HANDBOOK TIME LINE READ THE SPEX 1956-1983 SPEAKER ONLINE! Visit www.spexspeaker.com to read our unique trade journal that was published between 1956-1983.

1980s

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2014

2 SPEX SamplePrep, LLC has been providing superior sample preparation equipment and supplies since 1954. Our mission is to provide quality products backed by exceptional service and expertise. Our equipment is used to prepare samples for a wide range of analytical technologies including XRF, ICP, GC-MS and PCR. Much of our equipment is also used for cutting-edge research in pharmaceuticals, superconductors, polymers, forensics, genetics and biotechnology.

Our Products • Freezer/Mill® – Uniquely designed to • Katanax® Electric Fusion Fluxers – cryogenically grind samples normally Automated electric fluxers for borate fusions considered difficult or impossible to pulverize of cement, ores, ceramics and other materials at ambient temperature. for analysis by XRF, AA, ICP and wet chemistry. • Geno/Grinder® – Used for high-throughput • X-Press® – Laboratory press ideal for cell disruption and tissue homogenization. pressing sample disks for XRF, IR, and OES. • Mixer/Mill® – High-energy ball mills for • XRF Accessories – Spec-Caps® for supporting pulverizing brittle materials, mixing powders pressed disks, disposable X-Cells® and window and emulsions, mechanical alloying, and film for liquid samples, Prep-Aid® Binders and nanomilling. Grinding Aids. • Shatterbox® – Ring and puck mills used for • ShaQer - Specifically designed for preparation rapidly pulverizing brittle materials such as of samples using the QuEChERS method. cement, slag, ores, ceramics, etc.

Our Customers For the past six decades, SPEX SamplePrep’s customers have relied on our unique knowledge and expertise to select the proper products for their sample preparation needs. Our exceptional sales and service teams recommend and support reliable sample preparation equipment for the following fields: • Cement Manufacturing • Medicine and Genetics • Cosmetics • Mining • Pharmaceuticals and • Food and Agriculture\ • Geology and Mineralogy Drug Testing • Forensics and Crime Scene • Polymers • Environmental Protection Investigation • RoHS/WEEE and Remediation

3 TABLE OF CONTENTS INTRODUCTION Time line of SPEX SamplePrep's Handbook...... 2 Company Profile ...... 3 Contributing Editors ...... 6 Sample Preparation Techniques ...... 7

PRODUCTS AND ACCESSORIES Geno/Grinder®...... 8 2010 Geno/Grinder Features & Specifications...... 9 1600 MiniG Features & Specifications...... 10 2020 Geno/Grinder Features & Specifications...... 11 Geno/Grinder & MiniG Accessories...... 12 Technical Information ...... 19 Before & After Samples ...... 20 Application Notes ...... 21 ShaQerTM ...... 24 Features & Specifications ...... 25 ShaQer Accessories...... 25 Freezer/Mill®...... 26 6770 Freezer/Mill Features & Specifications...... 27 6870 Freezer/Mill Features & Specifications...... 28 6870D Freezer/Mill Features & Specifications...... 29 6970EFM Freezer/Mill Features & Specifications...... 30 Freezer/Mill Accessories...... 31 Before & After Samples ...... 35 Technical Information ...... 36 Application Notes ...... 40

Mixer/Mill®...... 42 8000M Mixer/Mill Features & Specifications...... 43 8000D Mixer/Mill Features & Specifications...... 44 5100 Mixer/Mill Features & Specifications...... 45 Mixer/Mill Accessories...... 46 Technical Information ...... 50 Before & After Samples ...... 52 Grinding Tests ...... 53 Grinding Container Materials ...... 54 Application Notes ...... 55 Shatterbox®...... 56 8530 Shatterbox Features & Specifications...... 57 8500 Shatterbox Features & Specifications...... 58 Shatterbox Accessories...... 59 4 Before & After Samples...... 61 Grinding Tests ...... 60 Technical Information ...... 62 X-Press®...... 64 3636 X-Press Features & Specifications...... 65 Carver Manual Presses ...... 66 X-Press Accessories...... 67 Technical Information ...... 69 Katanax® Fusion Fluxers...... 78 K1 Prime Features & Specifications...... 79 K2 Prime Features & Specifications...... 80 Katanax Accessories...... 81 Application note...... 85 Technical Information ...... 86 XRF Accessories...... 90 Spec-Caps...... 90 Prep-Aid Binders...... 91 X-Cells...... 91 Thin Film...... 92 Technical Information ...... 94 Technical Information Key Points about Grinding ...... 102 Cleaning Containers ...... 104 Respiratory Protection...... 104 When to Pulverize...... 105 Appendix Trademark References ...... 107 Sample Grind Request Form...... 108 Demo Request Form...... 109

Ordering Information ...... 110

Index Subject Index ...... 112 Product Index ...... 116

5 12TH EDITION CONTRIBUTING EDITORS

Ralph H. Obenauf, Ph.D. Richard Bostwick Tim Osborn-Jones Francine Henry Pierre-Emmanuel LeMay, Eng. Lea Anderson-Smith, Ph.D. Stephan Siniscalco John Martin Keith Tucker Grahame Mowatt Sarah Geiger Sandy Mangan Paul Lynch Dave Speake Mark Tutty Eric Smith

HEADQUARTERS SPEX SamplePrep, LLC 65 Liberty St., Metuchen, NJ 08840 Phone: (732) 623-0465 Fax: (732) 906-2492 Email: [email protected] Web: www.spexsampleprep.com

EUROPEAN DIVISION SPEX Certiprep Ltd., 2 Dalston Gardens Stanmore, Middlesex HA7 1BQ United Kingdom Phone: +44 (0) 208 204 6656 Fax: +44 (0) 208 204 6654 Email: [email protected]

KATANAX 2022 RUE LAVOISIER #100 QUEBEC, QC, CANADA, G1N 4L5 Phone: +1-418-657-6201 Fax: +1-418-657-6203 Email: [email protected] www.katanax.com

6 SAMPLE PREPARATION TECHNIQUES Sample preparation techniques are the building blocks used to prepare samples for specific scientific analyses. They are the foundation for ensuring high quality and reliable analytical results. Our equipment and accessories are used for a variety of common techniques as well as specialities, such as cryogenic grinding. Listed below are the symbols for each technique and some insight into the use of our equipment.

Grinding & Pulverizing Our laboratory mills and grinders are capable of pulverizing samples in both ambient and cryogenic environments. This versatility allows for grinding of a wide variety of samples, including metals, rocks, plastics, plant and animal tissue, bone and pharmaceuticals.

Mixing & Blending The non-homogeneity of materials in the real world presents a serious sampling problem for scientists. Our mills are effective at mixing and blending dry materials such as pigments, powders, pharmaceuticals and cosmetics as well as samples that require mixing for effective extraction with a solvent or buffer.

Tissue Homogenization /Cell Lysis Effective cell disruption and DNA/RNA extraction are critical for biotechnology and forensic applications. Our Geno/Grinders and Freezer/Mills aid scientists by providing high-throughput sample preparation solutions at both ambient and cryogenic temperatures.

Pressing & Pelletizing Analytical spectroscopic methods such as XRF, OES, and IR often require samples in the form of a round, flat-surfaced disc. Our laboratory presses are ideal for preparing sample discs for these methods. In addition, our automatic and air- actuated presses are designed to fit on the bench top, requiring less space than standard floor model presses.

Borate Fusion For samples that are difficult to prepare as homogeneous pressed powders (cement), difficult to dissolve in acid (zirconia and alumina), or both (metal ores and silicate rocks), borate fusions are widely used. SPEX SamplePrep offers the full line of Katanax Electric Fusion Fluxers & Fusion Fluxes for preparation of samples for XRF, AA, and ICP.

7 Mixing & Blending Grinding & Pulverizing

Tissue Homogenization & Cell Lysis

• 2010 Geno/Grinder® • 1600 MiniGTM • 2020 Geno/Grinder®

THE GENO/GRINDER® Our Geno/Grinders are versatile, high-throughput homogenizers and cell lysers. They were designed with a unique, vigorous, vertical pulverizing motion and an adjustable clamp that handles various sizes of titer plates and vials. Sample preparation is usually complete in two minutes or less. The 2010 Geno/Grinder® is a homogenizer ideal for labs that need high- throughput of samples. The 1600 MiniGTM is a smaller homogenizer useful for labs that process fewer samples. The 2020 Geno/Grinder® is an automated homogenizer that integrates with most automated robotic systems and platforms. APPLICATIONS SAMPLE TYPES • Tissue • Cell lysis Homogenization • Animal tissue • Seeds • QuEChERS Plant tissue Yeast • Pesticide residue • • • Protein extraction • Vegetables • Cereal extraction • Biofuels • DNA/RNA • Fruit • Beans extraction • Bacteria • Cell Cultures

TRY IT BEFORE YOU BUY IT! Demo and Sample Test Programs are available for this product. See pages 108-109 for more details

8 GENO/GRINDER® Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 9 2010-230 sampleprep For video, scan with video, For your smartyour phone or visit www.youtube.com/ 1/3 hp in minutes: Digital display (max 20:00) seconds 1.25in (3.2cm) vertical 1750 500 to from Adjustable strokes/minute Part number: 2010-115 number: Part 5 4 6 3 LCD screen displays run times in minutes: times in minutes: run displays screen LCD format. seconds adjust to you allow and timer controls Rate speed and set the time. start to you Start allow buttons and stop the grinding process. and stop

Motor Motor Timer/Controls Clamp Movement Clamp Speed 4. 5. 6. 2 1 Yes 15.00 in (38.1 cm) wide x 20.49 in. (52 cm) deep x 25.25 in.(64.1 cm) high 87 lbs (39.5kg) 50 Hz. 230V, for cord European 60Hz. 2-prong plug 115V, grounded 3-prong 115V/60Hz or 230V/50Hz Clamp has quick-release button to adjust for adjust for to button has quick-release Clamp plates. of vials or titer load any Lid has a safety interlock switch that stops stops that switch Lid has a safety interlock during the if the lid is opened the motor grinding process. Window in lid allows you to see the grinding to you in lid allows Window process.

CE Approved Dimensions (lbs) Weight Cord Power Voltage Features & Specifications The 2010 Geno/Grinder is a high-throughput plant & tissue homogenizer with an adjustable clamp & tissue homogenizer plant 2010 Geno/Grinder is a high-throughput The rapid Specificallyfor designed tubes. or 16 centrifuge plates six titer up to accommodates that preserve to available are Kryotech® accessories lysis and tissue homogenization. disruption, cell process. samples during the grinding sensitive temperature 3. 2. 1. Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX GENO/GRINDER® 10 4. 3. 2. 1. pesticide residue analysis. created for applications requiring samplepreparation for DNA/RNAandprotein aswell as extractions The isidealfor 1600MiniG labsthat want yet tissuehomogenizer acompact powerful Features &Specifications Motor Weight Dimensions CE Approved Voltage

2 double load. x 2mLvials, butallows stacking to hold a holdsonetiter plateClamp typically or24 during theshaking process. Easy-to-use clampkeeps samplessecure grinding process. the motor ifthelidisopenedduring interlockLid hasasafety switch that stops process. Window inlidallows you to seethegrinding 1/7 HP. 40lbs. (22kg) (43.2 cm)deep in. (28.6cm)widex17.0 21.5 in.(54.6cm)highx11.25 Yes 115V/60Hz or230V/50Hz 115V/60Hz 1 Timer/Controls Clamp Speed Clamp Clamp MovementClamp Power Cord 6. 5. 7.

speed andsettime. Rate andtimercontrols allow you to adjust in minute:second format. LCD display screen shows run times stop thegrindingprocess. andstop buttons allowStart and you to start 3 4 5 7 6 seconds (max10:00) displayDigital inminutes: strokes/minute Adjustable from 500to 1500 1.25 in.(3.2cm)vertical 230V, 50Hz. 2-prong60Hz. European cord for 3-prong grounded plug115V, Part number:1600 MiniG visit www.youtube.com/ your smart phoneor your smart For video, with scan sampleprep . Ithasbeen 16 00 ™ GENO/GRINDER® Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 11 2020-115 2020-230 sampleprep For video, scan with video, For your smartyour phone or visit www.youtube.com/ 3-phase servo motors plug 115V, grounded 3-prong cord European 60Hz. 2-prong 50 Hz. 230V, for 1.25 inches per minute 500-1750 strokes 4 Part number: number: Part Accommodates all standard titer plates plates titer all standard Accommodates and vials. Unique vertical grinding motion that samples. processes consistently

3. 4. Motor Motor Cord Power Clamp Movement Clamp Speed 3 2 1 115V / 230 V 115V / 230 Yes 12.88 in. x 18.88 in. x 35.88 in. 129 lbs (58.51 kg) Clamp is automatically secured before the before secured is automatically Clamp grinding process. Door automatically closes when cycleDoor automatically begins and opens when cycle ends.

