sample processing and analysis in the laboratory wolfgang … team/fritsch/fritsch data/lecture...

Sample Processing and Analysis in the Laboratory

Wolfgang SimonApplications Manager

FRITSCH GMBH Manufacturers of Laboratory Instruments

Industriestrasse 8D - 55743 Idar-Oberstein

GERMANY

http://[email protected]

Contents

Sample processingTaskComminution physicsComminution instruments

Particle size analysisTaskPhysics, MathematicsInstruments

Dividing

Laboratory instruments from the expertswith a worldwide reputation

Your partner for 80 yearsin the processing laboratory

Introduction

Laboratory analysisSample preparation

Sample processingto provide exact, reliable and reproducible samplesfor accurate functioning of the analytical instrumentsno poorly prepared samples

great risk of errorscorrect selection of comminution equipment and techniques

Sample Preparation

exact, reliable and reproducible samples

for accurate functioning of the analytical instruments

no poorly prepared samples

great risk of errors

correct selection of grinding technique and instrument

Task

comminution process

particle characterisationTOC instruments in environmental analysisXRF instruments in trace analysis

extend of comminutionhomogeneity of mixturessuitability for printing of dyestastegelation perioddrying behaviour

Main Criteria for the Selection of a Laboratory Grinder

Type of materialPhysical and chemical properties

Initial sample characteristicsFeed size (pre-crushing required ?), Quantity, Number of samplesMilling time, CleaningRepresentative sample

Universal applicabilityFinal sample characteristics

Contamination, AbrasionFinal particle size, Particle size range

Classification of comminuted products bysize

Fineness Definition

Term Upper particle size

Crushing > 5 mm

Grinding < 5 mm

Fine grinding < 100µm

Micro-fine grinding < 10 µm

Ultra-fine grinding < 1 µm

Mohs-Hardness

M ohs ‘

hard -ness

M ateria l

1 Talcum , graph ite , kao lin ite1.5 S oda, c lay , k iese lguhr2 G ypsum , b itum en, kao lin , su lphur, rock sa lt, po tash, b icarbonate o f

soda, n itre2.5 S ilver3 C alc ite , an thrac ite , bary tes , asbestos

3.5 D olom ite , copper ore4 F luorite , z inc b lend

4.5 S iderite , m agnes ite5 A patite

5.5 G ehlen ite6 Felspar, iron, hornb lende

6.5 P yrites , iron ore7 Q uartz , flin t8 Topaz9 C orundum

9.5 Fused corundum , s ilicon carb ide10 D iam ond

Hard

MediumHard

Soft

Material Properties

∫=B

VdEB

ε

εεσ0

)(EBv Energy expended until failureσ Stressε Strain

brittle (rocks) low fracture worklow comminution energy

elastic (steel) high fracture workhigh comminution energy

plastic (rubber) high fracture worklow comminution energy

visco-elastic high fracture work(thermoplastics) low comminution energy

Material Classification

Hard/Tough: most ferro alloys (ferro manganese, ferrovanadium, etc.), hardmetal tungsten carbide, slags, castings

Hard/Brittle: most minerals (quartz, basalt, granite, etc.), ceramics, refractories, cement, glass, coke

Medium Hard/Tough: bones, wood, leather, sewage sludge, PC-boards

Medium Hard/Brittle: coal, dragees/tablets, feed pellets, bakelite, gypsum, soils, demolition waste (rubble)

Soft/Brittle: inorganic salts, epoxy resins, pharmaceuticalpowders, detergents, pigments, foodstuff

Soft/Elastic: plastics, rubber, textiles, dry plants, cereals, cellulose, waste

Comminution Principlesaccording to Rumpf

cuttingpressure friction percussion

impact shearing

F = force, v = speed

Suitability for Comminution

Material property Pressure Percussion Friction Impact Shearing Cutting

hard and abrasive ++ ++ - ++ - -

hard and brittle ++ ++ - ++ - -

hard and tough ++ ++ - - - -

medium-hard ++ ++ - ++ + -

elastic and soft - - ++ - ++ ++

soft and brittle ++ ++ ++ ++ ++ +

soft and tough ++ ++ ++ + ++ ++

fibrous + - ++ ++ ++ ++

temperature-sensitive

- + - + ++ ++

moist and plastic + - ++ - ++ ++

Correlation between Material Behaviour and Comminution Principles

Overview

Action between two Crushing Tools

Percussion Action (i.e. Vibratory Micro Mill)

For fine milling of dry lab samples or solids in suspension.

