiation 94determination in oil 101determination in petroleum products, by

XRS 82determined by iodimetric titrations 174glow discharge to determine 29as ion chromatography application 658, 664ICP-determined in natural waters .41infrared detection, high-temperature

combustion 223in inorganic solids, applicable analytical

methods .4, 6in oil, EDS determination 101species weighed in gravimetry 172surface segregation during heating 564-565use of copper accelerators with 222volumetric procedures for 175

Sulfur dioxideelectrometric titration for 205oxidation, SERS analysis of 136removal by manganese dioxide in high-

temperature combustion 222use to determine sulfur in high-temperature

combustion 221-225Sulfuric acid

residue isolation using 176as sample dissolution medium 165

Sulfurous acid, as reducing agent 169Sulfur trioxide, removal of 222Sum peaks

defined 92, 683in energy-dispersive spectra 520and escape peaks 520

Supercritical fluid chromatography 116Superheterodyne detection, use for low-

temperature ESR studies 257Superlattices. See also Lattices; Ordered

structure.

Index / 753

and interface studies 634-635defined 683diffraction pattern from 540element location in planes of. 599as impeding determination of atomic

structure 344, 353strain measurement. 628

Supplementary SI units, guide for 685Supporting electrode, defined 683Suppressed chromatography

anion, reaction of. 659cation, reaction of. 659-660

Suppressorscolumns 660fiber. 660hollow fiber anion 660role in ion chromatography 659schematic, membrane-type 660

Surface. See also Surface analysis; Surfaceanalysis and characterization; Surfacecomposition; Surface contamination;Surface films; Surface roughness; Surfacesegregation; Surface-sensitive analyticaltechniques; Surface sensitivity; Surfacestructure.

adsorbates, identified on metalelectrodes 126, 134

adsorption 109, 114, 126, 134, 407, 583catalysts 114, 253chemical analyses of 177-178,591coatings, identified 168compressive residual stresses 380crystallography of 536-538crystallography, vocabulary for 537-538deeply etched, SEM analysis .490depth profiling through 583dielectric properties 136diffraction from, principles 538-539diffusion 583dynamic processes of, LEED analysis

of. 536effects of, determined 273-274electrode, XPS spectrum showing elements

present in 578elemental analysis by XPS 568enhancement. 136etching " 575finishing 93flat metal, IRRAS analysis 114fracture .490, 497free-radical reactions, ESR studied 253grinding 287, 390-391interaction of lubricants with, AES

analysis 565layers of glass, analysis of 624-625LEISS segregation of lead to 607-608materials, resource evaluations by NAA ..233metal 118,583,586microstructure by LEED 536modification of frictional 565near-, effect of stress gradient correction on

measurement of 388of nontransparent samples,

characterized 70-71oriented, structural information .407-phase detection, Mossbauer effect ..287, 293phase, qualitative XRPD analysis on

silicon 341preparation 93reactions, FIMJAP study of 583reconstruction 536, 583segregation 544, 564-566, 583, 593, 607-608single-crystal. .407solid 198, 603species 133, 134of stainless steel, SIMS analysis of effects of

laser treatment on 622-623stains and corrosion, LEISS identified 607strains of 607



754/ Index

Surface (continued)stress-corrosion crack fracture, AES

analysis 562-564tension, SI derived unit and symbol for 685topography 595UVIVIS characterizations of 70-71x-ray diffraction stress measurement

confined to 382Surface analysis. See also Surface; Surface

analysis and characterization.chemical, AES high lateral resolution

for 549, 556-566elemental, inorganic solids, analytical

methods .4-6elemental, of organic solids, methods for ...9by EPMA electron beam 517,529-530graphite, Raman spectroscopy 132of inorganic solids, applicable analytical

methods .4-6molecular/compound, of inorganic solids,

methods for .4-6molecular/compound, of organic solids,

methods for. 9of organic solids, methods for. 9Raman spectroscopy 126, 133-137smooth, Raman spectroscopy for. .... 135-136

Surface analysis and characterization. Seealso Surface; Surface analysis.

Auger electron spectroscopy 549-567infrared spectroscopy 109-125low-energy electron diffraction 536-545low-energy ion-scattering

spectroscopy 603-609Miissbauer spectroscopy 287-295particle-induced x-ray emission 102-108Raman spectroscopy 126-138Rutherford backscattering

spectrometry 628-636secondary ion mass spectroscopy 610-627x-ray photoelectron spectroscopy 568-580

Surface carbonscarbide or graphitic identified 568contamination, effect on painted, cold-rolled

steel. 556determined 223-224effects on paint adherence on metal

cabinetry 224Surface composition

analysis by SIMS 610effects during laser treatment of stainless

steel 622-623variation during heating 564

Surface contaminationAES analysis 549anion determination 658FMR analysis 268identification 168RBS analysis 628

Surface-enhanced Raman scattering .. 135-136Surface EXAFS detection technique .... .418Surface films

AES in-depth compositional evaluation 549on electrical contacts, XRS analysis 578heterogeneous, AES analysis of 565-566oxidation states of metal atoms, determined

in 568Surface oxides, determined 177Surface peak, RBS analysis for 633Surface phase

detection 293qualitative analysis, on silicon 341-342

Surface relief, topographic methodsfor 365, 368

Surface roughnesseffect in AES analysis 553effect in x-ray diffraction residual stress

techniques. . . . . . . . . . . . . . . . . . . . . . . . .387and surface electronic structure, SERS

and 136

Surface segregation, analysisof 536, 564-566, 583, 593, 607-608

Surface selection rule 119Surface-sensitive analytical techniques. See

also Surface; Surface sensitivity.Auger electron spectroscopy 549-567secondary ion mass spectroscopy 610-627x-ray photoelectron spectroscopy 568-580

Surface sensitivity. See also Sensitivity;Surface; Surface-sensitive analyticaltechniques.

dependence on takeoff angle 574ferromagnetic resonance 268LEISS analysis 605of x-ray photoelectron

spectroscopy 569-570, 573Surface structure

analysis of 133-134EXAFS electron detection studies,

adsorbates .418peak, RBS analysis for 633study by channeling and blocking 633

Surface tension, SI derived unit and symbolfor 685

Surfactant molecules, in water, structuralchanges in 118

SURF II, as synchrotron radiation source .. .413Swaging of rods and wires, preferred

orientation during 359Symbols and abbreviations 689-692Symmetry

center of 346x-ray diffraction analysis and 325

Synchronous excitation spectroscopy 78Synchrotron, defined 683Synchrotron radiation. See also Radiation.

