plugin-workshop fritsch 2011 part1
TRANSCRIPT
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FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011
Sample Preparation in the Laboratory
FRITSCH GMBH
Milling & Sizing
Dagmar Klein
Sales Manager
Industriestr. 8
55743 Idar-Oberstein
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Agenda
Presentation of the companySampling & sample division
Premium line a new reference class
Sample preparation
Task
Physics of comminutionComminution instruments
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Laboratory mills from the World Market Leader
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FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011
Your Partner with more than 80 years ofexperience
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SAMPLE PREPARATION AND PARTICLE SIZING Products and brand name
Instruments from FRITSCH are known around the world under thebrand names
PULVERISETTE
ANALYSETTE
LABORETTE
Instruments for comminution
Instruments for particle sizingInstruments for dividing and feeding
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Sample Preparation
exact, reliable and reproducible samples
better, accurate performance from analytical instruments
no poorly prepared samples
great risk of errors
proper selection of grinding technique and instrument
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Errors in sample preparation
Contamination
Material loss (recovery) and demixingChanges to the compositions (decay) & and the matrixthrough thermal and physical forces
Active ingredient analysis in the pharmaceutical industry
Quality parameters of polymers (colour, moisture, clusterdestruction)
SiC preparation (decay)
Samples surface
e.g. X-ray analysis (mineralogical effect - particle size effect)
Rheology of polymer powders such as pourability
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Sampling and sample division
The full initial quantity of a substance to be analysed, for instance todetermine its chemical composition, is generally significantly larger than the
quantity that can be analysed. This makes sampling, sample division andpreparation of the sample necessary.
The result of an analytical process can only supply meaningful information ifthe analysed sample is representative of the material investigated.
Initial quantity desired Q(x)
Sampling (laboratory sample) ?
Sample division analysis Q*(x)
Systematic, random and statistical errors can lead to deviations between
Q(x) and Q*(x).
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Theoretical aspects of sample preparation
The core problem of samplingand sample preparation is the
inhomogeneity of the samplesExtremely pronounced in solidmaterials, but flowing gases andliquids are also inhomogeneous.
Additional inhomogeneity ispossible over time (e.g. demixingduring sample preparation)
The max. achievable
homogeneity during samplepreparation is uniform, randommixing - true mixed state !!!!!!
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Main Criteria for the selection of a LaboratoryGrinder
Type of material
Physical and chemical properties
Initial sample characteristics
Feed size (pre-crushing required?)
Quantity, Number of samples
Milling time, Cleaning
Representative sample Universal applicability
Final sample characteristics
Contamination, Abrasion
Final particle size, Particle size range
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Criteria for selection of a laboratory mill
Additional usage options
Wet grinding possible?
Cryogenic grinding required?
E.g. plastics
Grinding under inert gas required?
CleaningSample carry-over
Duration
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Criteria for selection of a laboratory mill
Costs
Instrument costsAccessories
Personnel costs
Operating costs
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Material properties / Mohs hardness
Hard
Medium-hard
Soft
Mohs
hard-
ness
Material
1 Talcum, graphite, kaolin
1.5 Soda, clay, diatom earth
2 Gypsum, bitumen, kaolin, sulphur, rock salt, bicarbonate
2.5 Silver
3 Calcite, anthracite
3.5 Dolomite, copper ore4 Fluorite, zinc blende
4.5 Siderite, magnesite
5 Apatite
5.5
6 Feldspar, iron
6.5 Pyrite, iron ore
7 Quartz
8 Topaz
9 Corundum
9.5 Silicon carbide
10 Diamond
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Material Properties
brittle (rocks) low fracture work
low comminution energy elastic (steel) high fracture work
high comminution energy
plastic (rubber) high fracture worklow comminution energy
visco-elastic high fracture work
(thermoplastics) low comminution energy
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Material properties Facture toughness at room temperature
Ceramics Metals Polymers Composite materials
GFRP
Wood
Reinforcedconcrete
Polyethylene
PMMA
Polyester
Epoxy
Steels
Al alloys
Pb, Ag, Cu
Al2O3
SiC
Window glass
Concrete
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Material Classification
Hard/Tough: most ferro alloys (ferro manganese, ferro vanadium, etc.), hardmetaltungsten 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, drages/tablets, feed pellets, bakelite, gypsum, soils,demolition waste (rubble)
Soft/Brittle: inorganic salts, epoxy resins, pharmaceutical powders, detergents,pigments, foodstuff
Soft/Elastic: plastics, rubber, textiles, dry plants, cereals, cellulose, waste
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Fineness Definition
T e r m U p p e r p a r t ic le s iz e
C ru s h in g > 5 m m
G r in d in g < 5 m m
F in e g r in d in g < 1 0 0 m
M ic ro - f in e g r in d in g < 1 0 m
U lt r a - f in e g r in d in g < 1 m
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Comminution principles according to Rumpf
F = Force, v = Speed
Pressure Friction Impact
Collision, pounding
Cutting Shearing
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Sample preparation application example- Hard, brittle materials - (concrete)
The standard for pre-crushing
Jaw Crusher
Larger sample quantities should be used for an averaged sample, and the first
stage can only be accomplished with a hammer or Jaw Crusher
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Action between two Crushing Tools
Pressure Action (i.e. Jaw Crusher)
Mining and metallurgy: Niobium-titanium,ferrovanadium, chrome vanadium, tungstencarbide, ores, coal, slag, cokeChemicals: wide variety of various raw
materials in the chemical industryGeology and mineralogy: Rocks, granite,basalt, barite, silicatesGlass industry: Frits, glass, raw materialsCeramics: Steatite, fire-clay, sinteredceramics, electroporcelainConstruction materials: Bauxite, clinker,quartz, concrete
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Jaw Crusher PULVERISETTE 1
Operating principle Pressure
Max. feed size 95 mm
Max. capacity 200 kg/h
Final fineness 1-15 mm
Hard (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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FRITSCH - features
Closed grinding chamber
Cast-iron housing Gap setting
Smooth crushing plates
Easy cleaningLonger use
Conversion kit
11 / 22kW - motors TV-Safety
Large mouth opening
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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, sewagesludge, hydrological sediments, drillingcores, briquettes, coke, limestone, Thomas
meal (potash), pumice stone
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Laboratory Disk Mill PULVERISETTE 13
Operating principle Shearing,
pressureMax. feed size 20 mm
Max. capacity 150 kg
Final fineness 0.1-12 mm
Hard (abrasive) +
Medium-hard ++
Soft +Brittle ++
Tough -
Fibrous +
Temperature-sensitive -
Moist -
Mining, iron and steel industry, ceramics + glass, construction
materials, soil research
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FRITSCH - features
Design and construction
TV - Safety Dust tight, connection to dust exhaust
Compact, small instrument
Maintenance-free motor
Reproducible gap setting (steps of 0.1 mm)
Easy access for cleaning
Grinding disks WC+Co, ZrO2
Combination possibility with p-1