features of jobin yvon icp spectrometers - horiba€¦ · linear dispersion: 0.4 nm/mm working...

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Features of Jobin Yvon ICP Spectrometers Jobin Yvon S.A.S., Emission Division, Application Laboratory, May 2003 1 Radio Frequency (RF) Generator 1.1 Solid-state generator The solid-state generator offers a short warm-up time, 15 minutes compared to 45 minutes for typical free running generators. 1.2 40.68 MHz generator The JY 40.68 MHz generator has the following advantages over a 27.12 MHz generator: a) Lower background noise leading to an improved signal-to-background ratio and lower detection limits; b) More efficient RF coupling leading to increased power transfer efficiency and a superior more robust plasma; c) Low argon consumption; d) Excellent analytical precision due to stable plasma; 1.3 Forward power regulation Stability is better than 0.1%. Power regulation compensates for slow fluctuations in line power supply (±15). 1.4 Computer controlled generator The generator offers computer programmable RF power, start and shutdown of the plasma. It has continuously adjustable, computer-controlled, variable power from 800 to 1550 W. 1.5. Safety interlocks JY ICPs have a number of safety interlocks to protect the users and the instrument. They include: a) Argon gas pressure and flow b) Cooling water pressure and flow c) Plasma compartment door closure d) Excessive reflected power 2 Sample introduction 2.1 Nebulizers Any of the following nebulizers can be supplied with the JY ICP Spectrometers: a) Pneumatic Concentric Nebulizer This is a one-piece concentric glass type nebuli- zer. It is recommended for the analysis of clean solutions with high acid and salt concentrations, as well as organic solvents. This nebulizer gives excellent long term precision and detection limits. JY uses Type C as the standard, however Types A and K are also available. Figure 1: Pneumatic Concentric Nebulizer ICP OPTICAL EMISSION SPECTROSCOPY TECHNICAL NOTE 07

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Page 1: Features of Jobin Yvon ICP Spectrometers - Horiba€¦ · Linear Dispersion: 0.4 nm/mm Working Resolution: 0.012 nm Recommended application: rare earths and geologi-cal. Spectral

Features of Jobin Yvon ICP Spectrometers

Jobin Yvon S.A.S., Emission Division, Application Laboratory, May 2003

1 Radio Frequency (RF) Generator

1.1 Solid-state generator

The solid-state generator offers a short warm-uptime, 15 minutes compared to 45 minutes fortypical free running generators.

1.2 40.68 MHz generator

The JY 40.68 MHz generator has the followingadvantages over a 27.12 MHz generator:a) Lower background noise leading to animproved signal-to-background ratio and lowerdetection limits;b) More efficient RF coupling leading to increasedpower transfer efficiency and a superior morerobust plasma;c) Low argon consumption;d) Excellent analytical precision due to stableplasma;

1.3 Forward power regulation

Stability is better than 0.1%. Power regulationcompensates for slow fluctuations in line powersupply (±15).

1.4 Computer controlled generator

The generator offers computer programmable RFpower, start and shutdown of the plasma. It hascontinuously adjustable, computer-controlled,variable power from 800 to 1550 W.

1.5. Safety interlocks

JY ICPs have a number of safety interlocks to

protect the users and the instrument. Theyinclude:a) Argon gas pressure and flowb) Cooling water pressure and flowc) Plasma compartment door closured) Excessive reflected power

2 Sample introduction

2.1 Nebulizers

Any of the following nebulizers can be suppliedwith the JY ICP Spectrometers:

a) Pneumatic Concentric NebulizerThis is a one-piece concentric glass type nebuli-zer. It is recommended for the analysis of cleansolutions with high acid and salt concentrations,as well as organic solvents. This nebulizer givesexcellent long term precision and detection limits.JY uses Type C as the standard, however TypesA and K are also available.

Figure 1: Pneumatic Concentric Nebulizer

ICP OPTICAL EMISSION SPECTROSCOPY

TECHNICAL NOTE 07

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b) Parallel Flow Nebulizer

This is a one-piece Teflon nebulizer.