and bremsstrahlung output, compared .411defined 683dynamic processes monitored 375effect on EXAFS as atomic probe .408EXAFS scan of nickel using .408radiation sources .412from SPEAR, spectral distribution of. .411as x-ray source for EXAFS .407, 411-412and x-ray topography 365, 374-376

Synthetic diamond, metal impurities in ... .417Synthetic materials

analysis of new 353-354five-component, MFS analysis 78high-temperature combustion analysis of ..224

Systematic samples, defined 12-13Systems, disordered and ordered, EXAFS

analysis of. .407

T/L-/L diffractometers 337t. See Thickness; Time.T. See Temperature.Tannin and ammonium hydroxide, as

precipitant. 169Tantalum

epithermal neutron activation analysis 232evaporation fields for 587filament, gas mass spectrometer 152-153high-purity, SSMS analysis 144ores, fusion flux for 167ores, hydrofluoric acid as dissolution

medium 165photometric analysis methods 64species weighed in gravimetry 172TNAA detection limits 238

Tantalus I, as synchrotron radiation source 413TAR, as metallochromic indicator 174Target

defined 683in divergent-beam topography 370

Target population, defined 12

Tar sands, GC/MS analysis of volatilecompounds in 639

Taylor series expansion .414TCP. See Topologically close-packed.Technetium, determined 209Television scanners, conventional, with image

analyzers 310Tellurium

determined by 14-MeV FNAA 239-doped gamma-ray detectors 235gaseous hydride, for ICP sample

introduction 36gravimetric finishes 171quartz tube atomizers with .49radiochemical, destructive TNAA for 238in semiconductor alloys, electrometric titration

for 206TEM. See Transmission electron microscopy.Temperature

abbreviation for 691control, in ion selective electrode

measurement 185-186conversion factors 686Curie, abbreviation for. 691effect in AAS emission signals .44effect in emission sources 24effect in MFS analysis 77effect in Rietveld method .423effect on rates of phase transformations, in

metals 318effects in electrogravimetry 198electron 24gas kinetic, and kinetic energies of heavy

particles 24high, FMR probe for 270low, probe for FMR measurement at 270of premix flames 29room, variations 172structural changes as function of. .420thermodynamic, SI base unit and symbol

for 685variable, ESR spectrometers 257variation of field-evaporation rate with 594

Temperature-induced phase transformations,XRPD analysis 333

Tensile strength, in aluminum-killed steels 231Tension, surface, SI derived unit and symbol

for 685Terbium, TNAA detection limits for 238Terminal pins, and solder, elemental mapping

of. 532Ternary alloys, implantation in .486Ternary iron-cobalt-chromium alloys, FIMiAP

analysis 598-599Tesla

abbreviation for 691charge 32as SI derived unit, symbol for. 685

Tetragonal unit cells 346-348Texture. See also Crystallographic information;

Crystallographic texture measurement andanalysis.

analysis 357-364crystallographic, as measure of average grain

orientation 358crystallographic, measurement and analysis

of 357-364defined 683 I

determined by neutrondiffraction 420, 423-424, 425

fiber, defined 359and material behaviors, correlated 357-358nondestructive measurement .423orientation distribution function as

measurement of. 360-361preferred orientation 358-361rolling, in fcc material 363-364symmetrical variations 363and texture gradients .420



true volume-averaged, by neutrondiffraction 357

by x-ray topography 365Thallium


photometric analysis methods 64species weighed in gravimetry 172weighed as the chromate 171

Thallium-doped sodium iodide crystal, inscintillation detectors 89

Thermal analysis, of residues 177Thermal-conductive detection

of carbon and sulfur 223cell 230inert gas fusion 229-230

Thermal conductivitycarbon determined 221-225conversion factors 686as detector for C and S in high-temperature

combustion 221-222of gases 223, 230SI derived unit and symbol for 685

Thermal control plate, radioanalysis 248Thermal excitation, in optical emission

spectroscopy 24Thermal expansion

coefficients, aniosotropic, XRPDdetermined 333

conversion factors 686Thermally activated growth, and isothermal

phase transformations 317Thermally labile species, Raman analysis

of. 129Thermal motion, atomic, to determine crystal

structure 352Thermal neutron activation analysis

automated systems 238calibration for 236detection limits 238detection limits, rock and soil 237-238nondestructive 234-238radiochemical, destructive 238-239sample handling 236of zirconium 234

Thermal neutron capture, for radioisotopeproduction 234

Thermal neutron irradiationand epithermal irradiation, compared 234neutron sources for. 234

Thermal noise, defined 683Thermal polymerization of styrene, Raman

analysis 131Thermal sampling, and Grimm emission

source 27Thermal treatments, ion-implanted

alloys .486Thermal vibration, analysis of 536Thermite, flame AAS analysis of 56, 57Thermodynamics

first principle, half-cell potentials from ... 164of surface or grain-boundary segregation,

LEED analysis 544Thermodynamic temperature, SI base unit and

symbol for 685Thiazolyazoresorcinol, as metallochromic

indicator 154Thick films. See also Films; Thin films.

analysis of. 561LEISS analyses for 603RBS analysis for 631

Thick, infinitely, XRS samples 93Thickness. See also Thickness measurement.

abbreviation for 691effect in rocking curve profile for epitaxial

films 375effect on x-ray energy in crystals 367-370sample, and light absorption 61specimen, for EELS analysis .450

vs theoretical intensity, single-element x-rayspectrometry 100

of thin films, determined 100, 631-632Thickness measurements. See also

Thickness.optical metallography 299-308Rutherford backscattering

spectrometry 628-636scanning electron microscopy .490-515x-ray spectrometry 82-101

Thick-sample reflection technique, pole figuresdetermined by 360

Thick samplesand light absorption 61PIXE analysis 102

Thieves, as sampling devices 16Thin film dilTractometers, XRPD

analysis 337Thin films. See also Films; Thickfilms; Thin

samples; Ultrathin films.changes in nickel on silicon 631, 632characterization of. 559-561with columnar growth morphology 544compositional AES analysis ....549, 559-561composition and layer thickness of 631-632composition profiles by XPS 568diffractometer 337FIM!AP study of local composition

variation 583impurity analysis in LPCYD 624molecular structure and orientation in 109nucleation and growth 583passive 557-558rocking curve analyses of 371Rutherford backscattering spectrometry

analysis 628sample preparation for ATEM .452as samples, x-ray spectrometry 95, 100SIMS analysis of surface layers 610solvent evaporation for infrared analysis .. 112thickness determined 100x-ray intensity vs thickness, single element

analysis 100Thin, infinitely, XRS samples 93Thinning

electrochemical vs electrojet .451as sample preparation technique .450-452

Thin samples, PIXE analysis of 102Thorium

epithermal neutron activation analysis 239M lines for 86plutonium diffused into 249species weighed in gravimetry 172TNAA detection limits " 238weighed as the fluoride 171

