plugin-workshop fritsch 2011 part1

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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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    Agenda

    Presentation of the companySampling & sample division

    Premium line a new reference class

    Sample preparation

    Task

    Physics of comminutionComminution instruments

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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    Criteria for selection of a laboratory mill

    Costs

    Instrument costsAccessories

    Personnel costs

    Operating costs

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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    Comminution principles according to Rumpf

    F = Force, v = Speed

    Pressure Friction Impact

    Collision, pounding

    Cutting Shearing

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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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 GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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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    FRITSCH GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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 GMBH Milling and Sizing Idar-Oberstein Germany 2011

    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