sample processing and analysis in the laboratory wolfgang … team/fritsch/fritsch data/lecture...
TRANSCRIPT
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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]
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Contents
Sample processingTaskComminution physicsComminution instruments
Particle size analysisTaskPhysics, MathematicsInstruments
Dividing
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Laboratory instruments from the expertswith a worldwide reputation
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Your partner for 80 yearsin the processing laboratory
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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
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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
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Task
comminution process
particle characterisationTOC instruments in environmental analysisXRF instruments in trace analysis
extend of comminutionhomogeneity of mixturessuitability for printing of dyestastegelation perioddrying behaviour
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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
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Classification of comminuted products bysize
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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
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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
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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
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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
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Comminution Principlesaccording to Rumpf
cuttingpressure friction percussion
impact shearing
F = force, v = speed
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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 + - ++ - ++ ++
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Correlation between Material Behaviour and Comminution Principles
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Overview
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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.
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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
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Main advantages over the competition
Ergonomic designFrequency controlled amplitudeDigital timer and amplitude settingsLow power consumptionGrinding Head includedCryogenic millingGrinding head includedTÜV-Safety
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Action between two Crushing Tools
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
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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
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Main advantages over the competition
Closed grinding chamberCast-iron housingGap settingSmooth crushing plates
Easy CleaningLonger use
Conversion kit1,1/2,2kW - motors TÜV-SafetyLarge mouth openingCrushing ratio 1:100
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Action between two Crushing Tools
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
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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
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Action between two Crushing Tools
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
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Main advantages over the competition
250W – motor
Rimmed, protected mortar bowl
Very robust Construction
Large range of grinding pressure
Easy setting of scraper
TÜV - Safety
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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
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Main advantages over the competition
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
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“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.
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Action between two Crushing Tools
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
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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
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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
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Main advantages over the competition
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
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Action between two Crushing Tools
Combined Percussion, Impact and Friction Action (i.e. Planetary Ball Mill)
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Planetary Ball Mills
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Planetary Mill „pulverisette 5“
Operating principle Percussion
Max. feed size 10 mm
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
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Main advantages over the competition
bench top modelmodern design and technology digital rotation control8x80 ml volume bowls2 or 4 working stations. forced coolinghigh milling energyTÜV - SafetyGTM-SystemSafe-lock
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Planetary Mono Mill „pulverisette 6“
Operating principle Percussion
Max. feed size 10 mm
Max. capacity 1 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
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Main advantages over the competition
patented planetary ball Synchronous beltsEasier adjustable counter weightBench top modelRS232 interfaceProgrammable interval, break time and reversingTÜV - SafetyGTM-SystemSafe-lock
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Planetary Micro Mill „pulverisette 7“
Operating principle Percussion
Max. feed size 5 mm
Max. capacity 2 x 20 ml
Final fineness <1µm
Hard (abrasive) ++
Medium-hard ++
Soft +
Brittle ++
Tough -
Fibrous +
Temperature-sensitive +
Moist ++
Chromatography, X-ray spectral analysis, biology, pharmacology, galenics, nuclear research, technical science
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Main advantages over the competition
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
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Vario-Planetary Mill „pulverisette 4“
Operating principle Percussion
Max. feed size 10 mm
Max. capacity 2 x 225 ml
Final fineness < 1 µm
Hard (abrasive) ++
Medium-hard ++
Soft ++
Brittle ++
Tough ++
Fibrous +
Temperature-sensitive +
Moist ++
Research and development, technical science, mechanicalalloying, mechanical activation
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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
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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
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Sample Movement in Grinding Bowl
Sliding RegimeThrowing RegimeTurbulence RegimeCircle Regime
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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
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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
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NEW - pulverisette 23 -
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
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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
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Variable Speed Rotor Mill “pulverisette 14”
Operating principle Impact
Max. feed size 10 mm
Max. capacity 5 l/h
Final fineness 0.08-6 mm
Hard (abrasive) -
Medium-hard +
Soft ++
Brittle +
Tough +
Fibrous ++
Temperature-sensitive +
Moist -
Foodstuffs, cereals, plants, textiles, wood, chemicals, plastics, animal feed, coal, soils
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Main advantages over the competition
Motor speed 6,000 – 20,000 rpm, constant torque
Digital Display for rated speed
Soft-touch keyboard
Microprocessor controlled
TÜV - Safety
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Action between two Crushing Tools
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.
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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
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Action between two Crushing Tools
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.
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Cutting Mills
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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 - -
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Main advantages over the competition
Fast locking lidEasy access and very easy cleaningRotorsLess sample depositVery stable and robustCutting geometryBearingsSample exhausterMotors Sieves cassettesTÜV - Safety
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Cutting Mill „pulverisette 15“
Operating principle Cutting
Max. feed size 60 mm
Max. capacity 50 l/h
Final fineness 0.25-6 mm
Hard (abrasive) -
Medium-hard -
Soft ++
Brittle +
Tough +
Fibrous ++
Temperature-sensitive +
Moist -
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NEW - pulverisette 15 -
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
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Main advantages over the competition
Double bearings
Easy Cleaning
Cooling
Dust exhaust
Fast grinding
TÜV - Safety
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Cross Beater Mill „pulverisette 16“
Operating principle Impact
Max. feed size 20 mm
Max. capacity 80 l/h
Final fineness 0.12-10 mm
Hard (abrasive) -
Medium-hard ++
Soft +
Brittle ++
Tough -
Fibrous +
Temperature-sensitive -
Moist -
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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
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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
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Particle size
Particle features (measurable particle properties)
1. Geometrical features2. Mass3. Sinking speed4. Field disturbances
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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
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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
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FRITSCHSIEVE SHAKERS
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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
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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
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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
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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
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Particle Size AnalysisLaser-Particle-Sizer „analysette 22“
COMPACT
NanoTec MicroTec
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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
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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)
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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
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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
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Conventional Design
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FRITSCH Design „analysette 22“
convergent laser beam (patent)distance measuring cell - sensorfocal length of fourier lens
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Particle Size Analysis Laser-Light-Scattering
Abbe - Porter Experiment
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Diffraction Pattern
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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
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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
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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
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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
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Main Advantage of Rotary Cone Sample Divider
Rotation of Cone:
spreading sampleover 360°
splitting sample intovery small volumeelements
feeding samplesimultaneously to thesample containers
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Importance of sample dividing
Rotary Cone Sample Divider
Without sample dividing = Not representative
Normal Sample Divider
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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.
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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).
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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
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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.
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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
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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.