Three-dimensional defect analysis,ATEM .466

Threshold energy, EXAFS analysis .409Thresholding

gray-level. as feature detection mode, imageanalyzers 311

use in image analysis 311-312Thymol blue, as acid-base indicator 172Thymolphthalein, as acid-base indicator 172Tilt

angles across subgrain boundaries, evaluatedby x-ray topography 365

controlled, for phase/particleconfirmation .458-459

defined 683effect in determining orientation

relationships .453-454effect in XPS depth analysis 573experiment, for unknown phase or particle

confirmation .458Time

abbreviation for 691dead, live, and real, in x-ray

spectrometry 92

Index /755

gamma-ray spectrum changes as functionof. 236

vs potential, potentiometric membraneelectrodes 186

SI base milt and symbol for 685Time-of-flight measurement

atom probe analysis 591field ion microscopy 584imaging atom probe analysis 596spark source mass spectrometry 142

Time-of-flight powder diffractometer, neutrondiffraction .422

Time-of-flight single-crystal diffractometer, atpulsed neutron source .424

Time-of-flight spectrometers 142, 591Tin

chip combustion accelerators 222determined by controlled-potential

coulometry 209distillation 169evaporation fields for 587gaseous hydride, for ICP sample

introduction 36in hydrogen peroxide, GFAAS analysis

of 57-58iodimetric titration for 174in iron-base alloys, flame AAS analysis

of. '" '" 56ores, dissolution of inorganic materials in 167photometric analysis methods 64quartz tube atomizers with .49recovery from brass 200solvent extractant for 170species weighed in gravimetry 172trace, analysis in hydrogen peroxide by

GFAAS 57-58trace levels in H202 , GFAAS

determined 57-58volatilizing 166volumetric procedures for 175

Tin alloyssample dissolution medium 166Sn-0.2Pb, LEISS spectra 608

Tin chip combustion accelerators 222Tin-lead solder, LEISS segregation of lead to

surface of. 607-608Tin-nickel substrate, composition vs depth of

passive film on 608-609Tin tetraiodide, dissolution to 167Titanate phases, ceramic nuclear waste

forms 532-535Titanium

added to nuclear waste, EPMAanalysis 532-535

determination in paint, enhancement andabsorption effects 98


evaporation fields for 587intensity of K lines in 97ion removal from 200in iron-base alloys, flame AAS analysis

of. " 56Jones reductor for. 176neutron and x-ray scattering, and absorption,

compared .421ores, commercial, fusion with acidic

fluxes 167oxygen determined in 231photometric analysis methods 64species weighed in gravimetry 172structural problems analyzed by inert gas

fusion 231in titanium oxide, determined by controlled-

potential coulometry 207TNAA detection limits '" .237as unknown particle .457use in flame atomizers .48volumetric procedures for 175



756/ Index

Titanium alloysdiffraction techniques, elastic constants, and

bulk values for 382AM sample preparation of 586nitrogen-implanted .485

Titanium alloys, specific typescommercially pure, diffraction techniques,

elastic constants, and bulk values for ...382Ti-6AI-2Sn-4Zr-2Mo, diffraction techniques,

elastic constants, and bulk values for ... 382Ti-6AI-4V, diffraction techniques, elastic

constants, and bulk values for. 382Ti-6AI-4V ground, diffraction peak location

methods compared 386Ti-6AI-4V, nitrogen-implanted .485

Titanium-iron alloys, hydrided, phase analysisof '" 293-294

Titanium-iron intermetallic compounds, phaseanalysis of 293-294

Titer, in volumetric work 162Titer technique, for analyte

determination 172Titrants

common standardizations 172unstable 202

Titrationacid-base 172-173amperometric 204analytical, by potentiometric membrane

electrodes 181automated, biamperometry or bipotentiometry

use with 204back- 173biamperometric 204bipotentiometric 204buret 205chelometric 164of chloride in silver nitrate solution 164complexometric 164, 201conductometric 203coulometric 197, 202-205dead-stop end-point 204defined 683EDTA 173electrochemical. 202electrometric 202-206, 672iodimetric 174Karl Fischer, for surface oxides 177methods, with ion-selective membrane

electrodes 183Mohr, defined 164oscillometric (high-frequency) 203-204permanganate, for chromium and

vanadium 176potentiometric 204precipitation 173redox, miscellaneous 174-176spectrophotometric 70vessel, oscillometric (high-frequency) 203Vohhard, defined 164

Titrimetric potentiometry, and ion-selectionelectrodes 204

Titrimetryacid-base 172-173amperometric . " 204buret 205classical. 205complexation 173described 162iodimetric 174of metal alloys, by potentiometric membrane

electrodes 181precipitation 173redox 174-176

TNAA. See Thermal neutron activationanalysis.

Toepler pumps 152Tool steels, WI, case-hardened layer as OM

macrograph 303

Topographseffect of surface relief in 369Lang, of dislocations 370projection or traverse 369

Topographydefined 366Lang section 368neutron, capabilities 365projection 369reflection 368-369single-crystal and x-ray 330-331transmission 369-370x-ray 365-379

Topologically close-packed, abbreviationfor 691

Torchcutting, for sampling 16Fassel, for analytic ICP systems 36-37inductively coupled plasma 34, 36-37mini-, for the ICP 37

Toroidal-sector electrostatic lens,Poschenrieder analyzer as 597

Torque, conversion factors 686Torque-coil magnetometer, defined 683Total combustion 223-224Total consumption burners 28Total ion chromatogram, typical 644Total luminescence spectroscopy 78Total nuclear magnetization, defined 280Total transmittance, defined 683Toughness, fracture, conversion factors 686Toxic elements

pollution studies by NAA for 233SSMS analysis of natural waters for 141

Toxicology, PIXE analysis in 102Trace analysis. See also Trace analysis.