For homogenization of emulsions or pastes.

Vibratory Micro Mill “pulverisette 0”

Operatingprinciple

Percussion

Max. feed size 5 mmMax. capacity 10 mlFinal fineness 5-10 µmHard (abrasive) +Medium-hard ++Soft +Brittle ++Tough -Fibrous +Temperature-sensitive

++

Moist ++

Analytical chemistry (spectral and XRF-analysis), electronmicroscopy, nuclear research, mineralogy, microbiology

Main advantages over the competition

Ergonomic designFrequency controlled amplitudeDigital timer and amplitude settingsLow power consumptionGrinding Head includedCryogenic millingGrinding head includedTÜV-Safety


Pressure Action (i.e. Jaw Crusher)

Mining and metallurgy: Niobium-titanium, ferrovanadium, chromevanadium, tungsten carbide, ores, coal, slag, cokeChemicals: wide variety of various rawmaterials in the chemical industryGeology and mineralogy: Rocks, granite, basalt, barite, silicatesGlass industry: Frits, glass, rawmaterialsCeramics: Steatite, fire-clay, sinteredceramics, electroporcelainConstruction materials: Bauxite, clinker, quartz, concrete

Jaw Crusher “pulverisette 1”

Operating principle PressureMax. feed size 95 x 95 mmMax. capacity 200 kg/hFinal fineness 1-15 mmHard (abrasive) ++Medium-hard ++Soft +Brittle ++Tough -Fibrous -Temperature-sensitive +Moist -

Mining, iron and steel industry, geology, mineralogy, glass + ceramics, construction materials, raw materials, chem. industry


Closed grinding chamberCast-iron housingGap settingSmooth crushing plates

Easy CleaningLonger use

Conversion kit1,1/2,2kW - motors TÜV-SafetyLarge mouth openingCrushing ratio 1:100


Combined Friction and Pressure Action (i.e. MortarGrinder)

Mining and metallurgy: Ores, coal, coke, ashes, slagsChemistry: Fertilisers, dyes, pesticides, salts, detergents, synthetic resins, paintsGeology and mineralogy: Minerals (up to and includinga Moh’s hardness of 9), calcite’s, quartz, silicatesGlass: Sand, frits, glass, raw materialsCeramics: Porcelain, fire-clay, sintered ceramics, clayAgriculture: Soil samples, fertilisers, organic plant materialsFoodstuffs: Confectionery, gelatine, spices, yeast, pasta, sugarMetallurgy: Bauxite, slags, additivesPharmacy: Dragees, drugs, tablets, pastes rawmaterialsRocks and soils: Gypsum, lime, clinker, sand, cementElectrical Industry: Graphite, semi-conductors, insulating materials

Mortar Grinder “pulverisette 2”

Operating principle Pressure,friction

Max. feed size 8 mm

Max. capacity 150 ml

Final fineness 10-20 µm

Hard (abrasive) -

Medium-hard ++

Soft +

Brittle ++

Tough -

Fibrous +

Temperature-sensitive ++

Moist ++

Chemistry, pharmacy, stones and soils, bauxite, gypsum, foodstuffs


Combined Pressure and Shearing Action (i.e. Disk Mill)

Mining and steel industries: Ores, coal, coke, slagsCeramics: Steatite, sintered ceramics, electrotechnical porcelain, fire-proof clayRocks and soils: Bauxite, slags, quartz, clinker, gypsum, chalkGlass: Frits, glass types, raw materialsSoil research: Dried soil samples, sewage sludge, hydrological sediments, drilling cores, Briquettes, Coke, Limestone, Thomas meal (potash), Pumice stone


250W – motor

Rimmed, protected mortar bowl

Very robust Construction

Large range of grinding pressure

Easy setting of scraper

TÜV - Safety

Laboratory Disk Mill “pulverisette 13”