Voltage CE Approved Dimensions Weight Features & Specifications 2020 Geno/Grinder is an automated plant and tissue homogenizer that integrates with most integrates that homogenizer and tissue plant 2020 Geno/Grinder is an automated The tissue for & animal plant Its vertical grinding motion prepares and platforms. systems robotic or less. minutes in two extractions or proteins of DNA, RNA 2. 1. Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX GENO/GRINDER® ACCESSORIES 12 GENO/GRINDER order. Can and1600MiniG beusedinthe2010Geno/Grinder® bediscardedgrinding ballscan orcleanedfor re-use. Visit ourwebsite for more information andto determined basedonthesamplematerial andthesize ofthegrindingvialortiter plate. After use, the Stainless steel ballsare usefulfor grindinglarge ortough samples. The choice ofballsize shouldbe Grinding Media Grinding Plates & TraysPlates and onebottom plate. with two nestingmid-plates adjustable clamp. comes Set plates inthe2189 vertically Nesting trays usedto stacktiter 2189T sets (2240-PC2240-PE) (2230) 24-well titer plates andvial 24-pin magnet. Drops ballsinto grinding balls(2155)from (2110M) Separates 3/8in.(9.5mm)steel Magnet 2110S 2100 (2200 and2210titer plates.) standard 96-well titer plate, ball (2150)into eachwell ofa 5/32 in.(4mm)steel grinding dispensesone Simultaneously Dispenser 2110M 2110S separator. plates &vialsets. Used with balls (2155)from 24-well titer 3/8 in.(9.5mm)steel grinding with handle. Inserts/removes 24 magnet-tippedpinsonplate Geno/Grinders withfixed-heightGeno/Grinders clamps. threaded rod. The 2189Adjustable Clampberetrofitted can to older2010 hand-knob with a quick-release button to move it up or down a central titer plates, tubesandvialsofequalorlesserheight. The clamphasa Clamp. Itholdsupto three layers titer ofdeep-well plates andother The isnow 2010Geno/Grinder suppliedwiththe2189Adjustable 2189 GrindingBall Adjustablefor Clamp 2010Geno/Grinder® Nesting TraySet Separator for 24-Pin 24-PinMagnet ® & M & ini G TM ACCESSORIES TM . adjustable clamp. plates inthe1690 vertically Nesting trays usedto stacktiter 1690T 2150 plates. inbagsof5,000. Sold andall96-wellDispenser titer Used Ball with2100Grinding Made of440Cstainlesssteel. 5/32 in.(4mm) 2156 Vial inbagsof100. Sets. Sold in 2230titer plates and2250 grinding large ortough samples Made of440Cstainlesssteel. For in. (11mm) 2155 Sold inbagsof100. Sold 2241-PC and2241-PEFvials. 2190 Vial with3116PC, Rack For usein2230titer plate orin Made of440Cstainlesssteel. (9.5 mm) Nesting Tray for MiniG GrindingBalls, GrindingBalls, 7/16 GrindingBalls, 3/8in.

Click for video! GENO/GRINDER® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 13

Low Binding Binding Low Zirconium Grinding Silica Grinding Resin Low Binding Silica Low Silica Grinding Beads, Zirconium Beads, 200 µm Zirconium Beads, and chemically washed Acid samples from keep to treated 250 wells. plate titer binding to bottle. gram 2182 2170 2180 100-400 µm silica irregular washed Acid bottle. gram 200 resin. Molecular Biology Beads, 200-400 µm Grade, RNase/DNase-free washed Acid 250 beads. zirconium treated bottle. gram Beads, 400 µm Beads, and chemically washed Acid samples from keep to treated 200 wells. plate titer binding to bottle. gram 2167 400-600 µm 200 silica beads, washed Acid bottle. gram 2165 Low Binding Binding Low Silica Grinding Beads, Silica Grinding Resin, Low Binding Silica Binding Low Low Binding Silica Low Molecular Biology Grade, Molecular Biology Grade, 100-400µm RNase/DNase-free washed Acid 200 silica resin. irregular treated bottle. gram Beads, 100 µm Beads, and chemically washed Acid samples from keep to treated 200 wells, plate titer binding to bottle. gram 2181 2171 2168 Zirconium Beads, 100 µm Zirconium Beads, and chemically washed Acid samples from keep to treated 250 wells. plate titer binding to bottle. gram 2166 Molecular Biology Grade, Molecular Biology Grade, 400-600 µm RNase/DNase-free washed Acid 200 gram silica beads. treated bottle. Beads, 800 µm Beads, and chemically washed Acid samples from keep to treated 200 wells. plate titer binding to bottle. gram 2162 . Contact us for detailed instructions. detailed us for . Contact TM Molecular Biology Grade Grinding Beads are treated to inactivate contaminating enzymes and have enzymeshave and contaminating inactivate to Molecular treated Grinding Biology BeadsGrade are of binding non-specific reduce to coated BindingGrinding Beads are Low accordingly. been tested Grinding Beads Washed Acid samples of cells. dilute lysing used for are and acids and proteins nucleic 2010 Can be used in the Geno/Grinder®and fine particlescontaminants. and remove to treated are 1600 MiniG Grinding Beads Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX GENO/GRINDER® ACCESSORIES 14 well-to-well contamination. Rugged, silicone rubber Cap-Mats may besterilized andre-used. alphanumeric marksfor well identification. whenusedwith2600Cryo-Station. RNA extraction Titer plates are madeofpolypropylene, with automatedto-daughter plate pipetting, large sample dilutions and cell suspensions. for Suitable at highclampspeeds. They beusedfor can many applications includingsamplelibraries, mother- been tested extensively withvarious samplesandresist by steel perforation grindingballseven While most titer plates be used can in the Geno/Grinder, sturdy we titer plates carry that have Titer Plates andCap-mats analyte into thesolvent. Typically, are usedpersamplevial. 2cylinders to shearthesamplematrix duringprocessing,help thecylinders resulting of inathorough extraction ofoilresidues from andextraction methods suchasQuEChERS fishandseafood. ends The angle-cut andare are usefulwhenmixingsamplesfor extraction ceramic inert chemically Our cylinders CylindersGrinding 2183 of 100. centrifuge tubes. inbags Sold for usewithstandard 50mL ends withangle-cut cylinder Large size ceramic grinding Cylinder, 3/8in.x7/8 or assingleCap-Mat (2201). of100titer asacase platesSold working of2.0mL. capacity Square 2.4mL wells witha Plate, WellsSquare (2200). inpacksof100orsingle Sold marks for well identification. polypropylene, alphanumeric Round 1.0mLwells, rugged Plate,Round Wells 2210–100 2200–100 titer plates orsingle (2220). of100 ascase balls (2150).Sold well. Use withsteel grinding working of2mLper capacity 5mLwells witha Rectangular Plate for 2221Cap-Mat 2220–100 Ceramic Grinding 2185 5 or15mLcentrifuge tubes. inbags of100. Sold endsfor usewithstandard sizeSmall withangle-cut ceramic grindingcylinder 96-Well Titer 96-Well Titer 48-Well Titer Ceramic GrindingCylinder, 5/32in.x5/16 Cap-Mats sealtiter plate wells, preventing spillsand 10 Cap-Mats orsingle(2201). Plates, above. inpacksof Sold matsSealing for the2200 Titer Titer Plates. 2201–10 10 orsingle(2211). contamination. inpacksof Sold prevents leaksandcross-well Plates. Tough silicone rubber, matsSealing for 2210 Titer Titer Plate 2211–10 Cap-Mats orsingle(2221). Titer Plates. of10 ascase Sold Cap-Mats seal222048-Well Titer Plate 2221–10 2184 of 100. centrifuge tubes. inbags Sold for usewithstandard 15mL ends withangle-cut cylinder Medium size ceramic grinding Cylinder, 5/16in.x5/8 Ceramic Grinding Cap-Mats for 2200 Cap-Mats Cap-Mat for 2210 Cap-Mat Cap-Mat for 2220 Cap-Mat GENO/GRINDER® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 15 Frosted Frosted Polycarbonate Polycarbonate Cap-Mat 2230 for Pre-Cleaned Polycarbonate Vial, Vial, Polycarbonate 2231–10 Titer Plate Titer 2230 24-Well seal Cap-Mats Sold as case of 10 Plates. Titer (2231). or single Cap-Mats 2241–PEF-200 2251PC Polyethylene Vial 5 mL Vial Polyethylene x 2 in. long 1/2 in. diameter (12.7 mm x 50.8 mm). Grinding load per vial 1.5 mL. Sold in units of 200, 100 (2241-PEF- 100) or 1000 (2241-PEF-1000). 15 mL, Short vial with screw-on Polycarbonate x 1 2/3 in. 1 1/8 in. diameter cap, long (2.9 cm x 4.2 cm). Pre- cleaned with grinding load per vial 6 mL. 2253-PC-48 2240–PEF Vial, 50 mL Vial, vial with screw- Polycarbonate x 4 ½ 1 1/8 in. diameter on cap, in. (2.9 cm x 11.4 cm). Grinding load per vial 20 mL. Sold as a with 48 caps Vials pack of 48 (2253C-48). Frosted Polyethylene Vial Set, Set, Vial Polyethylene Frosted 5 mL each with one 3/8 Set of 24 vials, grinding ball in. (9.5 mm) steel (2155). Grinding load per vial 1.5 mL. Sold as case of 10. Polycarbonate Polycarbonate 24-Well Titer Titer Plate 24-Well Polycarbonate Polycarbonate Polycarbonate Vial Vial Polycarbonate mL Pre-Cleaned Polycarbonate Vial Vial Set, Polycarbonate 15 mL set includes 5 pre-cleanedEach 2251PC vials pre-loaded with a grinding 7/16 in. (11 mm) steel ball (2156), and caps (2250C). Grinding load per vial 6 mL. 2250 2241–PC vial with screw- Polycarbonate 1/2 in. cap. on polyethylene x 2 in. long (12.7 mm x diameter 50.8 mm). Grinding load per vial 1.5 mL. Sold in units of 240. Vial, 5 Vial, Vial, 15 mL, Tall 15 mL, Vial, vial with screw-on Polycarbonate x 4¾ in. 5/8 in. diameter cap, 12.1 cm). Grinding (1.6 cm x long. load per vial 6 mL. Sold as a pack of 30 vials. 2252–PC-30 2240–PC 2230–100 2230–100 Square 10 mL wells with a with wells 10 mL Square capacity per well. of 4 mL working one and Cap-Mat, with 2231 Use grinding steel 3/8 in. (9.5 mm) ball (2155). Sold as case of 100 or single (2230). Set, 5 mL Set, set includes 24 pre-cleanedEach each with a 3/8 2241-PC vials, grinding ball in. (9.5mm) steel (2155). Grinding load per vial 1.5 mL. Sold in case of 10. Vial sets are an alternative to titer plates. Vials can be filled and sealed individually, and the larger the larger and can be filled and sealed individually, Vials plates. titer to an alternative sets are Vial canballs purchased be steel and vials Replacement plates. titer than samples canvials bigger hold separately. Vials and Vial Sets Vial and Vials Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX GENO/GRINDER® ACCESSORIES All pre-loaded vialsareAll pre-loaded self-standing to make iteasierto addsamples. biologygrade beads,molecular silica acidwashed orzirconium silica beads, run® can upto vialsatGeno/Grinder 96pre-loaded atime. These vialsare prefilled with your choice of Pre-loaded vials are ideal for fast and simple setup: add samples and you’re ready to go. The 2010 VialsPre-loaded 16 2302–1700AW packs of50. washed zirconium beads. in Sold cap, prefilled with1.7mmacid 2 mLmicrofuge tubewithscrew- Beads Zirconium with 1.7mmAcid Washed 2301–100MB beads. in packsof100. Sold biologygrade molecular silica screw-cap, prefilled with100μm 2 mLmicrofuge tubewith Beads with 100μmSilica packs of100. acid washed beads. silica in Sold screw-cap, prefilled with 800 μm 2 mLmicrofuge tubewith Beads Silica with 800μmAcid Washed 2304–800AW 2302–1000AW packs of100. washed zirconium beads. in Sold cap, prefilled with1.0mmacid 2 mLmicrofuge tubewithscrew- Beads Zirconium with 1.0mmAcid Washed beads. inpacksof100. Sold 1.4 mmacidwashed zirconium cap, prefilled with800μmand 2 mLmicrofuge tubewithscrew- with Mixed Matrix 2 2304–100AW 2303–MM2 packs of100. acid washed beads. silica in Sold screw-cap, prefilled with100μm 2 mLmicrofuge tubewith Beads Silica with 100μmAcid Washed 2mL Tube 2mL Tube 2mL Tube 2 mL Tube2 2 mL Tube 2 2mL Tube in packsof50. stainless steel grindingballs. Sold screw-cap, prefilled with 2.8 mm 2 mLmicrofuge tubewith SteelBalls 2.8 mmStainless 2305-2800SS bead. inpacksof100. Sold and a4mmacidwashed silica beads, 1.4mmzirconium beads cap, prefilled with100μmsilica 2 mLmicrofuge tubewithscrew- with Mixed Matrix 3 2303–MM3 packs of100. acid washed beads. silica in Sold screw-cap, prefilled with400μm 2 mLmicrofuge tubewith Beads Silica with 400μmAcid Washed 2304–400AW 2302–1400AW packs of100. washed zirconium beads. in Sold cap, prefilled with1.4mmacid 2 mLmicrofuge tubewithscrew- Beads Zirconium with 1.4mmAcid Washed Also available as200μm μm acidwashed zirconium beads. cap, prefilled with600mgof100 2 mLmicrofuge tubewithscrew- Beads Zirconium with 100μmAcid Washed 2302–100AW2 200AW) 2302–3000AW packs washed zirconium beads. in Sold cap, prefilled with3mmacid 2 mLmicrofuge tubewithscrew- Beads Zirconium with 3mmAcid Washed silica beadsorsteelsilica balls. of50. Sold inpacksof100. Sold 2mL Tube 2mL Tube with 2 mL Tube 2 2mL Tube 2mL Tube 2 mL Tube2 (2302- GENO/GRINDER® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 17 Holder for 15 mL for Holder Holder 2 mL Foam Holder 50 mL Foam Centrifuge Tubes Centrifuge block holds foam rugged Thick, 15 mL centrifuge 24 standard tubes. MiniG for block holds 24 Rugged foam mL tubes. 2 standard MiniG for block holds six Rugged foam mL tubes. 50 standard 1680 1686 2197 Vial Vial Rack Cryogenic Grinding Vial Pack CryogenicVial Grinding Cryo-Station Holder for 50 for Holder Holds 24 x 3116PC vials, 24 2241-PC vials, or 24 2241-PEF-200 vials. Vials are are Vials vials. or 24 2241-PEF-200 2241-PC vials, 24 vials, 24 x 3116PC Holds 2010 Geno/Grinder the high- for into placed and the vial rack loaded into Sold in pairs. lysis. and cell tissue homogenization throughput 2190 Used to grind tough materials (e.g. bone) at cryogenic temperatures. Package Package cryogenic bone) at temperatures. (e.g. materials grind tough to Used and 2 2 end plugs, sets of cryogenic each with 1 cylinder, includes four vials, clamp and 2260 Cryo- use with 2189 adjustable For carbide balls. tungsten end plug removal. for Block. 6754 or 6756 extractor required A holding station for samples that must be kept chilled to preserve RNA for RNA for preserve chilled to must be kept samples that for A holding station of the Cryo-Station is chilled with liquid jacket outer insulated The extraction. can be plates titer Two or manually. can and be filled automatically nitrogen well hold also can The cold. kept and filled be to Cryo-Stationthe in placed well RNA analysis. for samples cut up sensitive to a chilled cutting board 2255 2600 15 mL Foam Holder Holder 15 mL Foam Holder for 2 mL for Holder mL Tubes Centrifuge block holds foam rugged Thick, 50 mL centrifuge 16 standard tubes. 2196-16-PE for MiniG for block holds 12 Rugged foam 15 mL tubes. standard 1685 Micro-centrifuge Tubes block holds foam rugged Thick, tubes. 48 microfuge 2300 Accessories ® These accessories are used to chill samples to cryogenic temperature and to maintain temperature temperature maintain and to cryogenic chill samples to temperature to used are accessories These such as handling, liquid nitrogen products for during grinding in the Geno/Grinder®. Additional section. and portable can in the Freezer/Mill® be found gloves Dewars, protective Racks and Holders are designed to hold vials securely in place on the 2010 Geno/Grinder on the 2010 during place in securely hold vials to designed Racks are and Holders These transport and to samples and can on the benchtop also be used lightweight are They processing. within the laboratory. Kryo-Tech Racks Holders and Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX GENO/GRINDER® ACCESSORIES Cryo-Blocks 18 a timeto balanceClamps. theloadinGeno/Grinder fitthe2189 Adjustable Clamp. shouldalways2261 and2664Cryo-Blocks two beused Cryo-Blocks at be aware fit the standard that fixed the2650,2660, 2662 and2665 Cryo-Blocks clamp, and the2260, fit the2189 Adjustable Clamp.All Cryo-Blocks However, should Geno/Grinders owners ofolder 2010 2660 2260 2662 in pairs. used in2240-PC Vial Set. Sold twenty-four 2241-PC vials, as Aluminum blockthat holds Polycarbonate Vials 2251PC vials. inpairs. Sold Aluminum blockthat holdssix Polycarbonate Vials inpairs.Sold samples to run simultaneously. allowing 16 two Cryo-Blocks, eight 2255vials. includes Set Aluminum blockthat holds Vial 2666 2664 centrifuge tubes. inpairs. Sold standard (1.5-2.0mL)micro- Aluminum blockthat holds48 Tubes orPCR Micro-centrifuge milling. inpairs. Sold centrifuge tubesfor cryogenic standard conical-bottom 50mL Aluminum blockthat holdssix Centrifuge Tubes Cryo-Block for 5mL Cryo-Block for 15mL Cryo-Block for 2255 Cryo-Block Cryo-Block for 48 Cryo-Block for 50mL Cryo-Block 2189C Cryo-Block or2650titer plates.Cryo-Block grinding process. Used with sample lidscold duringthe The 2189Ccryoplate keeps centrifuge tubes. inpairs. Sold standard (0.6mL)micro- Aluminum blockthat holds96 2663 2661 2650 in pairs. used in2240-PEF Vial Set. Sold twenty-four 2241-PEFvials, as Aluminum blockthat holds Polyethylene Vials centrifuge tubes. inpairs. Sold fifteen 15mL round-bottom Aluminum blockthat holds Centrifuge Tubes during grinding. inpairs. Sold samples intiter plate cold for 2210 Titer Plate. Keeps aluminuminsert Extruded Titer Plates 2665 centrifuge orPCR Tubes Cryo-Block for 5mL Cryo-Block for 15mL Cryo-Block for Cryo-Adapter Cryo-Block for Micro- Cryo-Block Cryoplate GENO/GRINDER® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 19 ® ime=1 minute grinding media in the sample vial or grinding media in the sample T