methods of; Ultratrace analysis.14-MeV fast neutron activation analysis 239of alkali metals 29de arc excitation for impurities in CaW04 •• 29habit plane determination as .453-455inductively coupled plasma atomic emission

spectroscopy 31-42of inorganic gases, analytic methods for ....8of inorganic liquids and solutions, applicable

methods " 7of inorganic solids, applicable analytical

methods .4-6of metals .44, 46of organic solids and liquids, techniques

for 10of organic solids, methods for. 9sampling quality assurance for 17of toxic elements in ground water 148-149

Trace analysis, methods of. See also Traceanalysis; Ultratrace analysis.

atomic absorption spectrometry .43-59classical wet analytical chemistry 161-180controlled-potential coulometry 207-211electrochemical analysis 181-211electrogravimetry 197-201electrometric titration 202-206electron probe x-ray microanalysis 516-535electron spin resonance 253-266gas analysis by mass spectrometry 151-157gas chromatography/mass


spectroscopy 31-42infrared spectroscopy 109-125ion chromatography 658-667liquid chromatography 649-659molecular fluorescence spectrometry 72-81neutron activation analysis 233-242particle-induced x-ray emission 102-108potentiometric membrane electrodes .. 181-187Raman spectroscopy 126-138Rutherford backscattering

spectrometry 628-636

secondary ion mass spectroscopy 610-627spark source mass spectrometry 141-150ultraviolet/visible absorption

spectroscopy 60-71voltammetry 188-196

Tracer, radioanalysis for. 243Transfer, material, AES analysis of sliding

during 566Transformations

amorphous to crystalline, EXAFSdetermined .407

in situ, studied by x-ray topography andsynchrotron radiation 365

material, and crystal kinetics 376Transformer cores, analysis of 224Transition-element ions, ESR identification of

valence states of 253-266Transition elements

compound analysis of 262on periodic table 688as system favorable for ESR 262

Transition group metals, ESR analysis ofhyperfine splitting in 260

Transition ioncontent, ESR analysis for 253content, of fossil fuels 253in solids, local crystal environments

around 253-266Transition-metal ions, ESR analysis of ....254Transition metals

ion chromatography separation and detectionof 660-661

as source of background fluorescence invibrational spectroscopy 130

TransitionsAuger electron via KL2 •3 and L2 •3 •.•..•.550identification of elements in 253-266interband, effect on Auger electrons' 551

Transmissionanomalous, in x-ray topography 367topography 369-370

Transmission electron microscopeselectron column .431as input device for image analyzers 310

Transmission electron microscopy. See alsoAnalytical transmission microscopy.

capabilities, and FlMIAP 583defect analysis by .464-468defined 683deformation, recovery, and recrystallization

analysis by .468-470and AM images, IN 939 nickel-base

superalloy ~ 598of inorganic solids, types of information

from .4-6of microstructure and magnetic properties,

ductile permanent magnets 599of organic solids, information from 9and Raman analysis, for intercalated

graphites 133Transmission grating, defined 683Transmission pinhole camera, schematic ..334Transmission topography

Berg-Barrett transmission arrangement 369configurations for 369defect imaging with 370

Transmittance 62-63, 683Transverse electric (TE) modes 256, 691Tribology, AES analyses in 566Triclinic crystal systems, unit cells as..346-348Triggered capacitor discharge, defined ....683Trigonal unit cells 346-348Tri-N-bulyl phosphate, solvent extractions

with 169Tri-N-octylphosphine oxide, as solvent

extractant 170Triplemate, use in Raman spectroscopy 129Triple monochromators, stray light rejection

for 129



Triplet states, ESR analysis of 254Triton

defined 683as surfactant, and adhesion of polymers on

silver 136-X-100, as maximum suppressor,

voltammetry 191Tubes. See also Photomultiplier tubes.

for image analyzer scanners 310Nessler, color comparison 66pure quartz sample, ESR spectrometer. 256x-ray, for x-ray spectrometry 87-90x-ray, and Z element determination by

XRS 101x-ray, molybdenum 88

Tubingcopper, (111) pole figures from 363copper, ODF using Euler plots method 361Inconel 600, residual stress and percent cold

work distributions 390inside surface measured 384midwall, pole figures from 362nonuniformity of texture in 363-364stainless steel, precipitate identification

in .459-461surface stress measurement in 390

Tunable infrared lasers, applications 112Tungsten

combustion accelerators 222epithermal neutron activation analysis 239field evaporation of 586, 587filament, gas mass spectrometer 152-153FIM sample preparation of 586grain boundary, FIM image 589gravimetric finishes 171high-resolution spectrum by ECAP

analysis 597neutron and x-ray scattering, and absorption,

compared .421photometric analysis methods 64stereographic projection 585TNAA detection limits " ..237typical field ion micrograph 585

Tungsten combustion accelerators 222Tungsten hairpin filament electron

gun 492Tungsten-iodide lamp, for continuum source

background correction 51Tungsten trioxide, analysis of calcination and

activation of 133Tunneling

electron, rate in field ionization 585field ionization as quantum mechanical

process of 584Tunnel junction structures

metal/solid surface analysis by SERS 136study of molecules by SERS in 137

Turbine alloysalloying element partitioning 583phase stability and transformations,

FIM/AP 583Turning

residual stress distributions 392samples, for chemical surface studies 177

Turquoise and metatorbernite, ESR analysisof 265

Twinning. See also Twinning. characterizationof.

analytic methods for. 3deformation-induced, effect on diffraction

pattern .440effect on texturing 358imaged by x-ray topography 366in rutile, bright- and dark-field images of

annealing .443subtle, as impeding determination of atomic

structure 344, 352-353Twinning, characterization of. See also

Twinning.


optical metallography: 299-308x-ray diffraction 380-392

Two-angle technique, plane-stress elasticmodel 384

Two-dimensional defect analysis .466Two-phase materials

atomic number contrast in analysis of ....508FIM images of. 589, 590

uUltrahigh vacuum

abbreviation for 691atom probe microanalysis 591EXAFS surface structure detection in .418

Ultrapure water, GFAAS trace metal analysisfor 57-58

Ultrasonic methods, capabilities of 380Ultrasonic nebulizers

for atomic absorption spectrometry 55for ICP sample introduction 36

Ultrasonics, measured by acoustic ESR 258Ultrathin films, LEISS coverage analysis 603Ultrathin window

abbreviation for 691-EDS light-element analysis .459-461energy-dispersive spectrometer 519

Ultratrace analysisgraphite furnace atomic absorption

spectrometry 57of inorganic gases, applicable methods for ..8of inorganic liquids and solutions, applicable

methods for. 7of inorganic solids, applicable methods

for .4-6of organic solids and liquids, applicable

methods for 9, 10uranium, determined by laser-induced

fluorescence spectroscopy 80Ultraviolet photoelectron spectroscopy, of

molybdena catalysts 134Ultraviolet radiation, defined 683Ultraviolet spectra, DRS and ATR

analysis 114Ultraviolet/visible absorption spectroscopy.