It is ideal for high dissolved solids and for solutionswith suspended particles. It is recommended for HFacid based solutions.

Figure 2: Parallel Flow Nebulizer

c) Steel-Zirconium Nebulizer

For the analysis of suspensions in oils, for examplewear metals.

d) Ultrasonic Nebulizer

For the analysis of sub-ppb concentrations in alltypes of samples with the exception of HF acidsolutions.

e) Hydride Generator

For increased sensitivity of the hydride forming ele-ments As, Bi, Ge, Hg, Pb, Sb, Se, Sn and Te.

f) Concomitant Metals Analyzer (CMA)

This patented Hydride Generation System is onlyavailable from JY. It provides the opportunity to

analyze the hydride and non-hydride forming ele-ments in a single analysis. The sensitivity of thehydride forming elements is enhanced and the sen-sitivity of the non-hydrides is not adversely affect-ed.This accessory increases productivity andreduces cost of analysis.

Figure 3: Concomitant Metals Analyzer

g) Spark Ablation

This accessory provides for the direct analysis ofconductive solids, such as metallurgical materials,without the need of sample preparation.

ICP OPTICAL EMISSION SPECTROSCOPY

TECHNICAL NOTE 07

Argon

Sample capillary tube

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ICP OPTICAL EMISSION SPECTROSCOPY

TECHNICAL NOTE 07

2.2 Sheath Gas

The argon sheath gas, originally patented by JobinYvon, enhances performance and stability in alltypes of matrices, but especially high solids orsalts. This device provides an additional argonstream that isolates the sample from the walls ofthe injector, thereby reducing contact and sampledeposition in the injector tube and tip.

This feature allows for the aspiration of solutionscontaining 30% salt directly into the plasma with-out blockage or drift. It also allows for the improve-ment of the Alkali detection limits via a computercontrolled increase in gas flow to allow for the opti-mization of viewing height.

2.3 Large Sample Injector Tube

JY uses a large 3 mm alumina sample injector tube,this has several advantages, firstly it allows for theanalysis of solutions containing high dissolvedsolids without blockage and drift. The use of the 3mm injector tube also creates a chain reaction ofother advantages: it increases the residence time,this improves the energy transfer efficiency foratomisation, this gives rise to an increased Mg ratioand makes the plasma more “robust”, and thusreduces matrix interferences.

2.4. Self-Aligning Demountable Torch

The Ryton torch body holds the inner and outerquartz tubes as well as the alumina injector tube. Allthree tubes are easily removed for cleaning andreplacement. No alignment is necessary whenreplacing tubes, as they are pre-aligned. All levels ofoperators can dismantle, clean, and reassemble thetorch.

A fully demountable torch is also more cost effec-tive than a one-piece torch, since the tubes can bereplaced as needed without replacing an expensivetorch assembly.

Figure 5: The demountable torch

2.5 Easily Interchangeable Cassettes

The torch and sample introduction system ismounted on a pre-aligned cassette. This allows forfast changing without the need for alignment andoptimization each time. Cassettes are available forall types of samples including aqueous, organic, HFsolutions and hydride generation.

The spray chamber is held in place with a spring-loaded clip, allowing for changing or cleaning with-out the need to remove the entire cassette.

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ICP OPTICAL EMISSION SPECTROSCOPY

TECHNICAL NOTE 07

Figure 6: The JY cassette, which includes thedemountable torch, the spray chamber, and nebu-lizer.

2.6 Viewing Zone of the Plasma

The large transfer optics of the JY ICPs allows forviewing the entire 6 mm of the Normal AnalyticalZone (NAZ) at once. By viewing the entire emissionzone at one time, the signal is increased and opti-mization of conditions on one element gives excel-lent results on all elements. This eliminates anymoving torch mechanisms, thereby increasing thespeed and eliminating worries about repositioningaccuracy or reproducibility. It also eliminates anywear and tear due to moving parts.