After for Bead Millingfor ate=1400 ® R

Before SPELT SEEDS BEAD MILLING BEAD SEEDS SPELT Grinding Balls=4 mm PROTOCOL plate. titer Insert of the deep well each well 1 seed and 1 grinding ball in Technical information for the Geno/Grinder for information Technical titer plate. Tough tissues may require precooling to embrittle the sample and this also serves embrittle the sample to to precooling require tissues may Tough plate. titer offers SPEX SamplePrep or Proteins. such as RNA components temperature-sensitive any preserve loading of the beads should The this purpose. for accessories of cryogenica full range Kryo-Tech® sample total the of 80% canbut up to be vials sample the inside movement adequate allow always grinding of the ratio higher The the bead slurry. of agitation adequate is still there provided volume, the beads homogenization, After disruption. of cell the rate the faster sample volume, media to extractsettle and the cell can be removed. or animal tissue for plant bead mill high-throughput versatile Geno/Grinder® analysts a offers The the most provides motion that linear grinding a true design has patented The homogenization. powerful The compact and design cell lysis. and for tissue homogenization mechanism efficient The with high yields. in about 1-3 minutes, with or without buffer disruption enables complete and extraction fruit pesticide residue from used for Geno/Grinder® has also been successfully samples using the QuEChERS technique. vegetable Bead milling is the preferred method to disrupt a variety of microorganisms and plant or animal and plant a variety of microorganisms disrupt method to Beadthe preferred milling is vigorously are balls or glass beads or ceramic media such as steel grinding In bead milling, tissues. balls used grinding commonly most The with the sample. plate sealed vial or titer inside a agitated of the crushing as a result lysis occurs Disruption or cell bearings 4 mm in diameter. ball steel are nucleic acids can shearing of Low action with the sample. as they collide of the grinding media for the method of choice It is considered varying by the mill. speed of the agitation be achieved tough-to-disrupt and fungi and as bacteria such of yeast cells and microalgae. disruption samples because between both vials cross-contamination avoids that of the few method is one The range of grinding comprehensive a offers SamplePrep SPEX disposable. and grinding media are of and amount size The 50 mL. mL to 0.6 from samples ranging for plates media, vials and titer is important.the grinding media used Speed increased of disruption can be and effectiveness of and amount form the density, increasing by dramatically Using the Geno/Grinder Using Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX GENO/GRINDER® TECHNICAL INFORMATION 20 2010 GENO/GRINDER for 2minutes. liquid nitrogen for 5minutes. speedfor 1500strokes-per-minute Geno/Grinder Set submerged samplein2251grinding container in usingour 2660Cryo-block Pre-chill Animal Tissue Spelt Seeds clamp and run Geno/Grinder fromclamp andrun Geno/Grinder 1000to 1500strokes-per-minute for 1minute. pre-homogenized fruit into intoInsert 50mLtubes. foam holders, Insert place into Fruit for oneminute at 1400strokes-per-minute. seal plate withalumniumfoil. Place titer plate andrun it inclampofGeno/Grinder speltseedsandone9mmgrindingballinto eachwellInsert ofatiter plate. Add a of vials in Cryo-Block inliquidnitrogen. 5minute grindatof vialsinCryo-Block 1500 rpm. in2255vialswith2 wasSample inserted WC balls(7/16”).15minute pre-cool Corn BEFORE BEFORE BEFORE BEFORE ® BEFORE & AFTER SAMPLES AFTER AFTER AFTER AFTER

GENO/GRINDER® APPLICATION NOTES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 21

buffer at pH 2 or trichloro-acetic acid. at pH 2 or trichloro-acetic buffer 4 PO 2 HOMOGENIZATION/ APPLICATION: DNA EXTRACTION DNA APPLICATION: HOMOGENIZATION/ The following are excerpts of application notes for the 2010 Geno/Grinder. To access our full library our full access To the 2010 Geno/Grinder. for notes of application excerpts are following The www.spexsampleprep.com/appnotes. visit note application the complete and download APPLICATION: RNA EXTRACTION RNA APPLICATION: APPLICATION NOTE SP014: RNA EXTRACTION FUNGUS RNA FROM SP014: NOTE APPLICATION RNA Extraction from Aspergillus parasiticus mycelium parasiticus RNA Extraction Aspergillus from and others produce nontoxic, are Paraciticus fungus Aspergillis Some of the filamentous strains extracted was from RNA this, study To products. food other and infected in grain aflatoxins adding then cryogenicallythem Geno/Grinder, SPEX a in pulverizing after samples Aspergillis the samples. homogenize the Geno/Grinder to them to the vials and returning to Puresol APPLICATION NOTE SP001: CELL DISRUPTION / APPLICATION: CELL LYSIS CELL APPLICATION: / DISRUPTION CELL SP001: NOTE APPLICATION APPLICATION NOTE SP013: GRINDING / DISRUPTION / GRINDING SP013: NOTE APPLICATION LEAVES IN MEASUREMENT METABOLITE SOLUBLE AND STARCH APPLICATION: APPLICATION NOTE SP011: SP011: NOTE APPLICATION MATERIAL LEAF OF Geno/Grinder that is run for two periods of one minute at 1000 strokes per minute. Then 300 Then per minute. 1000 strokes at periods of one minute two for is run Geno/Grinder that for 30 running the vials by homogenized contents to each vial and the is added µL of buffer tissue transferred and the lysed plant centrifuged vials are The 1000 strokes/minute. at seconds analysis. to DNA rinsed and dried prior filtered, then mixed, plates, microtiter to of Measurement for Extraction Acid of Leaves Perchloric and Soluble Metabolites Starch Perchloric liquid nitrogen. in SPEX 5-mL vials and chilled in up is placed material Harvested plant in a SPEX Geno/ run vials are The ball. vial along with a stainless steel each acid is added to the if necessary or longer pulverize per minute, to 1500 strokes at Grinder 90 seconds for The then centrifuged. which is mixed, vial, each acid is added to perchloric More contents. starch. for pellet assayed and the centrifuged soluble metabolites, for is analyzed supernatant Extraction of Nucleic Acids from Sugar Beet Sugar Extraction Leaves from Nucleic Acids of in a 2mL of each sample is placed 1 grams and 0.5 to Sugar beet leaf tissue is freeze-dried, in a SPEX a time, 96 at pulverized, are samples The Eppendorf balls. steel vial with two Sample preparation is often the bottleneck in the process of efficient analysis work. Up to now to work. Up analysis efficient of bottleneck in the process the is often Sample preparation of been based on the modification have grinding effortscells through to mechanically disrupt the Geno/Grinder® was The plates. titer micro for with an adapter ball or swing mills traditional for used (PP), well plates deep Two cell disruption. for mill specifically designed available first each next placed to were with 1.5 – 2 ml wells collecting of biological materials and storing in each placed were muscle or livers dried rat Freeze other in the Geno/Grinder clamp assembly. with 100mM KH and spiked well plate Mechanical Disruption for High-Throughput Fatty Acid Acid Fatty High-Throughput Mechanical Disruption for Samples Tissue Extraction Animal from GENO/GRINDER APPLICATION NOTES APPLICATION GENO/GRINDER Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX GENO/GRINDER® APPLICATION NOTES 22 used to disrupt yeast inamicrowell plate format. SamplePrep, Metuchen, NJ), a bead mill originally designed to smash seeds in deep well plates, be can combines disruption mechanical ofcells inahighthroughput format. The (SPEX Geno/Grinder® individual processing isamajorbottleneckandimpractical. Consequently, amethodisneededthat where large numbersofyeast clonesmustbeexamined inahighthroughput screening environment, mill (i.e., beadbeater). Inbothapproaches, samplesare processed individually. For experiments disruptionMechanical ofyeasts hastraditionally beenaccomplished by usingeithera High Throughput of Disruption Yeast ina96-Well Format FORMAT / APPLICATION: DNA/RNA AND OTHER EXTRACTIONS APPLICATION NOTE SP018: HIGH THROUGHPUT DISRUPTION OF YEAST IN A 96-WELL samples have beencapped, at grindthemintheGeno/Grinder 500strokes/minute for two minutes. one seed to each well. buffer into extraction each Dispense well and securelycap each well. After the bead into eachwell usingtheGrinding areSamples prepared usinga96-well one5/32in.(4mm)stainlesssteel 1mLassay Dispense block. from Seed Rice DNAExtraction Quick per well. systems are delivery Other commercially available. tip emptiedinto atiter plate well. This technique willdeliver approximately 0.4grams of a numberofways. micropipette Inthiscase tipswere filled to themarkwithgrindingbeads, andeach Grade, cat. no. 2166). The ofthebeadsinto delivery eachcell ofthetiter plate beaccomplished can in Standard 96-well titer plates were Biology grindingbeads(Molecular usedwith400-600μsilica The was Geno/Grinder tested to determine ifthistechnology could beusedto cells. lysebacterial Lysing Cells ofBacterial intheGeno/Grinder FROM RICE SEEDS APPLICATION NOTE SP016: LYSING / HOMOGENIZATION / APPLICATION: DNA EXTRACTION APPLICATION: DNA/RNA AND OTHER EXTRACTIONS APPLICATION NOTE SP020: LYSING OF BACTERIAL CELLS a rate of2000cyc/min. In addition,optimalhomogenization conditionswere usingtheGeno/Grinder found to be90sec. at providedof theGeno/Grinder weight DNA withhighermolecular thanthecompetitive instrument. Grinder, whilebuffers, from fresh basil. Inaddition,homogenization timeandoperating rate were varied for theGeno/ The was Geno/Grinder® compared withacompetitive cell lyser(Competitor ofDNA A) for extraction Fresh Lysed Basil in2ml Tubes withthe Geno/Grinder of Effect Lysis OtherTime and from Variables onDNAExtraction APPLICATION: APPLICATION NOTE SP017: LYSIS TIME AND OTHER VARIABLES ON DNA EXTRACTION / DNA EXTRACTION FROMDNA FRESH EXTRACTION BASIL LYSED grinding mediaandtubesize remained constant. Resultsindicated that use Ball Dispenser (SPEXSamplePrep Dispenser Ball Cat. No. 2100).Next, add ® ® press orbead silica beads silica GENO/GRINDER® APPLICATION NOTES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 23 QuEChERS VS MODIFIED High-Throughput Tissue Tissue High-Throughput ® APPLICATION NOTE SP024: PESTICIDE ANAYLSIS: STANDARD STANDARD ANAYLSIS: PESTICIDE SP024: NOTE APPLICATION / PESTICIDE EXTRACTION PESTICIDE QuEChERS / APPLICATION: / METHOD Extraction of RNA/cDNA and Genomic DNA from Tissue with Tissue Extraction of RNA/cDNA and Genomic DNA from PCR Real-Time mix samples and to the fruit/vegetable homogenize to employed the Geno/Grinder was In this study, extraction the in an effortto improve with the salts and solvent and thoroughly rapidly the produce whether the use of the Geno/Grinder during the determine to goal of the study was The step. manual QuEChERS method. the traditional, over pesticide recovery increase extraction would step APPLICATION NOTE SP022: THE BENEFITS OF THE GENO/GRINDER FOR PESTICIDE PESTICIDE FOR GENO/GRINDER THE OF BENEFITS THE SP022: NOTE APPLICATION EXTRACTION RESIDUE PESTICIDE APPLICATION: / ANALYSIS RESIDUE APPLICATION NOTE SP021: EXTRACTION OF RNA/CDNA AND GENOMIC DNA FROM TISSUE TISSUE FROM DNA GENOMIC AND EXTRACTIONRNA/CDNA OF SP021: NOTE APPLICATION EXTRACTIONS OTHER AND DNA/RNA APPLICATION: / PCR REAL-TIME WITH Sample preparation for pesticide residue analysis has typically followed DuPont Report No. AMR AMR Report DuPont No. has typicallyanalysis followed residue pesticide for Samplepreparation Residues in and Cymoxanil of Famoxadone the Determination for Method “Analytical 3705-95, extraction followed into jars, weighed samples are ground-up (2) In this procedure, Matrices.” Various is added and extraction. prior to Acetonitrile re-hydrate them to allow to the addition of water by settleout to is then allowed matrix plant The with a laboratory homogenizer. ground samples are The collected and in mixing sodium chloride. containing and liquid extracts cylinders filtered are aid in the dissolution of sodium chloride and to and inverted shaken, mixing cylinders capped, are Separate separated. phases water and layer) (upper acetonitrile the while stand to allowed then analysis. cymoxanil for and famoxadone taken aliquots are acetonitrile The Benefits of the The Geno/Grinder Fresh samples of animal tissue were collected, trimmed to approximately 50 – 100 mg of wet weight, weight, – 100 mg of wet 50 approximately trimmed to collected, of animal tissue were samples Fresh cow, mouse, cat, man, dog, were animals The –800º C. at and stored in liquid nitrogen, snap-frozen extraction, DNA and/or RNA 1. Table the tissues Before fish and clams; see as as well and horse, contained of dry standing on a block well Each plate a deep-well titer ice. to frozen transferred were (Applied of buffer and 500 microliters 2150) no. cat. CertiPrep balls (SPEX steel 4-mm stainless two and cover a plastic sealed with were The plates lysis buffer). nucleic acid purification Biosystems per minute. a setting of 1000 strokes at grinding in the 2000 Geno/Grindersubjected 2 minutes for to Extraction of RNA/cDNA and Genomic DNA from Tissue with with Tissue Extraction Genomic and of RNA/cDNA DNA from PCR Real-Time Homogenizer to Increase Sample Throughput for Pesticide Pesticide for Throughput Sample Increase to Homogenizer LC/MS/MS by Residue Analysis Grinding & Pulverizing 1500 ™ Mixing & ShaQer Blending