See also Optical and x-rayspectroscopy 60-71

absorbance 62adapted for inorganic solids .4-6advantages 60applications 60, 70-71Beer's law 61-63capabilities 181capabilities, MFS compared 72color comparison kits 66-67defined 683effect of complexing agent 64estimated analysis time 60experimental parameters 68-70filter photometers 67general uses 60for inorganic liquids and solutions 7instrumentation 66-68introduction and principles 61-63limitations 60molecular fluorescence 61-62monochromators 66NMR, ESR, and IR compared with 265of organic liquids and solutions, information

from 10of organic solids, information from 9Planck's constant 61quantitative analysis 63-66related techniques 60samples 60, 70-71sensitivity 63-65

Index /757

spectral region of interest 61terms and symbols used in 62

Ultraviolet/visible solution spectrophotometry,AAS spectrometers and 51

Umpire analysisgravimetry for. 170of stainless steel alloy 178-179

Uncertainties, sampling 12, 15, 17Uncertainty, defined 683Unit cells

arrangement of atoms within 345copper tetrahedra and molybdenum octahedra

in 354cubic 346-348defined 683described 346-347diffraction, and structure factor equation

for 329dimensions, for defining crystal structure .. 348geometry of 326-327hexagonal 346-348identification, by single-crystal x-ray

diffraction 344,346-347,351monoclinic 346-348orthorhombic 346-348tetragonal. 346-348triclinic 346-348trigonal (rhombohedral) 346-348use to identify unknown crystalline

phase 353Unit mesh size and shape, LEED analysis ..544Units

of measure 691SI standardized 685

Universailluxes, various 167Unknown crystalline phase identification, by

single-crystal diffraction 353Unknown phase identification, by electron

diffraction/EDSanalysis of metallized ceramic .457-458assessment, experimental/reference

data .455-456confirming .457data base use .456diffraction patterns obtained .458strategy of analysis .456-457

Unpaired electrons, ESR analysis of 254Unresolved doublets, Kn aluminum and

magnesium lines as 570Unsaturation

determined 219EFG determination in polymers 212

UPS. See Ultraviolet photoelectronspectroscopy.

Uptake delay, in concentric nebulizers 35Uranium

AFS analysis of .46assay by delayed-neutron counting 238determined by controlled-potential

coulometry 209, 211epithermal neutron activation analysis 239flow diagram for quantification of 80Jones reductor for 176M lines used for. 86species weighed in gravimetry 172TNAA detection limits .. '" 237ultratrace, determination by laser-induced

fluorescence spectroscopy 80-81volumetric procedures for 175x-ray absorption curve as function of

wavelength 85Uranium alloys

image analysis of cellular decomposition ofmartensite in. . . . . . . . . . . . . . . . . . . . . . .316

kinetics of cellular decomposition ofmartensite in 316-318

Uranium alloys, specific typesU-0.75Ti, effect of time on cellular

decomposition 319



758/ Index

Uranium alloys (continued)U-0.75Ti, effect of temperature on

decomposition time 319U-O.75Ti, cellular decomposition

kinetics 316U-O.75Ti aged, microstructure 318

Uranium dioxide, analysis ofimpurities 149-150

Uranyl, defined 683UTW. See Ultrathin window.UVSOR, as synchrotron radiation source .. .413UVIVIS. See Ultravioletlvisible absorption

spectroscopy.UVIVIS spectrophotometry, instrumentation

of. 61

y

v. See Electron velocity.Vacancies

in iridium 588as point defects 588

Vacuumelectromagnetic radiation in 83gas mass spectroscopy in 151melted, abbreviation for. 691-metal interfaces, SERS for 136pumping system, SEM microscope .491requirement for XPS instruments 571systems, LEISS analysis 607test chamber, Auger spectrometer. 554ultrahigh, abbreviation for 691ultrahigh, EXAFS electron detection for

surface structure in .418ultrahigh, for atom probe microanalysis 591x-ray spectrometer detectors in 91

Vacuum cathodic etching, for opticalmetallography samples 301

Vacuum fusioncapabilities 226of inorganic solids, types of information

from .4-6Vacuum melted, abbreviation for 691Vacuum spectrometers

application of .41polychromator 37,38for vacuum ultraviolet 29

Vacuum system, LEISS analysis 607Vacuum ultraviolet, as spectral region 61Valence-site symmetry, effect on XANES

spectrum .415Valence states, of transition-element ions 253Vanadium

in compounds, determined by coulometrictitration 206


electron channeling pattern 504, 508evaporation fields for 587ion removal from 200in iron-base alloys, flame AAS analysis 56K-edge XANES spectra .415neutron and x-ray scattering, and absorption,

compared .421permanganate titration for 176redox titrations 175TNAA detection limits 237volumetric procedures for 175

Vanadium oxidecatalysts, Raman analysis 133vanadium K-edge XANES spectra of .415

Vapor depositionRaman microprobe, TEM analysis, in

graphites 133for thin-film semiconductors 601, 602

Vaporization-atomization interferences 33, 34interferences, in flame spectroscopy 29, 47

selective 25Vapor pressure, for AES samples 556Variability

of population characteristics, in sampling .. 13sample, and measurement 12

Variable 26 geometry, in RDF analysis 396Variable takeoff angle method, for thin-film

sample preparation 95Variable-temperature ESR investigations 257Variable wavelength geometry, RDF

analysis 396Varian 9-Ghz cavity, insert for FMR high-

temperature studies 271veo. See Vibrational circular dichroism.Vegetable oils, unsaturation, determined by

electrometric titration 205Velocity

analyzers 570-571angular, SI derived unit and symbol for 685conversion factors 686electron, abbreviation for. 691of propagation, wave theory of. 83relation to electromagnetic radiation 83SI derived unit and symbol for 685speed of light, abbreviation 689

VEPP-2M, as synchrotron radiation source . .413VEPP·3, as synchrotron radiation source .413VEPP·4, as synchrotron radiation source .413Verification, of alloys 118Very large scale integration (microcircuit)

products, gas mass spectroscopyin 156-157

Vesselsfor sample dissolution treatments 165-167for sinters/fusions 166-167for sodium peroxide fusions 166