Operating principle Shearing,pressure

Max. feed size 20 mm

Max. capacity 150 kg/h

Final fineness 0.1-12 mm

Hard (abrasive) +

Medium-hard ++

Soft +

Brittle ++

Tough -

Fibrous +

Temperature-sensitive -

Moist -

Mining, iron and steel industry, ceramics + glass, constructionmaterials, soil research


Design and constructionTÜV - SafetyDust tight, connection to dust exhaustCompact, small instrumentMaintenance-free motorReproducible gap setting (steps of 0.1 mm)Easy access for cleaningGrinding disks WC+Co, ZrO2

Combination possibility with p-1

“pulverisette 1” in combination with “pulverisette 13”

Fine grinding from 95 mm to 0.1 mm in one working stepMounting rack and chute in combination with the Jaw Crusher „pulverisette 1“, model I + II and the Disk Mill „pulverisette 13“ make it possible to grind 95 mm feed material down to a final product fineness of 100 µm in a single process continuously.


Combined Percussion and Friction Action (i.e. Vibrating Cup Mill)

Mining: for processing of coal, ores or minerals forphysical or chemical analysisMetallurgy: for grinding blast furnace slag or castiron samples to determine additives neededCeramic industry: for grinding rock samples to produce raw powder to determine CaO3 and MgCO3 content or clinkers to study the constancy of themineralogical structureAgriculture and ecology: for preparing samples forchemical analysis of soils, sludges or vegetablematterInfrared and X-ray fluorescence analysis: forpreparing samples in a brief grinding period with no contamination by disruptive abrasion

Vibrating Cup Mill “pulverisette 9”

Operating principle Percussion,friction

Max. feed size 12 mmMax. capacity 250 mlFinal fineness 10-20µmHard (abrasive) ++Medium-hard ++Soft +Brittle ++Tough -Fibrous +Temperature-sensitive -Moist +

Geology, mineralogy, metallurgy, construction materials, glass + ceramics, mining, iron and steel industry

NEW - pulverisette 9 -

Vibrating Cup Mill

Our new model is the world’s only vibration cup mill with frequency converter control. This allows the vibration frequency of the motor to be optimally adapted to the load (grinding elements and grinding material) and the grinding is performed in a minimum of time.

Max. feed particle size: 12 mm

Useful capacity: 50, 100 or 250 ml

Final fineness: 10 – 20 µm


Up to 1,150 rpm for fast grinding

Different grinding sets, different materials

Noise insulation

Very heavy construction

Digital selection of operation time

2 kW – motor

TÜV - Safety


Combined Percussion, Impact and Friction Action (i.e. Planetary Ball Mill)

Planetary Ball Mills

Planetary Mill „pulverisette 5“

Operating principle Percussion


Max. capacity 4 x 225 ml

Final fineness <1µm

Hard (abrasive) ++

Medium-hard ++

Soft ++

Brittle ++

Tough +

Fibrous +

Temperature-sensitive +

Moist ++

Laser spectral analysis, chemistry, pharmacy, glass, ceramics, construction materials, coal, coke, mineralogy, geology, foodstuffs


bench top modelmodern design and technology digital rotation control8x80 ml volume bowls2 or 4 working stations. forced coolinghigh milling energyTÜV - SafetyGTM-SystemSafe-lock

Planetary Mono Mill „pulverisette 6“





Hard (abrasive) ++

Medium-hard ++

Soft ++

Brittle ++

Tough +

Fibrous +


Moist ++

Laser spectral analysis, chemistry, pharmacy, glass, ceramics, construction materials, coal, coke, mineralogy, geology, foodstuffs


patented planetary ball Synchronous beltsEasier adjustable counter weightBench top modelRS232 interfaceProgrammable interval, break time and reversingTÜV - SafetyGTM-SystemSafe-lock

Planetary Micro Mill „pulverisette 7“


Max. feed size 5 mm



Hard (abrasive) ++

Medium-hard ++

Soft +

Brittle ++

Tough -

Fibrous +


Moist ++

Chromatography, X-ray spectral analysis, biology, pharmacology, galenics, nuclear research, technical science


very versatile instrument (8 different materials)large range of quantities can be milled (up to 40 ml)best results in fine milling and simultaneousmixing/homogenising2 samples milled simultaneouslyeasy cleaning of bowlshigh milling energy and fast millingTÜV - Safety