The ShaQerTM APPLICATIONS The 1500 ShaQer™ is designed to effectively pulverize samples for food analysis. It is the ideal • Pesticide residue tool for QuEChERS and features many benefits over extraction handshaking including: increased recovery, higher • QuEChERS throughput, improved consistency and reduced user • SWeET method fatigue.

Its vigorous vertical motion is effective at improving SAMPLE TYPES analyte extraction from food products for analysis of pesticides, PAH’s, antibiotics, mycotoxins, and dyes. • Animal tissue In addition to increased analyte recovery, using the • Plant tissue ShaQer™ for this type of analysis ensures sample • Vegetables preparation consistency since every sample is • Fruit processed in exactly the same manner.

Voltage 115V/60Hz or 230V/50Hz 3-prong grounded plug 115V, 60Hz. Power Cord 2-prong European cord for 230V, 50 Hz. CE Approved Yes 21.5 in. (54.6 cm) high x 11.25 in. Clamp Dimensions (28.6 cm) wide x 17.0 in. (43.2 cm) 1.25 in. (3.2 cm) vertical Movement deep Weight 40 lbs. (18.2 kg) Clamp Speed 1500 strokes per minute Digital in minutes:seconds, Motor 1/7 HP Timer/Controls maximum 5:00

24 1500 ™ 1

ShaQer SHAQER Part number: 1500 Features & specifications TM 1. Safety interlock prevents unit from operating when lid is open. Window allows analyst to view samples during operation. 2 2. Vertical shaking motion ensures thorough mixing and analyte extraction. 3 3. Clamp holds six 50 mL vials or six 15 mL vials. Alternate clamp for six 50 mL vials or six 4 2 mL vials. 4. Spill tray for easy cleanup. 5 5. Digital timer display with adjustable operating time. 6 6. Compact, powerful motor shakes samples at 1500 rpm.

For video, scan with your smart phone or

visit www.youtube.com/ Order 24/7 online: www.spex.com sampleprep ShaQer ACCESSORIES

1590 Clamp 1595 Clamp This clamp for the ShaQer™ This clamp for the ShaQer™ holds six 50 mL vials or six holds six 50 mL vials or six 15 mL vials. 2 mL vials.

2183 Ceramic Grinding 2184 Ceramic Grinding Cylinder Cylinder 3/8 in. x 7/8 in., large, ceramic 5/16 in. x 5/8in., Medium,

grinding cylinders with angle- ceramic grinding cylinders . Call: 1- cut ends for use with standard with angle-cut ends for use 50 mL centrifuge tubes. Sold in with standard 15 mL centrifuge bags of 100. tubes. Sold in bags of 100. 855-GET-SPEX 2185 Ceramic Grinding Cylinder TRY IT BEFORE YOU BUY IT! Small size ceramic grinding Demo and Sample Test Programs cylinders with angle-cut ends are available for this product. for use with standard 5 or 15 See pages 108-109 for more mL centrifuge tubes. Sold in details bags of 100. 25 Grinding & Pulverizing

Tissue Homogenization & Cell Lysis

• 6770 Freezer/Mill® • 6870 Freezer/Mill® • 6870D Freezer/Mill® • 6970EFM Freezer/Mill®

THE FREEZER/MILL® Our Freezer/Mills are programmable cryogenic laboratory mills that cool samples to cryogenic temperatures, then pulverize them by magnetically shuttling a steel impactor back and forth against two stationary end- plugs. Since the vial is closed, the integrity of its contents is maintained, hazardous or critical samples are easily controlled, cleanup is simplified and cross-sample contamination is eliminated. The vial is cooled by liquid nitrogen throughout the grinding cycle which keeps the sample at cryogenic temperatures and preserves its key aspects. A touch screen control panel allows up to 10 user-defined grinding programs for simple and fast recall. Applications Sample Types • DNA/RNA • Drug testing • Animal tissue • Electronic extractions • RoHS/WEEE • Plant tissue components • Yeast analysis • Plastic • Polymers • Textiles • Yeast • Hair • Pharmaceutical • Polymers analysis • Pharmaceuticals • Teeth • Food Testing • Food products • Bone

TRY IT BEFORE YOU BUY IT! Demo and Sample Test Programs are available for this product. See pages 108-109 for more details

26 FREEZER/MILL® Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 27 6770-230 sampleprep For video, scan with video, For your smartyour phone or visit www.youtube.com/ Part number: 6770-115 number: Part 26 lbs (11.8 kg) 60Hz. plug 115V, grounded 3-prong 50 Hz. 230V, for cord European 2-prong 10 grinding programs Stores 5 4 Magnetically driven impactor in the vial is Magnetically driven part.the only moving tub is equipped liquid nitrogen Insulated sensor. with LN level

4. 5. Power Cord Power Weight (lbs) Weight Timer/ Controls

3 1 2 Yes 19 in (48 cm) x 10.5 in (27 cm) x 12.75 in (32 cm) 115V/60Hz or 230V/50Hz Pre-cooling and grinding chamber. Lid safety interlock for operator protection. protection. operator for Lid safety interlock Touch-screen controls for programming programming for controls Touch-screen impactgrinding cycles and time, rate, pre-cooling times. and cooling

CE Approved Dimensions Voltage Features & Specifications 6770 Freezer/Mill® is a small cryogenic mill that accommodates samples ranging from 0.1-5 g. 0.1-5 g. from samples ranging is a small cryogenic accommodates mill that 6770 Freezer/Mill® The Its specificallyfor designed set. microvial Its grinding chamber holds one small grinding vial or one samples in a grinding vial immersed in sensitive the cryogenic and/or temperature grinding of tough with cryogenic the sample at temperatures keeps This the grinding cycle. throughout liquid nitrogen aspects its key preserved. 3. 2. 1. Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX FREEZER/MILL® 28 samples inagrindingvialimmersedliquidnitrogen. grindingandpulverizing designed for cryogenic Specifically tough and/or temperature sensitive The 6870Freezer/Mill® isalarge millthat accommodates cryogenic upto 100grams ofsamples. 3. 2. 1. Features &Specifications Dimensions CE Approved Voltage

the only moving part. the onlymoving part. drivenMagnetically inthevialis impactor and protective foam. interlockLid safety for operator protection andcooling times.pre-cooling rate, andtime,grinding cycles impact Touch-screen controls for programming cm) x18in(46 20.5 in(52cm)x21.5 in(55 Yes or230V/50Hz 115V/60Hz 1 4 3 Timer/Controls Power Cord Weight 6. 5. 4.

5 Optional 6820LNautofillOptional available. level sensor. Liquid nitrogen tubisequippedwithLN grinding vialsorfour microvial sets one mid-sized vialorupto four standard Chamber holdsonelarge grindingvialor 2 6 Part number:6870-115 programs Stores up to 10grinding plug, 230V/50Hz or2-prong60Hz European 3-prong grounded plug, 115V 44 lbs(24kg) visit www.youtube.com/ your smart phoneor your smart For video, with scan sampleprep 6870-230 FREEZER/MILL® Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 2929 6870D-230 sampleprep For video, scan with video, For your smartyour phone or visit www.youtube.com/ Part number: 6870D-115 number: Part Stores up to 10 grinding up to Stores programs 78 lbs (35 kg) 115V plug, grounded 3-prong plug, European 60Hz or 2-prong 230V/50Hz 7 Magnetically driven impactor in the vial is Magnetically driven part.the only moving with LN level tub is equipped Liquid nitrogen sensor. with LN autofill Equipped Dual grinding chambers hold one large Dual grinding chambers hold one large vial or up to grinding vial or one mid-sized microvial grinding vials or four standard four sets each.

5. 6. 7. 4. Timer/Controls Weight Cord Power 3 2 4 5 1 6 115V/60Hz or 230V/50Hz Yes 20 in (50.8 cm) x 21 in (53.34 cm) x 25.5 in (64.77cm) Dual pre-cooling samples chambers keeps while other temperature appropriate the at grinding. samples are Lid safety interlock for operator protection protection operator for Lid safety interlock foam. and protective Touch-screen controls for programming programming for controls Touch-screen pre- impactgrinding cycles and time, rate, times. and cooling cooling

Dimensions CE Approved Voltage Features & Specifications 3. 2. 1. has dual grinding and cooling chambers allowing you to pre-cool to one set of you chambers allowing ® has dual grinding and cooling 6870D Freezer/Mill The in a Dual 200 grams grinding chambers can grind up to samples while another set is being ground. per chamber.) (100 grams single run. Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX FREEZER/MILL® 30 3. 2. 1. different protocols, providing andspeed. flexibility increased samplethroughput. These beprogrammed chamberscan for independent operation and accommodates samplesfrom 0.5-100grams (0.6-50mL).Ithasdualgrindingchambersfor The 6970EFM Freezer/Mill® Large capacity, high-throughput, enclosed,millthat cryogenic Features &Specifications Dimensions CE Approved Voltage

and protective foam. interlockLid safety for operator protection system. Totally enclosedliquidnitrogen withAuto-Fill andcooling times.pre-cooling rate, andtime,grinding cycles impact Touch-screen controls for programming cm) x17in.(43 22 in.(56cm)x18¼ in.(46 Yes or230V/50Hz 115V/60Hz 2 1 3 4 5 Timer/Controls Power Cord Weight 5. 4.