VF. See Yacuum fusion,Vibrating sample magnetometry 268Vibrational analysis

Fourier-transform infrared spectroscopy ... 126high-resolution electron energy loss

spectroscopy 126Raman and infrared as 126, 127

Vibrational behaviorof atoms, and determination of crystal

structure 352pyridine, model environments for , 134Raman, in intercalated graphite species 133ring-breathing, of pyridine 134of surfaces, SERS analysis 136surface, surface-enhanced Raman scattering

for 136Vibrational frequencies, infrared, calculation

of. 110Vibrations

information, by Raman analysis ..... 126-138metal-ligand, Raman spectroscopy for .... 126molecular, effect in infrared

spectroscopy 109molecular, in infrared spectroscopy 111molecular, in Raman spectroscopy 127

Vidicondefined 683and diode array detectors, use in Raman

spectroscopy 128-129Vilella's reagent, for etching stainless

steel. 311Vinyl chloride, in vinyl chloride and vinylidene

chloride copolymer, Raman analysis ... 132Vinyl films, identification of polymer and

plasticizer materials in 123-124Vinyl groups in silicone, Raman analysis ... 132Viscosity

conversion factors 686dynamic, SI derived unit and symbol for ..685of fossil fuels, ESR determination of .....253kinematic, SI derived unit and symbol

for 685of solution, in flame spectroscopy 29

Viscous flow, GMS analysis 152Visible 683, 691Visible radiation, defined 683Visible spectra, DRS and FT-IR analysis 114Vitreous carbon, Raman analysis 132Voids, as internal defect 587Volatile compounds, complex mixtures analysis

in 639Volatile liquids, analytical methods for 7, 10Volatile materials, removal for XPS

analysis 575Volatility, of nitric acid reactions 166Volatilization, of nitric acid reactions, 166Volatilization

and atomization, in graphite furnaceatomizers 53

of residues, gravimetric analysis 163spark, for solid-sample analysis 36

Volhard titrationfor arsenic 173defined .. . . . . . . . . . . . . . . . . . . . . . . 164indirect, for zinc 173of silver 173

Voltageapplied, and electrolysis 197applied, in field ion microscope 588constant increases, in electrogravimetry 198increases, effect in constant current methods,

electrogravimetry 198-pulsed and laser-pulsed atom probes,

compared 597value, as decomposition potential 199

Voltage contrast, as SEM specialtechnique 506-507, 683

Voltammetry. See also Classicalelectrochemical and radiochemicalanalysis 188-196

applications 1l18, 194-195capabilities 181cyclic 192defined 683electrometric titration and, compared 202estimated analysis time 188general uses 188improvements and developments 193information obtainable

from 188, 189, 193-194introduction and principles 189-191limitations 188linear sweep 191-192mass transfer processes in 189with other electrodes 191-193polarography with DME as 189principle of differential pulse stripping 193related techniques 188samples 188solid-electrode, capabilities 207stripping 192

Voltammogram, single-sweep peaked, withcarbon-base electrode 192

Voltmeter, for electrogravimetry 200Volume

CBED patterns to analyze .439conversion factors 686diffusion, compared to grain-boundary

diffusion .478electron scattering .434fraction measurement, image

analysis 313, 314per unit time, conversion factors 686relation to x-ray spatial resolution .448sample, production of inelastically

backscattered electrons by .499SI derived unit and symbol for 685of signals produced by electron

beam .498-500small, AEM-EDS microanalytical techniques

for .446specific, SI derived unit and symbol for ..685



Volume fraction measurements, imageanalysis 313, 314

Volumetric analysiscommonly used 175defined 683electrometric titration as 202equilibrium in 163vs gravimetric analysis 172molarity and normality in 162oxidation-reduction 163-164precipitation titrations as 164redox reaction 163as redox titrations 174-176

Vortex stabilization technique, Reed's .....32Vulcanization of polymers, Raman

analysis 132Vycor crucibles, for fusions with acidic

fluxes 167

wWafers, silicon, IR determination of oxygen

and carbon determined in 122-123Waste products

chemical, assay for toxic elements 233industrial, sampling of 12-18

Wastewater streams, UV/vIS analysis 60Water. See also Rainwater; Rinse waters;

Seawater.analysis ....7,31,41,43,60,102,141,152,

212analysis by biamperometric titration 204assay for toxic elements ... 141, 148-149, 233cationic, anionic, gaseous concentrations,

determined 181elemental analysis 102filtration of particles from 94ground, SSMS analysis 148-149Karl Fischer method to determine 219natural, analyses of .41, 141purest, conductance of. 203Raman scattering of 133as sample in gas analysis by mass

spectroscopy 152Standard Reference Materials for

environmental/industrial. 95structural changes in surfactant molecules,

determined 118trace analyses of 57-58, 60, 204ultrapure, trace metal analysis for 57-58voltammetric monitoring of pollutant metals

and nonmetals in 188and wastewater streams, UV/vIS analysis

of. 60well, as ion chromatography solution 658

Waterbury's reagent, as etchant for copperingot 302

Water softener, ion exchange in 658-659Wave

function, EXAFS analysis .409polarographic, defined 190theory, as applied to electromagnetic

radiation 83Wavelength

absorbance (UV/VIS) as function of. 63calibration, for MFS analysis 77characteristic x-ray, and atomic number,

Mosely's relationship between .433Compton, defined 84conversion factors 686defined and symbol for 683, 692in electromagnetic radiation 83infrared spectral 110selectors, MFS 76sorters 23variable, geometry of. 396x-ray absorption curve for uranium as function

of. 85

Wavelength-dispersive spectrometersartifacts 521direct defocusing map 527for x-ray spectrometry 83, 87, 89-93

Wavelength-dispersive spectrometry ..520-524analysis of cartridge brass 530defined 683-684detection limits 522dot map for minor constituent. 527dot mapping 525-529effect of bremsstrahlung sensitivity 528and energy-dispersive spectrometry,

compared 521-522instrument selection 522light-element analysis 522qualitative 522-525spectral resolution 521-522stainless steel. 87-88

Wavenumberdefined . . . . . . . . . . . . . . . . . . . . . . . . . . . . .684and depth of wave penetration, infrared

spectroscopy 113infrared spectra, as frequency 110SI derived unit and symbol for 685