Vario-Planetary Mill „pulverisette 4“




Final fineness < 1 µm

Hard (abrasive) ++

Medium-hard ++

Soft ++

Brittle ++

Tough ++

Fibrous +


Moist ++

Research and development, technical science, mechanicalalloying, mechanical activation

Planetary Ball Mill - Geometry

( )ψα +⋅−+= cosZCorZpr FFFF)sin( ψαµ +⋅−⋅= Zrt FFF

2MMZp RmF ϖ⋅⋅= MPMCor RmF ϖϖ ⋅⋅⋅⋅= 2

( ) ⎟⎟⎠

⎞⎜⎜⎝

⎛+−⋅

=ψα

αcos

cos MPZ

RRF

⎥⎥⎦

⎤

⎢⎢⎣

⎡

−⋅⎟⎟

⎠

⎞⎜⎜⎝

⎛+⋅⋅⋅=

αϖϖϖ

cos1

2

P

M

P

MPPr R

RRmF

P

M

P

M

RR⋅⎟⎟

⎠

⎞⎜⎜⎝

⎛+=

2

1cosϖϖα

k

M

P

P

Mkrit

RR

nnk

ϕ−±−==

11

( )ψαα+−⋅

=cos

cos MP RRR

Detach Angle

Critical Speed Ratio

Trajectories of Balls

( ) kritopt kbisk ⋅= 9,03,0

M

Popt R

Rk ⋅+= 2,054,1

p-5 1 : -2.19

p-6 1 : -1.82

p-7 1 : -2

Sample Movement in Grinding Bowl

Sliding RegimeThrowing RegimeTurbulence RegimeCircle Regime

GTM System

FRITSCH In-situ data acquisition and monitoring systemduring mechanical alloying

Technique continuous measurement of temperature and pressure during mechanical alloyingin-situ registration of thermal effects and gas reactions during milling investigation of phasetransformation and reactions

Investigations on TiC, SiC, ZrC, TiB2, ZrB2Silicideamorphous alloys

Offer complete data aquisition for the planetary mills“Pulverisette 5”, “Pulverisette 6” and “Pulverisette 4” (IFAM corporately developed with FRITSCH GmbH) realisation of milling tests using the dataaquisition system

Application monitoring and optimization of milling processesbasic research in the field of mechanical alloying

GTM System

reaction heat (<2s) 30kJmaximum rotation milling plate max. 360rpmrange pressure sensor 0-1MParange temperature sensor 0-100°Cresolution temperature sensor 0.4Klow pressure range 0-120 kParesolution 0,47kPahigh pressure range about 100-400kParesolution 1,6kParesponse time of pressure sensor <1msacquisition rate single mode 100 data per secondacquisition rate dual mode 20 data per secondoperating time up to 80h


Mini Mill

For fine comminution of very small-quantities, dry laboratory samples or solids in suspension. For mixing and homogenization of emulsions

A real minimum quantity mill that still allows a suitable recovery even for forensic applications

Max. feed quantity: up to 5 ml

Throughput: up to 100 ml/h

Final fineness 10 µm

Action with one Grinding Tool

Battering Action (i.e. Variable Speed Rotor Mill)

Soft materials like plants, wood, roots, leaves, coniferous needles, spices, textiles, leather,chemicals, foodstuffs, grains, cellulose, fillers, chalk, kaolin, coal, soils (withoutstones).Medium-hard samples like drugs, dragées, tablets, fertilizers, pellets, fodderTemperature-sensitive samplesElastic-samples like styrene, polyester, plastics, foils,PVC, PP or PE

Variable Speed Rotor Mill “pulverisette 14”

Operating principle Impact


Max. capacity 5 l/h


Hard (abrasive) -

Medium-hard +

Soft ++

Brittle +

Tough +

Fibrous ++


Moist -

Foodstuffs, cereals, plants, textiles, wood, chemicals, plastics, animal feed, coal, soils


Motor speed 6,000 – 20,000 rpm, constant torque

Digital Display for rated speed

Soft-touch keyboard

Microprocessor controlled

TÜV - Safety


Combined Percussion and Friction Action (i.e. SoilDeagglomerator)

Preparation of soil samples forchemical and physical analysis, e.g. to determine the activeingredients relative to crop yieldor identification of pollutants.