sets each. standard smallvialsorupto four microvial one large vial, onemid-size vial, orupto four vial. andcooling Grinding chamberholds uptoGrinds 100grams ofsamplesperlarge only moving part. drivenMagnetically inthevialis impactor programs Stores up to 10grinding 230V/50Hz or2-prong60Hz European plug, 3-prong grounded plug, 115V 70 lbs. (31.7kg) Part number: visit www.youtube.com/ your smart phoneor your smart For video, with scan sampleprep 6970D-230 6970D-115 FREEZER/MILL® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 31 Small Large Small Stainless Steel Large Cr-Free Vial Vial Large Cr-Free Small Poly-Vial Set Small Poly-Vial 6751C4 Polycarbonate Polycarbonate Cylinder Center 6751 vial set; sold in For in package comes of 4. Also pack of 20 (6751C20) Set grinding electronic For chromium for test to components under RoHS/WEEE directives. vial plus Set includes 1 complete 3 extra cylinders. Sample capacity 50 mL (1 - 100 g). up to Polycarbonate end plugs Polycarbonate polycarbonate- and cylinder, Encapsulated encased impactor. Includes one impactor. steel center vial and 3 spare complete cylinders. Sample capacity 0.5 - 4.0 mL (0.1 - 5.0 g). Grinding Vial Grinding Vial Set Set includes stainless steel center stainless steel impactor, and end plugs, two cylinder, O-rings. pack of one hundred 6801C4 6871 6761 6781S Polycarbonate Center Center Polycarbonate Cylinder polycarbonate Replacement cylinders 6801 Large center for Sold Set. as a Vial Grinding pack of 4. ACCESSORIES ® microvial set microvial Small Grinding ­ Cr-Free Vial Small Vial Set Cr-Free Large Steel Center Large Steel Center Large Grinding 3 microvials in a vial holder in 3 microvials simultaneous sample allowing vial holds up Each processing. Ideal 0.5 g of samples. 0.1 to to grinding small quantities for and of samples such as plant animal tissue. 6757 End plugs and impactor are Cr- plugs and impactorEnd are Set includes steel. 06 ASTM free 6751C cylinders. Sample capacity (0.1 - 5 g). 0.5 - 4.0 mL 6771 6751 Vial SetVial Set includes stainless steel and 4 2 end plugs, impactor, cylinders. center polycarbonate Sample capacity 0.5 - 4.0 mL (0.1 - 5.0 g) Cylinder in place Used Set. Vial 6801 For of 6801C when polycarbonate cylinder with is not compatible Made of nonmagnetic sample. stainless steel. Vial SetVial Set includes stainless steel impactor end plugs, and two center polycarbonate plus four cylinders. Sample capacity up to 50 mL (1 - 100 g) 6802 6801 Vials for the Freezer/Mill product line consist of a center cylinder, two end plugs, and an impactor. and an impactor. plugs, end two cylinder, a center of product line consist the Freezer/Mill for Vials extraction for removable are plugs end the while cylinder chamber, grinding the forms center The cylindrical end solid, to end impactorThe is magnetically shuttled from cleaning. of sample and impactor the end plugs. the against by struck is the sample as occurring grinding with in the vial, of Actual sample capacity depends on the nature a vial for range Sample capacity is approximate. the material. FREEZER/MILL Grinding Vials Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX FREEZER/MILL® ACCESSORIES 6881, 6883,and6885vialsrequire 6886adapter 32 Extractors Vial Racks 20 (6881C20). inpacksof4and mL (1-40g).Sold uptovial sets.25 capacity Sample for 6881,6883and6885 cylinders Replacement polycarbonate center Center Cylinder 6758 6881C4 6754 see thevideo. youtube.com/sampleprep to microvial sets. Visit www. end plugsfrom chilled6757 This removes endplugextractor removes endplugs. out ofallFreezer/Mills and smallgrindingvialsinand lifts The opener 6754extractor/vial VialsSmall for 6755 6814 (6814-230). size vialsets. CEApproved. Available for 115 operationV/60 Hz (6814-115)and230 V/50 Hz special adapter for small vialsets(6751,6761,6771,and6781S).Not adaptablefor mid- reduces operator effort. The 6814willopenlarge vialsets(6801,6871)andincludesa powered version openers. ofour6754and6804extractor/vial Itincreases throughput, Frozen Itisanelectrically beeasilyopenedwiththe6814AutoExtractor®. grinding vialscan storage andhandling. holds upto vialsfor sixteen Glass-reinforced acetal rack Vials 6881 plus three cylinders. extra includesonecompleteSet vial upto 25mL(1-40g). capacity Sample (6881C). cylinder impactor, polycarbonate center Stainless steel endplugs and Extractor for Microvials Extractor Extractor/Vial Opener Opener Extractor/Vial AutoExtractor® for Freezer/Mill® AutoExtractor® Vial Sets Vial Rackfor Small Mid-Size Mid-Size Vial Set Mid-Size PolycarbonateMid-Size 6805 storage andhandling six 6801or6871vialsetsfor Epoxy-coated steel rack holds Vials 6885 6883 mL (1-40g). steel. upto 25 capacity Sample polycarbonate-encapsulated are polycarbonate, is impactor End plugsandcenter cylinder up to 25mL(40g) center capacity Sample cylinders. 6811C4 mid-size polycarbonate steel endplugsandonepackof impactor, two 6883Emid-size Includes one6883Pmid-size steel 6804 6756 end-plug extraction. removes endplugs. Lever assists out ofallFreezer/Mills and largeLifts grindingvialsinand for andMid-Sized Large Vials sampleprep to seethevideo. www.youtube.com/6781S). Visit vials (6751,6761,6771and end plugsfrom smallgrinding This removes endplugextractor vials Vial Rackfor Large Mid-Sized Poly-Vial Mid-Sized CR-Free Mid-Size Vial Extractor/Vial Opener Opener Extractor/Vial for small Extractor FREEZER/MILL® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 33 Mid-Size Vial Mid-Size Vial Mid-Size Vial Adapter Vial Mid-Size Insert bell of 6804 extractor for plug extraction end allow to for Insert vials. is easily mid-size installed and removed. 6884 6870M Accessory Package Vial Includes 6884 Mid-Size 6804 Extractor/Vial for Adapter Vial and 6886 Mid-Size Opener, Freezer/Mills. large for Adapter Microvial SampleMicrovial Small Vial AccessoryVial Small Large Vial AccessoryVial Large Mid-Size Vial Adapter Vial Mid-Size Multi-Vial Holder Multi-Vial Positions and aligns mid-size mid-size and aligns Positions and vials in 6870, 6870D, Freezer/Mills. 6970EFM 6886 6807 four one to holder positions Vial small vials (6751, 6761, 6771, 6781S). It also holds the 6757 6870, 6870D, set for microvial Freezer/Mills. and 6970EFM 6753C 6753C Extraction Tool Sample extraction for tool samples from ground removing 6757 microvials. Package Holder, Includes 6807 Multi-Vial and Opener, 6754 Extractor/Vial 6755 Vial Rack. 6870L 6870S Package Includes 6804 Extractor/Vial Rack. Vial Opener and 6805 Accessory Packages Accessory Sample Adapters & Holders Sample Adapters Each 6870, 6870D, or 6970EFM is supplied with your choice of either a 6870L large vial accessory of either a 6870L large choice is supplied with your or 6970EFM 6870, 6870D, Each accessory 6870M mid-size package is also The package or a 6870S small vial accessory package. the 6870, that Note accessory packages as an option; descriptions of all three follow. available going are and if you vials, and large mid-size, can all hold small, Freezer/Mills and 6970EFM 6870D, will need the accessory of vial. of vial you packages each addition size for than one size use more to the individual but so are purchase, separate all the accessory for only are packagesNot available of each accessorycomponents package. Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX FREEZER/MILL® ACCESSORIES 34 be installedandcalibrated at ourfactory. Itisincludedwiththe6970EFM and6870DFreezer/Mills. The 6820 Auto-Fill System should be ordered at the same time as the 6870 Freezer/Mill so it can liquid nitrogen inthehoseandvalves at bothendsare closed. of the transfer hose, and vents nitrogen gas pressure that may build up in the hose when there is supply viaa1/2inch(12.7mm)JICfemale flare nut. The safety relief valve attaches at thehighpoint The Auto-Fill System relief isalsosuppliedwithasafety valve thatto theliquidnitrogen connects adapter to allow compatibility withthe6906and6907Cryogenic Transfer Hoses. (12.7 mm)JICfemale flare nut at eachend for proper installation. doesinclude an The 6820package beconstructed withdifferentand can materials. The transfer hosemustbe configured witha1/2inch Cryogenic Transfer Hoses, whichare soldseparately. Transfer hosesare available indifferent lengths The Auto-Fill System requires transfer hose, acryogenic suchastheSPEXSamplePrep 6906or6907 filling the reservoir. This automated system reduces thelossofliquidnitrogen andsaves thetimelostwhenmanually to handlethevolume ofliquidnitrogen required for processing samplesinthe6870Freezer/Mill. within the6870Freezer/Mill duringoperation. The Auto-Fill System isamore efficient andsafer way The 6820Auto-Fill System isdesignedto automatically maintain therequired level ofliquidnitrogen System6820 Auto-Fill for the6870Freezer/Mills for dispensing LN. Freezer/Mill LNcontact. withoutdirect We alsooffer transfer hosesas Dewarswell as25Land50 gloves mustbeworn to protect hands. 6820 Our of liquid nitrogen is -195.80º C. When working with liquid nitrogen directly or indirectly, cryogenic are products Our designedto aidtheuserinsafe handlingofliquidnitrogen. The boilingpoint Liquid Nitrogen Handling 6910 6907 22 psi.Capacityof50litres. nitrogen withpressure ofupto storing anddispensingliquid designedfor cylinder Cryogenic CylinderCryogenic * such asliquidnitrogen. fluids transferring cryogenic stainless steel hosesuitablefor 6 ft. (1.8m)longflexible Transfer Hose** 6900 large. small, medium,large andextra asapairandavailableSold in and liquidnitrogen exposure. arms from materials ultra-cold These gloves protect handsand Portable Pressurized Cryogenic Long Cryogenic Cryogenic Gloves Cryogenic Auto-Fill System isanoptionfor fillingthe6870 use withlow pressure LNtanks. (22psi) **Transfer hosesandAutofill Systems are for supplier for details. or 6870DFreezer/Mills. Call your local LN *We recommend a200LLN tank for the6970D 6906 such asliquidnitrogen. fluids transferring cryogenic stainless steel hosesuitablefor 4 ft. (1.2m)longflexible Transfer Hose** 6905 Capacity of25litres. amounts ofliquidnitrogen. storing anddispensingsmall Dewar designedfor Cryogenic Dewar* Short Cryogenic Cryogenic Short Portable Cryogenic Portable Cryogenic FREEZER/MILL® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 35 Polyethylene beads Polyethylene added into of this sample was 15 grams 6801 vial then pre-cooled in the 6870 ground Then 10 minutes. for Freezer/Mill of 15 cps. a rate cycles at 2 minute three for Beef lung small (5-8 mm) cut into Samples were bag then frozen. in a plastic placed pieces, lightly added to were pieces Frozen pre-chilled in 6870 then placed 6801 vial, 12 min. for programmed Freezer/Mill a rate pre-cool, at 3 cycles of 2 minutes of 12 cps. 0.6 grams of trimmed hair was added into added into of trimmed hair was 0.6 grams a 6801 vial then pre-cooled in the 6770 ground Then 15 minutes. for Freezer/Mill of 15 cps. a rate cycles at 2 minute three for Hair (0.6 grams) Dog Treats 1-cm cut into pieces. of treats 20 grams a 6801 vial into loaded were 15 pieces then pre-cooled 6870 Freezer/Mill in the 3 cycles for ground Then a 15 minutes. for of 12 cps. a rate at of 2 minutes Plastic toys Plastic pre- 10 minute 1 cm pieces. into toy Cut each, 3 cycles 3 minutes of period, cool with an period down cool minute two of 15 cps. impactor rate Potatoes Insert vial 6801 1 cm pieces. into into Cut pre-cool, 3 cycles minute 10 in 6970EFM. each with an impactor rate 1 minute at of 8 cps. AFTER AFTER AFTER AFTER AFTER AFTER BEFORE & AFTER SAMPLES AFTER & BEFORE ® BEFORE BEFORE BEFORE BEFORE BEFORE BEFORE FREEZER/MILL Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX FREEZER/MILL® TECHNICAL INFORMATION 36 grinding ofmultiple smallersamples. The 6870and6870DFreezer/Mill alsohold upfour can 6751,6761,and6771vialsfor simultaneous Mid-Size The new series of Mid-Size Vials of the 6801 vial and includes the 6883 has about half the capacity are 10to 20mL,equivalent to weights of 10to 20grams for polymersand20to 40grams for bone. 50 mLmaximumsamplecapacity, 10timesthat ofthe6751Small Vial Set. Typical samplevolumes holdasmallamountcan between ofsample, 30mgand200mg. typically The 6801 Vial hasat least forAs otherFreezer/Mill vials, The 6757Microvial includesthree Set 6757VMicrovials. Each Microvial incompatible withpolycarbonate. components withoutaddingchromium andthe6871SStainless Steel Vial for grindingsamples Poly-Vial for metal-free grindingofdelicate samples, the6771Cr-Free Vial for grindingelectronic polymers and2to 4grams for bone. are Specialized grindingvialswithsimilarcapacity the6761 grinding, samplevolume typical shouldbe1to 2mL,corresponding to weights of1to 2grams for samples may movement restrict oftheimpactor. For efficient hasasamplevolumeSet limitofabout5mLandbulkier anexampleAs ofsamplecapacity, the6751Small Vial colder thesample,can beground. thefinerit the temperature theoutcome; affect asa alsocan rule, the size grinding willbe.time, Incryogenic thefinerparticle cases, thesmallersampleandlongergrinding operator, and the requirements of the analyst. In most determined by experimentation, theexperience ofthe for anyfrequency sampleground intheFreezer/Mill are The optimumvolume, weight, grindingtimeandimpact Guide to Freezer/Mill Capacity Sample using “filler” sand. grindingagents suchasquartz periodtoeven 30minutes orso. lengtheningthepre-cooling Successes have alsobeenscored by samples respond to thestrategies ofreducing thesamplevolume, increasing grindingtime, and When asampleinitiallyresists grinding, itmay itis notbebecause “ungrindable.” Many such remains malleable. Metalsamplesasarule shouldbetest-ground. impure copper aswell asmany copper alloys beground can withoutmuchtrouble, whilepure copper The behavior millingishighlyvariable. ofmetalsandmetalalloys duringcryogenic For example, any form. progressively more difficult togrind. Many silicone compounds in remainelasticandhard-to-grind become size smallertheybecome more samples. asbiological theparticles flexible, As particle and flexible even at -200°C. For thesame reason, polymersingeneralcannot beground to asfinea routinelycan bemilledinpelletform are difficult togrindasthinfibersandfilms, which remain Polymers ingeneral beground, can buttheirphysical Many form isimportant. flexible plasticswhich roots, seeds, cotton andfiber. ground, size. usuallyto afineparticle This includeshair, muscletissue, bone, wood, plant stems and for test-grinding. naturally Nearly every occurring material becryogenically origincan ofbiological begroundabout whetherasamplecan inaFreezer/Mill we besubmitted willrequest that aportion grinding requirements withoneofourspecialistsbefore amill. Ifthere selecting isany question milling. For thisreason we at SPEXSamplePrep recommend that you your discuss samplesand substance thatNot every isdifficult togrind at room temperature canbepulverizedcryogenic by Limits of Cr-Free Vial andthe6885Mid-Size Poly-Vial aswell asthestandard 6881Mid-Size Vial. Cryogenic Grinding Cryogenic FREEZER/MILL® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 37 Fig. 2 Fig. AFTER Fig. 1 Fig. BEFORE Consider analyzing circuit boards: for example, USB flash drives that act as portable hard disk drives, act that as portable USB flash drives disk drives, example, hard for boards: analyzing circuit Consider 1) samples (Fig. These motherboards. on computer installed are modules that RAM and the larger a board from taken A small piece etc. substrates, resins, metals, materials: of many composites are batch much less an entire whole board, of the not be representative would random at or there here the sample that and in effect homogenizing them, assures boards, sampling many Hence, of boards. and be rugged made to memory are boards However, of the batch. analysis is representative used for Furthermore, powder. veryinto grind to difficult and are of conditions, range a wide over durable all have and other materials resins Metals, than others. fragile be more may some of the components components Some laboratory mills. conventional properties distinct when put through and different a shearing action and other require Some may not. and some may temperature, room grind at may abrasion. part it is impractical memory are to same integral of the components all of these board, When For special type their own for of mill. each suited components, its several into board the down break principle behind general The is the answer. cryogenic grinding in the Freezer/Mill such situations, impact, them up through and then break brittle, they are cryogenic until chill samples grinding is to or RAM such as the USB flash drive the sample, In the case of the Freezer/Mill, or shearing. crushing, sized in the appropriately then placed These are manageable pieces. be first cut into would module, Cr-free (6771, 6871, or 6883) with its magnetically driven Vial Grinding Cr-Free SPEX SamplePrep the until and immersed in liquid nitrogen the Freezer/Mill into vial is then loaded The impactor. for minutes 20-30 as much as but minutes, 10-15 of matter a usually chilled, thoroughly are contents the vial is The sample inside module. and RAM flash drive such as the USB components complicated contamination cross-sample in a closed grinding vial, and because the sample is isolated pulverized, Grinding depending on time can vary is maintained. and sample integrity greatly is easily controlled the type of sample and its pliability can be expected in the case but a grinding time of 8-10 minutes 2) can then be used (Fig. powder uniform result is fine, The module. and RAM of the USB flash drive fusion, or other types of analyses. XRF, for The Restriction of Hazardous Substances (RoHS) and Waste Electrical and Electronic Equipment (WEEE) Electrical Equipment and Electronic Waste (RoHS) and Restriction Substances The of Hazardous waste hazardous of the accumulation minimize to introduced Union were the European of Directives of hazardous concentrations The disposal of electrical the from in landfills electronic and equipment. (PBDEs), diphenylethers polybrominated VI, chromium cadmium, mercury, lead, as such substances in electrical restricted and electronic products and/or (PBBs) are biphenyls and polybrominated components. is each component then can be mechanically separated, if the component that RoHS/WEEE states However, process. ongoing exactly an is means this of definition what The subjectlimits. RoHS the to these products and components analyticalresult, get an accurate one thing is certain; to in order boards, as circuit such components Many samples. representative homogeneous, to must be reduced traditional methods. grind using to difficult if not impossible are resins polymers and solder, wire, these homogenize to way the easiest is Freezer/Mill® CryogenicSPEX SamplePrep in the grinding materials. Cryogenic RoHS/WEEE for Grinding Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX FREEZER/MILL® TECHNICAL INFORMATION 38 cryogenically. rigid whenchilled, butthefilmsandfibers may remain flexible and become difficult togrind pellets, bemadeinto butcan thinfilmsorfibers;thepelletsgrindfairlyeasily, astheybecome grind whileothersare difficult. very For example, polypropylene issupplied tomoldersassmall time. In addition,agiven samplematerial may exist inseveral forms, someofwhichare easyto their “grindability,” anditisdifficult theoptimumsamplesize, to predict chillingtime, orgrinding withsamplesgroundAs at room temperature, enormouslyin those processed vary cryogenically a few minutes witheithermill. 30 minutes or more. Once chilled, be samples pulverizedcan quickly; grinding times rarely exceed range ofthesamplebutcan withthemillandinsulating from ability 10minutestimes vary to whilethesamplevialisimmersedinliquidnitrogen.impel asteel magnetically impactor Chilling temperatures required are hard equipment. very onmechanical SPEXSamplePrep Freezer/Mills grinding presentsCryogenic uniquechallengesfor mills, designers of laboratory asthelow in preparation withoutdamagingDNAandeven RNAthrough for nucleicacidextraction heating. structure. Bone, fingernails, ground materialstheir crystal andotherbiological can becryogenically its more volatile components, andclay minerals may bepulverized for XRDstudywithoutdistorting are properties critical preserved by chilling. Coal, for ground example, to becryogenically can retain There are also many samples which degrade in various ways during normal grinding, but whose include polymers, rubber, textiles, cereal grains, hair, fingernails, skin, bone, andmuscletissue. at roombe impact-ground temperature beembrittledby can chilling, andthenpulverized. These Many sampleswhichare analytical too flexible orsensitive to after they hadbeenground inaSPEXSamplePrep Freezer/Mill. was successfully from extracted theRomanov bonefragments techniques inbothforensic andarchaeological research. DNA years ofcryogenic oldbutalsoemphasized theimportance Nicholas IIofRussianotonlysolved nearlyeighty amystery publicity. The recent identification ofthe Czar remains of preparation tool forchemist, theanalytical itrarely receives grindinghaslongbeenavitalsample While cryogenic Key Points Grinding AboutCryogenic Technical information for theFreezer/Mill ® and techniques for your application. We strongly suggestsubmittingsamplesfor test grinding ifthere ofourmills isany thesuitability questionabout samples. Freezer/Mill themosteffective inthe world, the “mill oflast resort” for many normallyungrindable the low temperature ofthesampleismaintained duringgrinding. These features have madethe immersed inaliquidnitrogen bath insidethemill. Thus there isnocross-sample contamination, and driventhem withamagnetically impactor. Each sampleisplaced inaseparate grindingvialwhichis The Freezer/Mill millthat laboratory chillssamplesinliquidnitrogen isacryogenic thenpulverizes processing your samples. are orflexible soft at room temperature, grindingmay be theonlyviable cryogenic technique for well below temperaturesthese critical during the automated grinding sequence. For samples that process.extraction Utilizing SPEX SamplePrep Freezer/Mills will maintain thesample temperatures thatSamples require ofnucleicacidsmustbekept at extraction -80ºCorlower duringtheentire effective grindingofplanttechnique for themicrobiologist. andanimaltissueisavery Cryogenic Using theFreezer/Mill ® for