Weak-beam microscopybright-field image of dislocation tangle,

aluminum alloy .467for defect analysis .466-467for high-resolution diffraction contrast

images .446showing dislocations in molybdenum-

implanted aluminum .484Wear

AES analysis of 566debris, SEM analysis .490elements, determined in petroleum products

by XRS 82metals, OES analysis in oils 21surface, AES analysis for 549

Wedging, mechanical, for sputteringproblems 556

Weight, equivalent, defined 162Weight fraction of crystalline phases, XRPD

determined 333Weissenberg cameras, for diffraction

patterns 346Weissenberg pattern, single-crystal

diffraction 330Welding

ofrailroad rail, longitudinal residual stressdistribution in 391-392

relay weld integrity, gas mass spectroscopyfor 156

soundness, analyzed .478-481zone, chromium depletion in 179

Weld metalmicrostructure .478-480stainless steel, measurement of 8-ferrite

in 287Weld metal microstructural analysis

by AEM .478-481elemental compositions examined .479experimental method .479-480

Wet analytical chemistryfor inorganic liquids and solutions 7for inorganic solids .4-6for organic liquids and solids 10

Wet cutting, for optical metallography specimenpreparation 300

Wettability, of graphite 543Wet washing, liquid fire method 166White radiation. See also Continuum.

defined 325-326sources, UV/vIS 66

Wigner coefficients 290Wilks' ATR attachment, effects in

analysis 120-121Window

function, EXAFS data analysis ..... .413, 414

Index /759

spectrometer, ultrathin beryllium 519Window technique, for ATEM sample

preparation .451Wire

aluminum, EPMA analysis of connectionfailure 531-532

coated, as samples, x-ray spectrometry 95fiber textures in 245preferred orientation in 359

Wolfram, evaporation fields for 587Wood products, analytic methods for 9

xXANES. See X-ray absorption near-edge

structure.X-band microwave frequency, use in

ESR 255Xenon, ionization potentials and imaging fields

for 586Xenon lamps

arc AASIAFS 52sources, spectral output 76

XPS. See X-ray photoelectron spectroscopy.X-ray absorption. See also Absorption; X-ray

absorption near-edge structure.effect of absorption-edge energy 85and fluorescence, effect in

448mass absorption 84photoelectric effect. 84and scatter. 84in x-ray spectrometry 84

X-ray absorption near-edge structurein EXAFS analysis .415-416multiple scattering effects .410

X-ray analytical electron microscopycapabilities, and FIMIAP 583

X-ray and optical spectroscopy. See Opticaland x-ray spectroscopy; X-rayspectrometry.

X-ray anomalous scattering, capabilities .. .407X-ray area scans

across pure-element standard, map ofdefocusing 527

of dental alloy 525-526limit of spatial resolution 527

X-ray detectors. See also Detectors.effect with SEM .498

X-ray diffraction residual stress techniques.See also Diffraction methods 380-392

applications 380, 389-392basic procedure 384-387as confined to surfaces 382defined 684effect of Bragg's law 381estimated analysis time 380, 385general uses 380instrumental and positioning errors 387introduction and principles 381-382limitations 380macrostress measurement by 380microstress measurement by 380plane-stress elastic model of 382-384and proton microprobe 107related techniques 380samples 380, 384-385sources of error 387stress measurement, principles of 381-382subsurface measurement and required

corrections 388-389X-ray diffration stress measurement. See also

X-ray diffraction residual stresstechniques 381-382

X-ray diffraction. See also Diffraction 325-332analysis, types of 325Bragg's law 327,329capabilities 277,287,402,407,420,429,490



760/ Index

X-ray diffraction (continued)and crystallographic texture measurement and

analysis, compared 358defined 684detection methods, XRPD 331diffraction experiments, types of 329-332and extended x-ray absorption fine structure,

compared .417geometry of powder diffraction 331of inorganic solids, types of information

from .4-6introduction 325, 332line profile, factors controlling 331,332microstructure and magnetic properties,

relationship between 599of organic solids, information from 9pattern, for silica glass 398-399as residue analysis 177samples 325single crystal or polycrystalline 325spectral peaks 520stress measurement, principles of 381-382theory 325-329

X-ray elastic constantsdetermination for Inconel 718, 388recommended for ferrous and nonferrous

alloys 382in X-ray diffraction residual stress

techniques 387X-ray emission

characteristic 84continuum 83-84as radioactive decay mode 245ratio to Compton scatter peak, in x-ray

spectrometry 99in x-ray spectrometry 83-84

X-ray emission spectroscopy, defined 684X-ray energy, abbreviation for. 690X-ray fluorescence. See also X-ray

spectrometry.capabilities 102, 197, 233defined 684neutron activation analysis and,

compared 233and optical emission spectroscopy,

compared 21and PIXE, detection limits 105-106

X-ray fractographydetermined failure modes in refractory

materials 376of molybdenum crystal, fracture

surface 376-377X-ray gages, for chemical surface

studies 177X-ray interferometry, as x-ray

topographical 371X-ray line broadening applications 374X-ray maps, See also Dot mapping; Elemental

mapping; Mapping.analog and digitally filtered, of iron in

aluminum matrix .448defined 684by EMPA analog mapping 525-529or scan, of dental alloy 526and superimposed quantitative data, results

of. 529X-ray microanalysis

in analytical electron microscopy .... .446-449of diffusion-induced grain-boundary

migration .462by energy-dispersive spectrometry .461-464

X-ray microbeam method, for polycrystallinemicrostructure 374

X-ray photoelectron spectroscopy. See alsoElectron or x-ray spectroscopicmethods 568-580

applications 568, 576-579Auger parameter 572capabilities 549, 603

capabilities, and FIMIAP 583capabilities, compared with infrared

spectroscopy 109capabilities, compared with classical wet

analytical chemistry 161chemical shifts measured 572as compared with x-ray analysis and

AES 569defined 684depth analysis 573-574electronic transitions 569electron spectroscopy for chemical

analysis 568general uses 568of inorganic solids, types of information

from .4-6instrumentation 570-571introduction and principles 568-569kinetic energy measurement as basis of 85multiplet splitting 572nomenclature 569of organic solids, information from 9preparing and mounting samples 574-576qualitative analysis 571-572quantitative analysis 572-573related techniques 568samples 568, 574-576shake-up satellites 572spectrum, carbon Is lines in ethyl

trifluoracetate 572surface sensitivity 569-570use with Auger electron spectroscopy 554