Agglomerates are reduced to 2 mm grain size, e.g. as per thesewage sludge code or DIN 19683.

Soil Deagglomerator “pulverisette 8”

Operating principe Percussion,shearing

Max. feed size 30 mmMax. capacity 2 kgFinal fineness ‹ 2 mmHard (abrasive) -Medium-hard ++Soft -Brittle -Tough -Fibrous -Temperature-sensitive -Moist -

Institutes for soil investigations, agricultural research and investigation laboratories


Combined Cutting and Shearing Action (i.e. Cutting Mill)

Materials: rubber, leather, paper, cardboard, tissues, plastics, wood, non-metallic waste, coal, animal feeds, maize, grain, confectionery, malt, farinaceous products, spices, driedmeat, bones, horn, dragees, tablets, leaves, fibres, peat, roots, tobacco, cork, straw or film.Furthermore, the universal cutting millcan also be used in the pharmaceuticalor animal feed industries, in dental, medicinal and metallurgical technology as well as in veterinary institutes.

Cutting Mills

Universal Cutting Mill „pulverisette 19“ / Power Cutting Mill „pulverisette 25“

Operating principleCutting

p-19 p-25

Max. feed size 70 x 80 mm 120 x 85 mm

Max. capacity 60 l/h 85 l/h

Final fineness 0.25-6 mm 1.0-10 mm

Hard (abrasive) - +

Medium-hard ++ ++

Soft + +

Brittle ++ ++

Tough ++ ++

Fibrous ++ ++

Temperature-sensitive

- -

Moist - -


Fast locking lidEasy access and very easy cleaningRotorsLess sample depositVery stable and robustCutting geometryBearingsSample exhausterMotors Sieves cassettesTÜV - Safety

Cutting Mill „pulverisette 15“

Operating principle Cutting


Max. capacity 50 l/h


Hard (abrasive) -

Medium-hard -

Soft ++

Brittle +

Tough +

Fibrous ++


Moist -


Cutting Mill

Our decades of experience in the production of cutting mills have been invested in our new model with significantly improved grinding material feeding and grinding material recovery. The head of our laboratory is excited by this instrument.

Max. feed particle size: 60 mm

Throughput: up to 50 l/h

Final fineness depending on the

selected sieve insert: 0.25–6 mm


Double bearings

Easy Cleaning

Cooling

Dust exhaust

Fast grinding

TÜV - Safety

Cross Beater Mill „pulverisette 16“

Operating principle Impact


Max. capacity 80 l/h


Hard (abrasive) -

Medium-hard ++

Soft +

Brittle ++

Tough -

Fibrous +

Temperature-sensitive -

Moist -

Typical working ranges of different principles

Method Range

Dry sieving 63 µm – 125 mm

Wet sieving 20 µm – 200 µm

Micro sieving 5 µm – 100 µm

Gravitational sedimentation 0,5 µm – 500 µm

Laser diffraction 0,01 µm – 2000 µm

Electron microscope 0,05 µm – 1 µm

Projection microscope 1 µm – 10 mm

Particle size analysis everywhere

Powder metallurgy - sintering processes

Cement industry - reactivity

Chemical industry - paints, toners

Food industry - chocolate, rice, beans

Pharmaceutical industry - sprays, eye drops, tablets

Particle size

Particle features (measurable particle properties)

1. Geometrical features2. Mass3. Sinking speed4. Field disturbances

Instruments for Particle Size Analysis

Sieve Shaker

Laser Particle Sizer10 nm - 2,000 µm

Method RangeDry sieving 32 µm – 125 mmWet sieving 20 µm – 10 mmMicro sieving 5 µm – 100 µm

Sieving

Advantages

large Size rangelow costfractionationsimple handlingsieving tower with up to 16 sieves

Disadvantages

careful cleaningerrors caused by needle shaped particleserrors get larger with low sample weightsieving losses

FRITSCHSIEVE SHAKERS

Particle Size AnalysisSieve Shaker „analysette 3“ PRO

AMPCONTROL - rated amplitudeDigital display of actual amplitude and sieve vibrations per secondUp to 9 sieve programmes which can be saved and recalledTest equipment inspection in accordance with ISO 9001 (Sieve shaker can be calibrated as a testing instrument)Auto-validation of the sieving process via RS232 and AUTOSIEVE for Windows

NEW Sieve tensioning System TorqueMaster for Sieve Shakers

The sieve tensioning system has great influence on the sieving result. Therefore use the sieve tensioning system TorqueMaster, which enables an automatic, reproducible tensioning of the sieve stack.