Cryogenic Grinding Cryogenic Grinding Grinding Motion

Impactor FREEZER/MILL® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 39 30 50 200 200 200 200 200 100 100 200 100 200 200 100 200 25-50 Mesh 50-100 100-200 100-200 100-200 100-200 100-200 100-200 Final Size Size Final 4 2 2 3 2 2 3 2 2 2 x 2 2 x 2 1 x 2 2 x 2 3 x 1 3 x 2 2 x 2 3 x 1 2 x 2 2 x 2 2 x 2 3 x 3 1 x 2 3 x 2 2 x 2 Time* 5 2 1 2 2 3 2 1 2 3 1 2 2 1 1.5 0.5 0.5 1.5 0.5 0.5 1.3 0.5 0.5 1.5 (g) 20g 1.5 Weight Weight Animal 2 / 1 Wad Tape Stick Chips Fibers Chunk Chunk Form Pellets Pellets Chunks 2 mil Tape 2 mil Piece 2 mm Shot Corrugated 3 mm Beads 10 mil Sheet 7 mm Pieces Whole Tooth Whole in. Thick Sheet Thick in. 10 mm Flakes Raw, 5 mm Shearings 1 Dog Hair Clipping 5 3 Fish Scales Fish Hair Melt Adhesive Hot Mouse Skin Black loaded thermoplastic Wax Candle Cardboard Permalloy Permalloy Material Foil Aluminum Nylon Elastomer Urethane Wood Sheep Wool Food Space Duct Tape Polyethylene Rubber Human Tooth Human Vertebrae Rubber, Oil-Extended Rubber, Teflon Potatoes Polypropylene *3 x 2 denotes three grinding periods of 2 minutes each with re-cooling of approximately 4 minutes between grinds. 4 minutes of approximately each with re-cooling periods of 2 minutes grinding three *3 x 2 denotes added. was detergent 1) 0.5 g of Tide agent. added as was of sodium dehydrating sulfate weight 2) Equal results. nylons yielded similar different 3) Three period between. cooling with one-minute grinds 4) 2x – two-minute extraction. amount of sand added; purpose: ethanol-toluene 5) Equal Grinding Tests with the Freezer/Mill® the with Tests Grinding Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX FREEZER/MILL® TECHNICAL INFORMATION 40 Freezer/Mill isdriven there magnetically isnowear andtear onmoving parts. sealed inthegrindingvialandimmersedliquidnitrogen, socross contamination iseliminated. the As samplesembrittleatplastics andbiological liquidnitrogen temperatures. The sampleishermetically The Freezer/Mill mill)iseffective where (acryogenic othergrindingprocesses fail. Flexible materials like Preparation ofDomestic Waste for Elemental Analysis download thecomplete application note visitwww.spexsampleprep.com/appnotes. The following are excerpts ofapplication notes for theFreezer/Mill. To and access ourfulllibrary APPLICATION: PLANT PARTS APPLICATION NOTE SP006: MILLING/BLENDING (HOMOGENIZING) APPLICATION: POLYMER BLENDING APPLICATION NOTE SP008: CHANGES IN STRUCTURAL POLYMERS APPLICATION:DOMESTIC WASTE APPLICATION NOTE SP002: GRINDING/HOMOGENIZATION FREEZER/MILL APPLICATION NOTES nitrogen bath for approximately 12minutes. the coil assemblyandimmersedinto aliquidnitrogen bath. For brittlenessthesamplewas inthe left material to ensure brittlenessofthesample. To into theopeningof thisendthefilledvialisinserted for a successful aspect The grinding procedure most important is the sufficient cooling of the milling Preparation Husksfor ofRice theAnalysis of Their Contents APPLICATION NOTE SP009: REDUCTION/HOMOGENIZATION / APPLICATION: POLYMERS subjected to cryogenic grindingthebiggerchange. to subjected cryogenic weightmolecular or a weightchange in molecular distribution. The longer the samples were tests showed temperatures, Calorimetry) Scanning changedcrystallization whichindicates reduced polymersshowed–196°C) that characteristics differ from theoriginalpolymers. DSC(Differential ground both cryogenically (at polystyrol (sPS). Aftersyndiotactic melting and re-crystallization, (CMM) withthe Freezer/Mill® polypropylene were withtwo polymers;isotactic (iPP) and started Trials to introduce permanent changes in polymers byMilling Mechanical means of Cryogenic ChangesStructural inPolymers Grinding by ofCryogenic Means two minutes. This assured sufficient coolingandtherefore optimumbrittleness. utilizing theprecool oftheFreezer/Mill, function thesampleswere heldat about-196°Cfor another adapter optionupto fourbehomogenized samplescan simultaneouslyinthelarge Freezer/Mill®. By geneswas analyzed ofcertain viaPCRormicro arrayand theactivity analysis. With themulti-vial diseases, genes. especiallyoftheknee joint andcertain Total RNAwas isolated tissue from cartilage ofthestudywasThe to object determine ifthere between theseriousnessofarthritic isaconnection from Cartilage RNA Extraction Tissue Using Grinding Cryogenic to the25- 175μmthickmembrane. approx. 10μm during grinding. The resulting powder ismixed withacatalyst andsprayed onto dry whichobviouslysoft makes milling difficult.particle size) TheNafion granules(5mm are reduced to Nafion powder, the Freezer/Mill, millisutilized. acryogenic flexible and As apolymerNafionis very The DLRhasnow developed a methodto applytheNafioninpowder form. ofthis For theproduction Nafion APPLICATION NOTE SP005: DNA/RNA / EXTRACTION APPLICATION: PCR ® -Powder for theProduction ofFuel Cell Electrodes Visit our youtube channel

Our YouTube channel has all the latest videos for our products! Scan the QR code with your smart phone or visit www.youtube.com/ sampleprep

subscribe today! 41 Mixing & Blending Grinding & Pulverizing

Tissue Homogenization & Cell Lysis

• 8000M Mixer/Mill® • 8000D Mixer/Mill® • 5100 Mixer/Mill®

THE MIXER/MILL® The SPEX SamplePrep 8000-series and 5100 Mixer/Mills are laboratory mills that pulverize small amounts of hard, brittle samples to analytical fineness. They are functionally described as shaker mills or high-energy ball mills. The vial, which contains a sample and one or more balls, is shaken in a complex motion that combines back-and-forth swings with short lateral movements, each end of the vial describing a figure-8. The clamp's motion develops strong G-forces in the vial, to pulverize the toughest rocks, slags and ceramics.

APPLICATIONS SAMPLE TYPES • Blends • Nanomilling • Rocks • Pharmaceuticals Powders • Minerals • Plant Tissue • Extractions • Sand • Animal Tissue • Makes • Slurry Grinding • Cement • Seeds Emulsions • Slag • Catalyst • Mechanical • Ceramics Supports Alloying • Glass

TRY IT BEFORE YOU BUY IT! Demo and Sample Test Programs are available for this product. See pages 108-109 for more details

42 MIXER/MILL® Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 43 8000M-115 8000M-230 sampleprep For video, scan with video, For your smartyour phone or visit www.youtube.com/ 1/3 hp, 1725 RPM @ 60Hz, 1/3 hp, 1425 RPM @ 50Hz plug 115V, grounded 3-prong for cord European 60Hz. 2-prong 50 Hz. 230V, 2 1/3 in (5.9 cm) back-and-forth, 1 in (2.5 cm) side-to-side @ 60Hz1060 cycles per minute @ 50 Hz875 cycles per minute 6 Part number: number: Part 3 Shock-mounted electric motor for tabletop electric tabletop for motor Shock-mounted operation. swings back-and-forthClamp with a short "figure-8" movement. lateral is factory-set Timer range. 100-minute for extend timer to Optional chip is available 1,000 or 10,000 minutes to range

4. 5. 6. 4 Cord Power Movement Clamp SpeedClamp Motor Motor 1 5 Yes 19 in (48 cm) x 14 in (36 cm) x 18 in (46 cm) 76 lbs (35 kg) 115V/60Hz or 230V/50Hz Equipped with safety interlock system for for system with safety interlock Equipped protection. operator Forced air cooling fan. cooling air Forced Steel housing protects the clamp mechanism housing protects Steel a long life constructionand rugged ensures of heavy work. 2

CE Approved Dimensions Weight Voltage Features & Specifications 3. 2. 1. is a high-energy ball mill that accommodates sample sizes ranging from from ranging sample sizes accommodates ® is a high-energy ball mill that 8000M Mixer/Mill The Accepts or mixing emulsions. blending powders 60 mL for and up to grinding, 10 mL for 4 mL to 2 ¼ in. (5.7 cm) 3 1/8 in. (7.9 cm) in length and up to 1 ¾ in. (4.5 cm) to grinding/mixing vials from adapter. vials as small as ½ in. x 1 in. (12.7 x 25.4 mm) with proper accepts Also in diameter. ® 2 1 Part number: 8000D-115

8000D-230 MIXER/MILL

For video, scan with your smart phone or visit www.youtube.com/ 3 sampleprep

4 5 6

The 8000D Mixer/Mill is an efficient two-clamp laboratory mill that offers increased sample throughput while using the same vials as the 8000M. Grinds an average of 20 grams of sample per run, 10 grams per clamp.