Other manufacturers offer auto-alignment hardwareand software as a so-called benefit. However, thisfeature is only necessary due to the limited opticaldesign that does not allow for viewing the entireNAZ. For instance, there is no way to automatesuch a routine for axial plasma viewing.

2.7 Argon Humidifier (option)

The argon humidifier minimizes sample depositionin the torch injector and nebulizer tip by saturingthe nebulizer argon flow with water. Improved pre-cision and less interferences are found when ana-lyzing samples with high dissolved solids.

2.8 AS 421 Autosampler (option)

Unattended analysis of up to 540 samples with theAS 421 computer controlled, programmable randomaccess automsapler. It features the choice of a vari-ety of sample and standard racks.

2.9 Water Recirculator (option)

The water recirculator is necessary for providing asafe, environmentally friendly controlled means ofcooling the RF coil.

3 Optics

3.1 Minimum of Optical Surfaces

Each optical surface causes light loss, the amountdepending on the type of optical surface and thecoating. Therefore, minimizing the number of opti-cal surfaces improves light throughput. Theincreased light throughput improves the sensitivityand detection limits of the instrument.

Figure 7: Czerny-Turner optical configuration, show-ing the small number of optical surfaces.

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ICP OPTICAL EMISSION SPECTROSCOPY

TECHNICAL NOTE 07

3.2 Choice of Slit Widths

The JY sequential instruments provide automatedsoftware that selects the most appropriate slitwidths for an analysis based on user input. If pre-cision is of primary importance, the slit widths canbe increased. When the best detection limits pos-sible are required, using the smaller slit widthswould be appropriate.

3.3 Holographic Grating

Holographic gratings offer the advantage of mini-mum stray light and no ghost images in comparisonto ruled gratings. They provide clean spectra and animproved signal-to-background ratio, thus providingimproved (lower) detection limits.

Holographic gratings are manufactured using pre-cise laser technology, whereas ruled gratings aremade using mechanical methods that lead tounavoidable ruling imperfections resulting inincreased stray light, higher background and higherdetection limits.

3.4 Large Grating

The signal gathering power of an instrument isdirectly proportional to the grating area. A largergrating area provides more signal, allowing for high-er signal-to-background ratio and therefore superiordetection limits. JY uses the entire surface of thegrating for even more light throughput. Using a largergrating allows JY to use lower orders of light andstill achieve excellent resolution. Lower order offermore signal, which results in shorter integrationtime and faster analysis.

3.5 Choice of Grating

The following gratings are available for the instru-ments indicated:

Spectral Range: 160 - 800 nm (120 - 800 nmwith the Halogen Option)

Linear Dispersion: 0.4 nm/mm in 1st orderWorking Resolution: 0.005 nm in 2nd order,

0.010 nm in 1st order* This grating is used for the JY 2000-2 with theVUV option for the analysis of halogens.

Spectral Range: 160 - 800 nm (120 - 800nmwith Halogen Option)

Linear Dispersion: 0.4 nm/mm Working Resolution: 0.012 nm

Recommended application: rare earths and geologi-cal.Spectral Range: 160 - 500 nm Linear Dispersion: 0.26 nm/mm Working Resolution: 0.007 nm

Recommended application: Rare Earths, Geologicaland Precious Metals, where full spectrum isrequired.Spectral Range: 160 - 800 nm Linear Dispersion: 0.2 nm/mm (160 - 420

nm), 0.4 nm/mm (420 - 800 nm)

Working Resolution: 0.005 nm (160 - 420 nm),0.010 nm (420 - 800 nm)

3.6 Direct Drive Grating

JY Sequential instruments use a direct drive gratingsystem. The advantages of a direct drive follow:

a) Speed: Full wavelength coverage in 7 seconds,with a mechanical reproducibility of 0.0004 nm.

b) Precise analysis: A minimum step size of 0.0003nm permits correct peak location, thus providingmore accurate analyses.