Fast, easy handling

Enables calibration of sieve tensioning as part of the monitoring of test equipment according to ISO 9001.

Can be attached and used with any sieve shaker

Control and evaluation programme “autosieve”

For professional evaluation and filing of sieving results according to DIN ISO 9001

Automatic weighing of single sieves or sieve sets; capability of storing tare weights of sieves

Comprehensive presentation of results

On-line auto-validation of “analysette 3” PRO sieve shaker

Heavy Duty Sieve Shaker„analysette 18“

large sieve material throughputsieve diameter up to 450mm can be usedsieves with mesh widths of 63 µm to 125 mmmaterial quantity up to 6 kgsmooth and stable operationlow noise outputcontinuous operation possible

Particle Size AnalysisLaser-Particle-Sizer „analysette 22“

COMPACT

NanoTec MicroTec

Measuring Range

Model Measuring rangeWet dispersion

Measuring rangeDry dispersion

NanoTec 0,01 - 2000 µm 0,1 - 2000 µm

MicroTec 0,1 - 600 µm 0,1 - 600 µm

COMPACT 0,3 - 300 µm 0,3 - 300 µm

NEW “analysette 22” NanoTecLaser-Particle-Sizer

The world’s first laser measuring instrument for the determination of particle size distributions together with recognition of particle shape detection in a single process ! A completely new sensor geometry and revolutionary software make this world premiere possible.

Measuring range: 10 nm-2000 µm

Particle shape detection in the same process

Dual line measurement (wet and dry dispersion)

NEW “analysette 22” MicroTecLaser-Particle-Sizer

The MicroTec Version is the “little” brother of the NanoTec

Measures samples in the micron and sub-micron range

Measuring range: 0.1 - 600 µm

very compact and economical in space because of the shortenedoptical bench

All hardware and softwarecomponents are identically to those of the „analysette 22“NanoTec except of the Nano-measuring range

NEW “analysette 22” COMPACTLaser-Particle-Sizer

Our standard model with the unbeatable price-to-performance ratio enters the market with a complete overhaul and shows what even a small budget can still do in particle measurement technology.

Measuring range: 0.3 - 300 µm

Wet and dry dispersion in a single instrument

One-Touch operation

Conventional Design

FRITSCH Design „analysette 22“

convergent laser beam (patent)distance measuring cell - sensorfocal length of fourier lens

Particle Size Analysis Laser-Light-Scattering

Abbe - Porter Experiment

Diffraction Pattern

Fraunhofer - Mie

( ) 22)()( 10

2

⎥⎦⎤

⎢⎣⎡

⋅⋅⋅⋅⋅

==uak

uakJIPUPIFraunhofer Diffraction

⎟⎟⎠

⎞⎜⎜⎝

⎛⋅⋅

⋅⎟⎟⎠

⎞⎜⎜⎝

⎛=⎟⎟

⎠

⎞⎜⎜⎝

⎛

⊥

⋅⋅+⋅⋅−

⊥ i

illzkiRki

S

Sll

EE

Rkie

SS

EE

)(00)(

2

1

θθMie

Scattering

{ })(cos)(cos()1(

12)(1

1 θτθπθ nnnnnn

bagnnnS +⋅++

= ∑∞

=

{ }∑∞

=

+⋅++

=1

2 )(cos)(cos)1(

12)(n

nnnnn abgnnnS θτθπθ

Fritsch Particle Sizer 'analysette 22'

Meas.N o. 15 Da te 05-14-2002 Tim e 15:33 O perator D ieter Hahn ID 007 Serial No. 108

SiC CF 500in w ater + Na4P2O7 + Im bentin and ultra sonic

Measuring Range 0.31 [痠 ] - 300 .74 [痠 ] Pump 100[rpm]Reso lution 62 Channels (17 mm / 114 m m ) Stirrer 1[rpm]Absorption 10 .00 [% ] Ul trasonic 100Measurement Duration 3 [Scans]

Model l Independant

Fraunhofer Ca lcula tion se lected .