X-ray photon emissionand fluorescent yield 86inner-shell ionization and de-excitation

by .433and secondary electron ejection 86

X-ray photons. See Photons.X-ray powder diffraction. See also Diffraction

methods 333-343applications 333,341-342automated 338Bragg's law 337Debye-Scherrer camera 335direct comparison method 340estimated analysis time 333Gandolfi camera 335general uses 333geometry of 331lllcorw'd"w method, XRPD analysis 340instrumentation 334-338internal/external standard methods 340introduction 333-334lattice-parameter method 339Laue camera 334-335limitations 333qualitative analysis 338-339quantitative analysis 339-340related techniques 333Rietveld refinement, capabilities of 344samples 333sources of error in 340-341spiking method 340standardless method 340

X-rays. See also Electron or x-rayspectroscopic methods; Optical and x-rayspectroscopy.

absorption 84-85absorption curve for uranium, as function of

wavelength 85absorption edges 85beams, in x-ray spectrometry 82characteristic 82-84, 326, 435collimating, basic methods .403continuum, as inelastic scattering

process .433as continuum radiation 83detection of. 326diffraction of 326-327

and elements, relationship in x-rayspectrometry 84

emission, as radioactive decay mode 245energy, vs mass absorption, in

copper. 85, 87family lines of. 522-523fluorescent yield and, defined 86, 87hard 83history of development 82-83mass absorption coefficients 85nature and generation of. 325-326photographic film detection 334primary, defined 679production, vs mass, PIXE analysis 104Rayleigh and Compton scatter of 85secondary, defined 681sequential or simultaneous detection 87soft 83sources 395, 570spectra, measuring 518-522spatial resolution, effect in microanalysis . .448spectrograph, defined 684spectrometers, EDS/WDS 518-522

X-ray spectrometers, EDS/WDS 518-522X-ray spectrometry. See also Energy-dispersive

x-ray spectrometry; Optical and x-rayspectroscopy; X-rays 82-1OJ

absorption edges 85advantages 82analysis time, qualitative 82applications 82, 94, 99-101basis for qualitative analysis 96boron and fluorine determined in borosilicate

glass 179Bragg's law 87calculation of LLD 96capabilities " 197,212,243,333capabilities, compared with infrared

spectroscopy 109capabilities, compared with classical wet

analytical chemistry 161characteristic x-rays 82, 83-84of coal " 100continuum 83defined 684electromagnetic radiation 83elements and x-rays, relationships

between 84-85emission 85-87energy-dispersive x-ray spectrometers 89-93general use 82of inorganic liquids and solutions, information

from 7of inorganic solids, types of information

from .4-6instrumentation 87-93interelement effects 87introduction 82-83limitations 82mass absorption coefficient 84neutron activation analysis and,

compared 233operation 89of organic liquids and solutions, information

from 10of organic solids, information from 9photoelectric effect. 84Planck's constant 83qualitative analysis 95-96quantitative analysis 96-99related techniques 82sample preparation 93-95samples 82, 88, 93-95, 99-101scatter of x-rays 84selectivity of. 96of stainless alloy 178wavelength-dispersive x-ray

spectrometers 87x-ray emission and absorption 84



X-ray spectroscopy. See X-ray spectrometry.X-ray topography. See also Diffraction

methods; Reflection topography . . . .365-379applications 365. 375-379estimated analysis time 365general uses 365introduction 366-368limitations 365methods and instrumentation 368-375related techniques 365samples 365types of 368-375

X-ray tubesanode materials 89-90Coolidge 88excitation vs secondary-target excitation, x-ray

spectrometers 89molybdenum, in wavelength-dispersive x-ray

spectrometer 88for x-ray spectrometry 87-90

X-ray wavelength and atomic number,Mosely's relationship between .433

XRD. See X-ray diffraction.XRPD. See X-ray powder diffraction.XRS. See X-ray spectrometry.Xylenol orange, as metallochromic

indicator 174XYZ transition, as x-ray notation 569X zeolites, Raman analysis of pyridine on 134

y

Yielding, studied by x-ray topography andsynchrotron radiation 365

Yield, of secondary and backscatteredelectrons 502

Yield strength, aluminum-killed steels, inertgas fusion analysis 231

Y lens, gas mass spectrometer 153Young's modulus. See Modulus of elasticity.

Ytterbium, TNAA detection limits 237Yttrium

fluoride separation 169segregation, at grain boundaries .483species weighed in gravimetry 172weighed as the fluoride 171

Y zeolites, Raman analysis of pyridine on 134

Z. See Atomic number.ZAF corrections

defined 684in EDS mapping 528

Zeeman effectbackground correction for 51-52defined 264, 684

Z elements, x-ray tubes for 101Zeolites

transition metals as source of fluorescenceon 130

X and Y, Raman spectroscopy of pyridineon , 134

Zero-dispersion double spectrometer, withTriplemate device 129

Zero-field splitting, in ESR spectra 261Zero-order Laue zone

abbreviation for 691-CBED patterns .439, 441

Zincconstant-current electrolysis 200-containing copper, digital composition

map 528determined by controlled-potential

coulometry 209dot map, diffusion-induced grain-boundary

migration in 527EDTA titration 173evaporation fields for. 587gravimetric finishes 171

Index /761

ICP-determined in plant tissues .41ICP-determined in silver scrap metal .41indirect Volhard titration 173species weighed in gravimetry 172TNAA detection limits 238volumetric procedures for 175weighed as the phosphate 171weighed as the sulfide 171

Zinc oxidein binary phosphate glasses 131lattice image of. .446LEISS spectra 604quantitative XRPD analysis in calcite 342

Zinc-phosphate coating, Auger imagingof 556, 558

Zinc selenldeas internal reflection element. 113as internal reflection element, in surfactant

study 118Zircon, fusion flux for 167Zirconium

AFS analysis of .46epithermal neutron activation analysis 239evaporation fields for 587gravimetric finishes 171high-energy neutron irradiation of. 234organic precipitant for 169photometric analysis methods 64solvent extractant for 170species weighed in gravimetry 172TNAA analysis for. 234weighed as the phosphate 171

Zirconium alloys, analysis for manganese byperiod ate method 69

Z lens, gas mass spectrometer 153ZOLZ. See Zero-order Laue zone.ZOLZ·CBEDPs. See Zero-order Laue zone.Zone axis patterns, use in identifying unknown

phases/particles .456-457Zone-refined

abbreviation for 691nickel rod, sulfur segregation in 562



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