FRITSCH GMBH Manufacturers of Laboratory Instruments Industriestrasse 8 D - 55743 Idar-Oberstein GERMANY
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Sample Processing and Analysis in the Laboratory Wolfgang Simon Applications Manager FRITSCH GMBH Manufacturers of Laboratory Instruments Industriestrasse 8 D - 55743 Idar-Oberstein GERMANY http://www.fritsch.de [email protected] Contents Sample processing Task Comminution physics Comminution instruments Particle size analysis Task Physics, Mathematics Instruments Dividing Laboratory instruments from the experts with a worldwide reputation Your partner for 80 years in the processing laboratory Introduction Laboratory analysis Sample preparation Sample processing to provide exact, reliable and reproducible samples for accurate functioning of the analytical instruments no poorly prepared samples great risk of errors correct 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 characterisation TOC instruments in environmental analysis XRF instruments in trace analysis extend of comminution homogeneity of mixtures suitability for printing of dyes taste gelation period drying behaviour Main Criteria for the Selection of a Laboratory Grinder 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 Classification of comminuted products by size Fineness Definition Term Upper particle size Crushing > 5 mm Grinding < 5 mm Fine grinding < 100 µm Micro-fine grinding < 10 µm Ultra-fine grinding < 1 µm Mohs-Hardness Mohs‘ Material hard- ness 1 Talcum, graphite, kaolinite 1.5 Soda, clay, kieselguhr 2 Gypsum, bitumen, kaolin, sulphur, rock salt, potash, bicarbonate of soda, nitre 2.5 Silver Soft 3 Calcite, anthracite, barytes, asbestos 3.5 Dolomite, copper ore 4 Fluorite, zinc blend 4.5 Siderite, magnesite Medium 5 Apatite 5.5 Gehlenite 6 Felspar, iron, hornblende Hard 6.5 Pyrites, iron ore 7 Quartz, flint 8 Topaz 9 Corundum Hard 9.5 Fused corundum, silicon carbide 10 Diamond Material Properties εB EBv Energy expended until failure E = σ (ε)dε σ Stress BV ∫ 0 ε Strain brittle (rocks) low fracture work low comminution energy elastic (steel) high fracture work high comminution energy plastic (rubber) high fracture work low comminution energy visco-elastic high fracture work (thermoplastics) low comminution energy Material Classification Hard/Tough: most ferro alloys (ferro manganese, ferro vanadium, 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, pharmaceutical powders, detergents, pigments, foodstuff Soft/Elastic: plastics, rubber, textiles, dry plants, cereals, cellulose, waste Comminution Principles according to Rumpf pressure friction percussion cutting 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” Operating Percussion principle Max. feed size 5 mm Max. capacity 10 ml Final fineness 5-10 µm Hard (abrasive) + Medium-hard ++ Soft + Brittle ++ Tough - Fibrous + Temperature- ++ sensitive Moist ++ Analytical chemistry (spectral and XRF-analysis), electron microscopy, nuclear research, mineralogy, microbiology Main advantages over the competition Ergonomic design Frequency controlled amplitude Digital timer and amplitude settings Low power consumption Grinding Head included Cryogenic milling Grinding head included TÜV-Safety Action between two Crushing Tools Pressure Action (i.e. Jaw Crusher) Mining and metallurgy: Niobium- titanium, ferrovanadium, chrome vanadium, tungsten carbide, ores, coal, slag, coke Chemicals: wide variety of various raw materials in the chemical industry Geology and mineralogy: Rocks, granite, basalt, barite, silicates Glass industry: Frits, glass, raw materials Ceramics: Steatite, fire-clay, sintered ceramics, electroporcelain Construction materials: Bauxite, clinker, quartz, concrete Jaw Crusher “pulverisette 1” Operating principle Pressure Max. feed size 95 x 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 Main advantages over the competition Closed grinding chamber Cast-iron housing Gap setting Smooth crushing plates Easy Cleaning Longer use Conversion kit 1,1/2,2kW - motors TÜV-Safety Large mouth opening Crushing ratio 1:100 Action between two Crushing Tools Combined Friction and Pressure Action (i.e. Mortar Grinder) Mining and metallurgy: Ores, coal, coke, ashes, slags Chemistry: Fertilisers, dyes, pesticides, salts, detergents, synthetic resins, paints Geology and mineralogy: Minerals (up to and including a Moh’s hardness of 9), calcite’s, quartz, silicates Glass: Sand, frits, glass, raw materials Ceramics: Porcelain, fire-clay, sintered ceramics, clay Agriculture: Soil samples, fertilisers, organic plant materials Foodstuffs: Confectionery, gelatine, spices, yeast, pasta, sugar Metallurgy: Bauxite, slags, additives Pharmacy: Dragees, drugs, tablets, pastes raw materials Rocks and soils: Gypsum, lime, clinker, sand, cement Electrical 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 Action between two Crushing Tools Combined Pressure and Shearing Action (i.e. Disk Mill) Mining and steel industries: Ores, coal, coke, slags Ceramics: Steatite, sintered ceramics, electrotechnical porcelain, fire-proof clay Rocks and soils: Bauxite, slags, quartz, clinker, gypsum, chalk Glass: Frits, glass types, raw materials Soil research: Dried soil samples, sewage sludge, hydrological sediments, drilling cores, Briquettes, Coke, Limestone, Thomas meal (potash), Pumice stone 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 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, construction materials, soil research Main advantages over the competition Design and construction TÜV - 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 “pulverisette 1” in combination with “pulverisette 13” Fine grinding from 95 mm to 0.1 mm in one working step Mounting 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. Action between two Crushing Tools Combined Percussion and Friction Action (i.e. Vibrating Cup Mill) Mining: for processing of coal, ores or minerals for physical or chemical analysis Metallurgy: for grinding blast furnace slag or cast iron samples to determine additives needed Ceramic industry: for grinding rock samples to produce raw powder to determine CaO3 and MgCO 3 content or clinkers to study the constancy of the mineralogical structure Agriculture and ecology: for preparing samples for chemical analysis of soils, sludges or vegetable matter Infrared and X-ray fluorescence analysis: for preparing 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 mm Max. capacity 250 ml Final fineness 10-20µm Hard (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