2400 grooves/mm (1st and 2nd orders)JY ULTIMA 2, ULTIMA 2C and JY 2000-2*

2400 grooves/mm (1st order)JY 2000-2

3600 groove/mmJY ULTIMA 2 and ULTIMA 2C

Dual 4320 and 2400 groove/mm (two sided, back-to-back gratings)JY ULTIMA 2, ULTIMA 2C and JY 2000-2

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ICP OPTICAL EMISSION SPECTROSCOPY

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3.7 Simultaneous Internal Standard Capa-bility (option)

The internal standard option compensates forchanges in signal due to variations in nebulization,gas flows, RF power, electronics, voltage etc, byproviding a real time ratio to a reference element.The Internal Standard Monochromator allows anyelement wavelength to be used as an internal stan-dard.

3.8 Thermal Regulation of Optics

The optics are thermally regulated to within ±1oCto provide excellent long and short term stability in the real lab environment. The temperature can beadjusted to compensate for the highest temperaturereached in the laboratory environment, up to 40oC(104°F).

3.9 Nitrogen Purge for UV Sensitivity

The use of a nitrogen purge allows for the analysisof elements below 190 nm with excellent detectionlimits. The purge includes not only the monochro-mator itself, but also the optical path from the plas-ma to the monochromator.

The use of the nitrogen purge allows for the analy-sis of wavelengths down to 160 nm, such as themost sensitive line of Al, at 167 nm. With the Halo-gen option this wavelength range can be extendeddown to 120 nm for the analysis of Cl, Br, and I.

The use of the nitrogen purge also extends the life-time of the optics by keeping out dirt, dust, and anysample residue. Vacuum pumps will deposit a filmof oil on the surface of the optics and grating, thusrequiring regular cleaning of the optics.

3.9.1 Nitrogen Generator (option)

A nitrogen generator produces nitrogen from com-pressed air, reducing operating costs and eliminat-ing the need for a dedicated nitrogen gas supply. JYoffers several models of nitrogen generators thatprovide high purity nitrogen (99.9995%) from 3-6

L/minute.

3.10 Far UV Analysis (option)

The VUV analysis option allows for the analysis ofthe Cl, Br, and I at wavelengths in the VUV. Forexample, Cl is analyzed at 134 nm with a typicaldetection limit of 200 ppb. For analysis between120 - 160 nm, it is necessary to use MgF2 opticsand increase the nitrogen purge. This feature can beadded to the system as an upgrade once the instru-ment is installed.

3.11 Upgrade to a Combination ICP

Any sequential JY ICP can be upgraded in the fieldto a combination simultaneous/sequential spec-trometer with the addition of a polychromator. Theviewing of the plasma is done through a directtransfer of the light, with no fiber optic connections.

3.12 High Dynamic Detector system(HDD®)

The patented High Dynamic Detector system pro-vides optimum detection across the full range ofthe spectrum from 160 to 800 nm (down to 120with the optional halogens kit). They allow meas-urement of concentration levels ranging from ppb topercentage levels, giving a dynamic range of 108

(compared with 104 for instruments with solid-statedetectors).

4 Analyst™ Software

4.1 Analyst V5 Software

The software runs under Windows 95/98/NT. As aWindows based package the software is intuitivefor the novice user. Some of the features include:

(a) Step-by-step guide through the creation of amethod with the "Wizard"

(b) Library of over 125,000 lines

(c) Compatibility with automatic, random accessautosampler for unattended analysis

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ICP OPTICAL EMISSION SPECTROSCOPY

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(d) Multi-user security

(e) A choice of analytical mode of analysis, includ-ing single point and Gaussian fit

(f) Data export capability

(g) Correction for weight/volume dilution factors

(h) On-line help at any point in the software

Figure 8: The Analyst "Tasks and Sequences" win-dow.