Features & Specifications 1. Steel housing protects the clamp 4. Shock-mounted electric motor for tabletop mechanism and rugged construction operation. ensures a long life of heavy work. 855-GET-SPEX 5. Clamp swings back-and-forth with a short 2. Forced air cooling fan. lateral "figure-8" movement.

. Call: 1- 3. Equipped with safety interlock system for 6. Timer is factory-set for 100-minute range. operator protection. Optional chip is available to extend timer range to 1,000 or 10,000 minutes.

1/3 hp, 1725 RPM @ 60Hz, Voltage 115V/60Hz or 230V/50Hz Motor 1425 RPM @ 50Hz 3-prong grounded plug 115V, CE Approved Yes Power Cord 60Hz. 2-prong European cord for 230V, 50 Hz. 24 in (61cm) x 17 in 2 1/3 in (5.9 cm) back-and-forth, Dimensions Clamp Movement (43cm) x 11 in (28cm) 1 in (2.5 cm) side-to-side 1060 cycles/minute (115V) Weight 82 lbs (37 kg) Clamp Speed

Order 24/7 online: www.spex.com or 875 cycles/minute (230V)

44 MIXER/MILL® Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 45 5100-115 5100-230 sampleprep For video, scan with video, For your smartyour phone or visit www.youtube.com/ in (12.7 mm) front-to- Part number: number: Part 1/15 hp, 3000 RPM @ 60Hz, 1/15 hp, 2500 RPM @ 50Hz 1 back, 3/8 in (9.5 mm) side- to-side 3000 back-and-forth cycles at 60Hz, 50Hz. 2500 cycles at Shock-mounted electric motor for tabletop electric tabletop for motor Shock-mounted operation. is factory-set Timer range. 100-minute for

1 3. 4. Motor Motor Movement Clamp SpeedClamp 2 3 4 15.2 lbs (7 kg) 60Hz. plug 115V, grounded 3-prong 115V/60Hz or 230V/50Hz 12 in (33 cm) x 8 in (20cm) x 8 in (20cm) Equipped with a lid latch for safety. for with a lid latch Equipped Steel housing protects the clamp housing protects Steel constructionmechanism and rugged of heavy a long life work. ensures

Power Cord Power Weight Dimensions Voltage Features & Specifications 2. 1. 5100 Mixer/Mill is an efficient, compact samples in laboratory mill of pulverizing capable is an efficient, 5100 Mixer/Mill The ½ inch clamp can hold three The 3 mL. up to or mixing samples with volumes range, the 1 gram 2 inches. with lengths up to vials, ¾ inch diameter or two vials, diameter Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX MIXER/MILL® ACCESSORIES 46 Small Vials & Vial Sets & VialSmall Vials Mixer/Mill Accessories For useinthe5100Mixer/Mill, andwithadapters inthe8000Mand8000DMixer/Mills . *3111, 3116 and3116PCaccept balls. 3112 3/8in.(9.5mm) acrylic vial that includes a slip-on vial that includesa slip-on 12 mLpolycarbonate grinding balls. asabagof100vials. Sold x 50.8mm).Use 3112 or8006A diameter x2in.long(19.1mm polyethylene cap. Vial is 6133PC one cylinder, caps, and two slip-on 47.6 mm).Includesacenter x 17/8in.long(19.1mm 5 mLvialset. 3127 steel ball. andone¼in.(6.35mm) cap 25.4 mm).Includesaslip-on diameter x1in.long(12.7mm 2.5 mLgrindingvialset. 3117 100 vials. asabagof x 50.8mm).Sold diameter x2in.long(12.7mm polyethylene cap.Vial is 3116 and two 5/16in.(7.9mm)tungsten grindingballs. carbide center sixdisposablemethacrylate withtungsten caps inserts, cylinders carbide Delrin® 5 mLgrindingvialset. 5004 5 mL grinding vial with slip-on 5 mLgrindingvialwithslip-on Vial Set Vial Set as abagof100vials. long (12.7mmx25.4mm).Sold cap. Vial is 3111 includes a slip-on polyethylene includes aslip-on 2.5 mLgrindingvialthat 1 Hardened Tool Steel Hardened Tool Steel Polystyrene Vial in.(6.35mm)steel ball. Tungsten Vial Carbide-Lined Set Polystyrene Vial Polycarbonate Vial 1 in.diameter x1in. 3 in.diameter 3 1 3 1 in.diameter x21/8in.long(19.1mm54mm).Includestwo in. in. in. polyethylene cap. Vial is 6133 balls. asabagof100vials. Sold x 50.8mm).Use 3112 or8006A diameter x2in.long(19.1mm vial that includes a slip-on vial that includesa slip-on 12 mLpolystyrene grinding of 20. 5004 Vial inunits Set. Sold for SPEXSamplePrep cylinder; center methacrylate Disposable Cylinder 3120 5004C for wet or dry grinding.for wet ordry 3118A agate ball, beused can mm) long. Includesone1/4in. (22.2 mm)diameter x2in.(50.8 3.5 mLgrindingvialset. 7/8in. 5 mLgrindingvialwithslip- 100 vials. asabagof x 50.8mm).Sold diameter x2in.long(12.7mm on polyethylene cap. 3116PC stainless steel ball. andone cap x 25.4mm).Includesaslip-on diameter x1in.long(12.7mm 2.5 mLgrindingvial. 3114 Polystyrene Vial

AgateSet Vial Stainless Steel Stainless Vial Set Methacrylate CenterMethacrylate Polycarbonate Vial 1 in.(6.35mm) 1 1 in. in. 3 in. MIXER/MILL® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 47 in. 1 in. (5.7 cm) 1 Clamp for 8003 Vial Vial 8003 Clamp for Stainless Steel Vial SetVial Stainless Steel * Vial Polystyrene in. (12.7 mm) and four in. (12.7 mm) and four Tungsten Carbide Vial SetVial Carbide Tungsten Zirconia Vial Ceramic Round-Ended Hardened Hardened Round-Ended 1 in. (12.7 mm) and four in. (12.7 mm) and four in. (6.35 mm) stainless steel in. (6.35 mm) stainless steel 1 Set clamp permits slurryThis grinding in the 8003 Alumina Sold Set. Vial Grinding Ceramic in pairs. 8015 135 mL vial with plastic screw- 135 mL vial with x 2 ½ 2 1/8 in. diameter on cap., x 6.7 cm). Soldin. long (5.4 cm vials. as a bag of 100 8002 Set 2 ½ in.diameter 45 mL vial set. 11/16 in. long (6.35 cm x 6.8 x two cm). Includes 2 ½ in. zirconia corprene balls and seven ceramic gaskets. balls. 8005 8007 2 65 mL vial set, x 3 in. (7.62 cm) long. diameter O-ring, Includes screw-on cap, two 1 8004 55 mL vial set, 2 ¼ in. diameter x 2 ¼ in. diameter 55 mL vial set, 2 ½ in. long (5.7 cm x 6.35 cm). carbide-linedIncludes tungsten on tungsten screw- two body, carbide-lined 7/16 in. two caps, carbide balls (11.2 mm) tungsten gaskets. corprene and eight Steel Vial Steel Vial Set 2 3/8 in. diameter 35 mL vial set, x 3 in. long (6.0 cm x 7.62 cm). 1 O-ring, Includes 1 screw-on cap, 8009 2 balls. (6.35 mm) steel in. (12.7 mm) 1 Steel-Jacketed Steel-Jacketed Silicon Nitride Vial SetVial Silicon Nitride Methacrylate Vial SetVial Methacrylate Agate Vial Vial Set Agate Hardened Steel Vial Vial Steel Hardened Alumina Ceramic Vial SetVial Alumina Ceramic 8004SS Tungsten Carbide Vial SetVial Carbide Tungsten 2 ¼ in. diameter 55 mL vial set, x 2 ½ in. long (5.7 cm x 6.35 7/16 in.(11.2 cm). Includes two carbide balls and mm) tungsten Viton Gaskets. eight 8008 45 mL vial set, 2 ½ in. diameter x 2 ½ in. diameter 45 mL vial set, 2 11/16 in. long (6.35 cm x 6.8 cm). nitride Includes one solid silicon 8008A vial and slip-on two cap, ½ in. (12.7 Nitride Balls, Silicon gaskets. corprene mm) and seven 45 mL vial set, 2 ¼ in. diameter 2 ¼ in. diameter 45 mL vial set, x 2 ¾ in. long (4.7 cm x 7.0 cm). slip- two vial body, Includes agate 8014A agate two caps, on agate ½ in. (12.7 mm) and eight balls, gaskets. corprene 8014 two 8006A two 3112 3/8 in. (9.5 mm) and four methacrylate balls. 8006 55 mL vial set, 2 ½ in. diameter 2 ½ in. diameter 55 mL vial set, x 2 5/8 in. long (5.7 cm x 6.7 cm). gasket, corprene Includes seven Set 2 ¼ in. diameter 65 mL vial set. cm x 7.62 cm). x 3 in. long (5.7 includes a screw-on cap with and ½ in (12.7 mm) two O-ring, balls. steel ¼ in.(6.35 mm) four 8001 45 mL vial set. 2 ¼ in. diameter 2 ¼ in. diameter 45 mL vial set. x 2 ¾ in. long (5.7 cm x 7.0 cm). Includes 99.5% alumina ceramic slip-on two grinding vial, alumina one ½ in. (12.7 mm) caps, ceramic ball and eight alumina ceramic gaskets. corprene 8003 For use in 8000-series Mixer/Mills use in 8000-series For Accepts 3112 3/8 in. (9.5 mm) or 8006A ½ in. (12.7 mm) acrylic balls. *Accepts Large Vials Vials Large Vial & Sets Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX MIXER/MILL® ACCESSORIES 48 Grinding Media Grinding 6134 100 vials. grinding. asabagof Sold slurry for cm x7.62cm).Suitable in. diameter x3in.long(2.54 35mL vialwithattached cap,1 per set. and 3127 Vial Sets. Four balls diameter steel ball;for 3117 1/4 in.(6.35mm)inch Steel BallSet 3117B 3112 of 100. plastic vials. inunits Sold Fits allSPEXSamplePrep 3/8 in.(9.5mm)diameter. of 100. and 8006vials. inunits Sold Fit 6133,6134,6135,8002, 1/2 in.(12.7mm)diameter. Balls 8004 and8004SS Vial Sets. tungsten ballfor carbide 7/16 in.(11.2mm)diameter Ball and 8009vialsets. hardened steel ballsfor 8001 four 1/4 in.(6.35mm) Two 1/2in.(12.7mm)and 8006A 8004A 8001B 3119 of 100. plastic vials. inunits Sold Fit allSPEXSamplePrep 1/8 in.(3.2mm)diameter. Polyethylene Vial Methacrylate Balls Methacrylate Methacrylate Balls Methacrylate Hardened Tool

SteelBallSet Methacrylate Methacrylate Tungsten Carbide 8007 vialset. 440C stainlesssteel ballsfor 1/4 in.(6.35mm)hardened Two 1/2in.(12.7mm)andfour Set 8003A 3118A 8007B Vial Set. alumina ceramic ballfor 8003 1/2 in.(12.7mm)diameter agate ball;for 3120Vial Set. 1/4 in.(6.35mm)diameter per set. the 3114vialset. Four balls stainless steel ball;for (440C) 1/4 in.(6.35mm)diameter Ball Set 5004A 3114SB Vial Set. zirconia ceramic ballfor 8005 1 8005A Vial Set. Four ballsperset. tungsten ball;for carbide 5004 5/16 in.(7.9mm)diameter Ball Set as abagof100vials. long (3.81cmx7.62cm).Sold Vial is1 6135 75 mLvialwithattached cap. ⁄ 2 in.(12.7mm)diameter Polyethylene Vial AluminaCeramic Ball Agate Ball Tungsten Carbide Stainless SteelBall Stainless 1 Zirconia CeramicZirconia Ball Stainless Steel Stainless in.diameter x3in. MIXER/MILL® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 49

(Part no. 51714 51714 (Part no. Agate Ball Agate Multiple-Sample Adapter for 6134 vial Adapter Aluminum adapter for 6134 for adapter Aluminum use with the 8000M For vial. or 8000D 8016 8011 Adapter vials ¾ in. (19.1 mm) four Holds be used with Must in diameter. 3127 run with to 8012 Adapter vials in 8000D. 1/2 in. (12.7 mm) diameter mm) diameter 1/2 in. (12.7 set. 8014 vial ball for agate 8014A Prep-Aid Vertrel® XF Liquid fluorocarbon grinding aid. Prevents caking, caking, Prevents grinding aid. Liquid fluorocarbon grinding. after evaporates contamination, reduces One-quart bottle. Prep-Aid® Grinding Aids Prep-Aid® 3650 Silicon Ball Nitride