Inte rpola tion Values... C :\Program me\a22___32 \F RIT SC H \033-300.fps0 .09 % < 0.33 痠 0 .24 % < 0.40 痠 0.39 % < 0 .50 痠0 .63 % < 0.80 痠 0 .71 % < 1.00 痠 0.80 % < 1 .50 痠0 .84 % < 2.00 痠 1 .37 % < 5.00 痠 6.36 % < 8 .00 痠

16.09 % < 10 .00 痠 54.56 % < 15 .00 痠 83.38 % < 20.00 痠99.22 % < 30 .00 痠 100 .00 % < 40 .00 痠 100 .00 % < 50.00 痠

100.00 % < 60 .00 痠 100 .00 % < 70 .00 痠 100 .00 % < 80.00 痠100.00 % < 90 .00 痠 100 .00 % < 100.00 痠 100 .00 % < 150.00 痠100.00 % < 200.00 痠 100 .00 % < 250.00 痠 ****** % < 300.00 痠

Inte rpola tion Values... C :\Program me\a22___32 \F RIT SC H \10_100.fpv10.00 % < 8.89 痠 20.00 % < 10 .59 痠 30.00 % < 11.92 痠40.00 % < 13 .16 痠 50.00 % < 14 .39 痠 60.00 % < 15.73 痠70.00 % < 17 .29 痠 80.00 % < 19 .25 痠 90.00 % < 22.09 痠

100.00 % < 34 .66 痠

Software and Hardware

PC minimal 486DX2, 66 MHz(better if faster)

8 MB RAM1 free COM port1 free slot for ISA bus cardWindows 3.1 / 3.11 or Win 95 or higherPrinter

Rotary Cone Sample Divider „laborette 27“

Representative division of dry solids or suspensions

Dividing heads with ratios1:8, 1:10 and 1:30

Representative division of randomly segregatedsamples

Main Advantage of Rotary Cone Sample Divider

Rotation of Cone:

spreading sampleover 360°

splitting sample intovery small volumeelements

feeding samplesimultaneously to thesample containers

Importance of sample dividing

Rotary Cone Sample Divider

Without sample dividing = Not representative

Normal Sample Divider

GMP, GLP RegulationsValidation

Validation confirms that products with pre-determined quality characteristics and attributescan be reproduced consistently / reproduciblywithin the established limits of themanufacturing process operation at themanufacturing site.

Validation is an ongoing commitment that isintegral to every aspect of commercial productmanufacturing.

Validation of Equipment and Equipment Systems

Category I equipmentreliability can be assured through calibration and preventive maintenance programs (i.e. balances, pHmeters, pipettes).

Category II equipmentneeds validation (i.e. process equipment, test equipment, air systems, clean rooms, etc.)validation is commonly performed as a 3 phaseprocess consisting of Installation Qualification (IQ), Operation Qualification (OQ) and Performance Qualification (PQ).

IQ - Installation Qualification

Documentation of the installation of theequipment, including

"As built" drawingsEquipment or system requirementsA statement declaring the adequacy of the equipmentfor it's intended useEquipment identity characteristicsUtility requirementsSafety featuresReference to operator or maintenance manualsReference to vendor support services or partssuppliers

OQ - Operation Qualification

Confirmation of the adequate operation of theequipment as expected under ideal conditions, including

Calibration of sensors and measuring devicesQualification of

support processing (i.e. equipment cleaning, disinfection)monitoring or controlling softwaretest methods

A systematic demonstration of electromechanical features and functionscycle performanceprocess consistency (i.e rotational speed)safety features and reset procedures after likely eventslike a power failure.

OQ - Operation Qualification

The OQ protocol must be supported by SOPs on topics such as

operating

cleaning

assembling and calibrating the equipment

perform routine maintenance programs

PQ - Performance Qualification

heart of validationconfirmation that the equipment will continue to operate as expected under routine and challenged conditions of operation and that theoutcome is acceptable. It is basically about challenging the equipment to confirm its operation within the establishedlimits of operation. This run must bedemonstrated repeatedly in 3 consecutivesuccessful runs.

sample processing and analysis in the laboratory wolfgang … team/fritsch/fritsch data/lecture...

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