4.2 Win-IMAGE and IMAGE Navigator(option)

Win-IMAGE and IMAGE Navigator allow the fullacquisition of the spectrum in less than 2 minuteswith no compromise in optical resolution.

a) High dynamic range electronics

A patented electronic system extends the dynamicrange of the detector to 5 X 1010. It allows theacquisition on the same detector of both trace and major concentrations, eliminating possible satura-tion or necessary set up.

b) Fast acquisition electronics

A fast data acquisition board allows fast scanningand acquisition of the full spectrum

Data on acquisition of entire spectrum:

• Time: 115 seconds• Number of measurements: 228,900• Dynamic range: 5 X 1010

Figure 9: A spectrum acquired using Win-IMAGE

showing a wavelength range of 160 to 320 nm.

C. Software

The NAVIGATOR software brings the full power ofWin-IMAGE to the analyst in a user-friendly Win-dows environment.

Four main functions are available:

a) Search of a specific element in a spectrum

After selection of an element in the periodic table,NAVIGATOR displays the five most intense emissionlines for that element, overlaid with the correspon-ding parts of the spectrum to determine if the ele-ment is in the solution. The heights of the theoret-ical lines are calibrated for 10 ppm, allowing for anestimation of the element concentrations.

b) Peak identification

Mouse driven zooming capabilities allow the user to select any peak in the spectrum. NAVIGATOR iden-tifies the selected peak using a 125,000-line library, and then displays the five most intense lines forthat element to confirm identification and to esti-mate the concentration.

c) Full automatic semi-quantitative analysis

The most powerful feature of the NAVIGATOR, thesemi-quantitative analysis, returns the concentra-

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ICP OPTICAL EMISSION SPECTROSCOPY

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ICP OPTICAL EMISSION SPECTROSCOPY

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tion ranges of all elements selected by the user. Itfeatures:- Point and click selection of desired elements froma periodic table or selection of all ICP elements- Selection of concentration ranges- Display of the concentration results in a color-coded periodic table- Detailed reporting of the concentration results- ASCII storage of the results in any data process-ing software

d) Quantitative analysis

Calibration of the NAVIGATOR with standardsallows for quantitative analysis.Figure 10: The five most sensitive lines of Fe, dis-

played within Win-IMAGE, for two different sam-ples.

4.3 Remote Diagnostics (option)

Remote diagnostics allows remote access to thecomputer and instrument from a JY Service/Appli-cation Center for service troubleshooting and appli-cations support. Using a modem, the softwareallows all functions within the instrument to be tested. This lowers maintenance cost by elim-inating unnecessary service calls and reducesdowntime.

Note: Remote Diagnostics is not available in allareas of the world. Please contact Jobin Yvon Ser-vice for more information.

4.4 ALLIANCE Service

ALLIANCE is an extension of JY to more than 3500users of JY ICP, Glow Discharge, and Spark spec-trometers around the world.

The global program is accessed through the JYwebsite at www.jyhoriba.com/emission/alliance. Itoffers an online spare parts and accessories cata-log, which provides online quote requests andWorld Link - a user forum. This worldwide JY userdiscussion group features communication with ourapplications and service centers around the world.

1-866-JobinYvon

www.jobinyvon.com

In the USA:Jobin Yvon Inc.3880 Park AvenueEdison, NJ 08820Tel: 1-732-494-8660Fax: 1-732-494-8796E-mail:[email protected]

In France:Jobin Yvon S.A.S.16-18, rue du Canal91165 Longjumeau CedexTel: (33) 1/64 54 13 00Fax: (33) 1/69 09 90 88

Germany: (49) 89/46 23 17-0Italy: (39) 2/57 60 56 90U.K.: (44) 20/82 04 81 42

In Japan:Horiba Ltd.2 Miyanohigashi, KisshoinMinami-ku, Kyoto 601-8510TEL: (81) 75 313 8121FAX: (81) 75 321 5725www.horiba.com

China: (86) 10/6836 6542Spain: (34) 91/724 16 57Other Countries: Contact JYS.A.S.