Multiple-Sample Adapter for 6135 vial for Adapter Vial Clamp Adapter for for Clamp Adapter Vial Adapter vials ½ in. (12.7 mm) seven Holds be used with Must in diameter. vials 1 in. run to 8012 Adapter (25.4 mm) long in 8000D Mixer/Mill. 8010 Aluminum adapter for 6135 for adapter Aluminum use with the 8000M For vial. or 8000D 8017 8008A 1/2 in. (12.7 mm) diameter mm) diameter 1/2 in. (12.7 8008 ball for nitride silicon vial set. the 8000D Mixer/Mill 8010 when running Required with vials 1 in. (25.4 mm) adapter in length (3111, 3114, 3117) or 3127 vials with when running in the 8000D. 8011 adapter 8012 Vial Adapters Vial Part no. 39322 optional gasket for 8004; Part no. 39515 optional gasket for 8003, 8005, 8008, 8014) 8003, 8005, 8008, for 39515 optional gasket 8004; Part for no. 39322 optional gasket Part no. and most other fluids. solvents, oils, to with good resistance and neoprene of cork - A combination Corprene XF. Vertrel® with Incompatible acids. and strong bases, strong solvents, organic are avoid Chemicals to for gasket 10010 standard 8003, 8005, 8008, 8014; Part for no. gasket 10009 standard (Part no. 8004SS) for 10010 optional gasket 8004 ; Part no. and alcohols, ketones, esters, phosphate to monomer with good resistance diene propylene EPDM - Ethylene for Recommended acids. fuel oils and strong hydrocarbons, aromatic are avoid to Chemicals most other fluids. 40004 optional gasket 8004, 8004SS; Part for no. optional gasket 40002 (Part no. XF. Vertrel® use with 8009) 8001, 8007, 51715 optional O-ring for 8003, 8005, 8008, 8014; Partfor no. range of chemicals. to a wide resistance excellent with fluoropolymer - Synthetic Teflon® A fluoroelastomer with good resistance to oils and most other fluids. Chemicals known to degrade to degrade known Chemicals to oils and most other fluids. resistance with good - A fluoroelastomer Viton® XF. Vertrel® with Incompatible acid. bases (NaOH) and acetic strong amines, esters, ethers, ketones, are Viton 8004SS; for gasket 39322 standard 8009; Part 8001, 8007, O-ring for no. 51746 standard (Part no. optional O-ring for 8001, 8007, 8009 vials) 8001, 8007, optional O-ring for Standard/Optional Gaskets and O-rings 8000 Series Mixer/ Standard/Optional for Mill Vials adapters enable simultaneous running of multiple samples in the 8000 Series Mixer/Mills. The 8010 The samples in the 8000 Series of multiple running enable simultaneous Mixer/Mills. Special adapters vials, and 3/4 in. (19.1 mm) diameter 1/2 in. (12.7 mm) and 8011 multiple-sample accommodate adapters respectively. Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX MIXER/MILL® TECHNICAL INFORMATION 50 Grinding Vial Sample Specifications Grinding Vial Sample Technical information for Mixer/Mill 6133PC 3116PC 8004SS 6133 8006 8002 6135 6134 3116 3111 8008 8005 3118 8003 8004 5004 3114 3117 8014 8007 3127 8009 8001 P/N Sample VolumeSample 0.5-1.0mL 0.2-0.6 mL 0.5-1.5 mL 0.2-0.6 mL 0.2-0.6 mL 3 –10mL Grinding 20-50 mL 3-10 mL 3-10 mL 2-8mL 2-8 mL 2-8 mL 2-8 mL 30 mL 20 mL 30 mL ------Typical Grinding Sample WeightSample Tungsten Carbide Alumina Ceramic Zirconia CeramicZirconia 0.5 g 0.5 g 0.5 g 10g 10 g 10 g 10 g 10 g 10 g 10 g 10 g 10 g Hardened Steel 1 g 1 g Stainless Steel Stainless Silicon Nitride Silicon ------Plastic Agate Blending Sample Volume 2.5 mL 20mL 15 mL 20 mL 40 mL 50 mL 20 mL 20 mL 25 mL 25 mL 20 mL 25 mL 25 mL 25 mL 5 mL 2 mL 5 mL 2 mL 1 mL 1 mL 1 mL 1 mL 2 mL Grinding orBlending Suitable for Slurry Suitable Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes No No No No No MIXER/MILL® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 2 51 50 Ni 50 Khorkounov, B., Gebert, A., Mickel, Ch., Schultz, L. Journal of Alloys Schultz, Ch., L. Journal of Alloys Gebert, Mickel, A., B., . Khorkounov, 7 Y 30 Ni 63 Effect and electrode of mechanical conditions on the microstructureevolution alloying characteristics of Mg Concas, A., Lai, N., Pisu, M., Cao, G. M., Cao, N., Pisu, A., Lai, Concas, Mixer/Mill. in Spex Modeling of comminution processes 3746-3760. 2006. pp. 11, June, 61, Issue: Vol. Science, Chemical Engineering S. J. L., McHenry, and planetary of the milling balls in shaker Takacs, mills. Temperature 5246 – 5249. 2006. pp. 16, August 41, Issue: Vol. Science, Journal of Materials Effect TiC-TiB synthesis and densification of ball milling on simultaneous spark plasma of 434, Vol. A, Science and Engineering Z.A. Materials G., Munir, R., Cao, A.M., Orru, Locci, composites. 23-29. 1-2, OctoberIssue: 25, 2006. pp. International Journal of K. International Gasan, H., Aybar, O., Celik, N., Nuri Aydinbeyli, amorphous alloy. 2266-2273. 2006. pp. 15, December, 31, Issue: Vol. Energy, Hydrogen Effect of the heating rate on crystallization behavior of mechanically alloyed Mg of mechanically on crystallization behavior alloyed rate Effect of the heating Over the years nearly one hundred articles have been published in refereed scientific journals journals scientific articles in refereed been published one hundred nearly have the years Over includes This mechanical alloying. and its use for Mixer/Mill the SPEX SamplePrep regarding other topics. and numerous of grinding vial materials, evaluations techniques, mechanical alloying are we that publications recent the more highlight to list is intended publication following The own your for the Mixer/Mill considering are If you be comprehensive. to of and is not intended aware applicable for search own do your to you encourage strongly we application, mechanical alloying and references. publications Mechanical alloying, also referred to as reactive milling, is a process originally developed for the for originally developed is a process milling, as reactive to also referred Mechanical alloying, used is often mechanical alloying Today, superalloys. dispersion strengthened production of oxide unique microstructures. with powders generates that technique processing powder as a solid-state the SPEX decades, the past few Over this. accomplish A high-energy mill can ball be used to the industryhas become for standard “SPEX Mill”, as the widely known Mixer/Mill, SamplePrep milling action, of the high energy and the durability of the The applications. mechanical alloying extended periods. for running allow motor, Mechanical Alloying Perez, R.J., Huang, B.-L., Crawford, P.J., Sharif, Sharif, P.J., Crawford, B.-L., Huang, R.J., Perez, of nanocrystallineSynthesis powders. Fe-B-Si 47-56. 1-2, January 7, Issue: 2, 1996. pp. Vol. Materials, Nanostructured E.J. A.A., Lavernia, Huang, B.-L., Perez, Perez, B.-L., Huang, mechanical solid solutions by alloying. of supersaturated Formation 1-2, January 7, Issue: 2, 1996. pp. Vol. Materials, Nanostructured M.J. Luton, E.J., Lavernia, R.J., 67-79. Materials Materials P.G. C., McCormick, S., Nishimura, Hwang, Mechanical milling of magnesium powder. 22–33. 2001. pp. 1-2, November, 318, Issue: Vol. A, Science and Engineering: Rojas, P., Ordonez, S., Ordonez, P., during mechanical and Ni. Rojas, of Mg Microstructural alloying evolution April 5, Issue: 1-2, 391, Vol. Compounds, and Alloys E. Journal of Lavernia, A., Zuniga, D., Serafini, 267-276. 2005. pp. A study of mechanical alloying processes using reactive milling and discrete element element A study of mechanical using reactive milling and discrete processes alloying 53, Issue: Vol. E.L. Acta R.N., Dreizin, Materialia, Schoenitz, M., Dave, W., Chen, T.S., Ward, modeling. 2909-2918. 2005. pp. 10, June, and Compounds, Vol. 416, Issue: 1-2, June 8, 2006. pp. 110-119. 1-2, June 416, Issue: 8, 2006. pp. Vol. and Compounds, Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX MIXER/MILL® TECHNICAL INFORMATION 52 MIXER/MILL 18 minutes in8001steel vialwith2steel balls. 11 grams ofred sandstone was ground inthe8000MMixer/Mill for Sandstone Red minutes in8001steel vialwith2steel balls. 11 grams ofgranite was ground inthe8000MMixer/Mill for 18 Granite The result was afinealmostsilky texture. lumpy powder. Itwas thenground intheShatterbox for 6mins. Ground inthe8000MMixer/Mill for 15mins. Resultwas aslightly Superalloy BEFORE BEFORE BEFORE ® BEFORE & AFTER SAMPLES AFTER AFTER AFTER MIXER/MILL® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 53 * * * * * * ** ** ** 83 50 98 82 38 10 50 94 95 84 91 39 50 20 30 35 90 92 97 75 86 97 100 100 100 100 100 100 100 100 % Passing 325 Mesh * 6 3 1 5 5 5 5 * 5 * 5 3 5 * 2 5 3 7 5 5 5 5 5 3 5 ** 15 25 10 10 15 10 20 10 10 12 15 26 Amount (g) Amount Polystyrene Vial Polystyrene * 5 * 2 5 2 5 ** 30 15 30 10 10 30 10 15 60 10 20 20 10 15 10 10 10 20 30 20 15 10 10 15 10 30 20 20 10 30 10 Time (min) Time L-D L-D L-D L-D PJ-D PJ-D HS-E AC-D AC-D AC-D AC-D PV-D HS-D HS-D HS-D Vial - Vial AC-W AC-W WC-D WC-D WC-D WC-D WC-D WC-D WC-D WC-D WC-D HS-W WC-D WC-D WC-D HS-W HS-W WC-W WC-W WC-W WC-W WC-W WC-W WC-W Method ------fluff Shot Piece Chips Chips Form Pieces Pieces Pieces Pieces Pieces Grains Grains Chunk Chunk Chunk Chunk Grains Lumps Chunks Chunks Chunks Chunks Chunks Chunks Powder 60 mesh 100 mesh 100 mesh 3mm Beads 6mm Lumps Fused Button Fused Porcelain Zirconium Carbide Zirconium Limonite Ore Limonite Wood Ilmenite Germanium Floor Tile Floor Welding Flux Welding Tungsten Transite Tungsten Carbide Tungsten Ferro Nb Ferro Tomato Stems Tomato Straw Ferro Cr Ferro Slag (open hearth)Slag (open Copper Chrome Ore Chrome Chromium Cobalt Slag (copper) Cement (Portland) Cement Slag (blast furnace) Brake Linings Brake Boron Carbide Boron (activated) Carbon Wax Carbnauba Silicon Silicon Bone Silica Silica Asbestos Bauxite Catalyst Reforming Sand Bismuth Potassium Pyrosulfate Potassium Material Antimony Table References: Table or trichloroethylene (water ground | W – Wet Vial Carbide – 8004 Tungsten | WC | L – 8006 Acrylic Vial Vial Steel HS – 8001 Hardened | PV – 6133 Vial – 8003 Ceramic | AC – Dry | D ground Vial – 8002 Polystyrene slurry) | PJ | **- Satisfactory extractions emission spectroscopy for or optical *- Suitable X-ray for Grinding Tests with 8000-series Mixer/Mills 8000-series with Tests Grinding Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX MIXER/MILL® TECHNICAL INFORMATION 54 1 selecting theproper application. containerselecting for aparticular elements, hardness, resistance to abrasion, durability, andefficiency. These are usuallythebasis for reviewsThis thekey ofeachgrindingcontainer chart properties material, includingmajorandminor Allreported lessthan0.02% Material Nitride Silicon Zirconia Steel Cr-Free Plastic Carbide Tungsten Agate Ceramic Alumina Steel Hardened Steel Stainless Elements W,C,Co Major Fe, Cr Fe, Fe Fe Al Zr Si Si C Element(s) Cr, C Mn, Si, Y, Al, Fe, Ca K, Ca,K, Mg Al, Na,Fe, Si, Ca,Si, Mg C, Mn, Si, Si, C, Mn, Ta,Nb Ti, Ni, Mn, Ni, Mn, Minor Mg,Hf S, Si Mo - 1 1 Rockwell:R45N Mohs: 5- Mohs: 5- Mohs: 5 Knoop: 1160 Mohs: 8 Mohs: 8 Knoop 1600 Knoop 1160 R45N 74-79 Mohs: 6-7 1400-1800 Rockwell:C Rockwell:C Rockwell:C Mohs: 1 Hardness Mohs: 8 Rockwell: 550-800 Mohs: 9 Knoop: Knoop: 74-79 55-60 55-60 60-65 1 1 1 / 2 / / 2 + 2 1 1 -6 + / / 2 2 1 1 / / 2 2 to Abrasion Extrememly Extrememly Resistance Extremely Extremely Very High Moderate Moderate Moderate High High High High Low Long-wearing, Long-wearing, Durability disposable Very long- Very long- Very long- subject to subject breakage wearing wearing wearing brittle High High High Low, Comparative Efficiency Very High Moderate Moderate Moderate Moderate grinding; blending High for Low for High High High MIXER/MILL® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 55 HT002: HOW TO GUIDELINE: MILLING & EXTRACTION / APPLICATION: CRUDE FAT CRUDE APPLICATION: EXTRACTION/ & MILLING GUIDELINE: TO HOW HT002: Evaporate the solvent on a steam-heated water bath under the hood. Place the beaker with residue with residue the beaker Place under the hood. bath water on a steam-heated solvent the Evaporate the Weigh in a desiccator. cool and beaker the and dry100 °C. Remove oven in the air at it 1 hour the dry calculate and beaker extract weight. Mix the sample thoroughly and weigh accurately about 4-5 g into the steel grinding vial. Add one Add grinding vial. the steel about 4-5 g into accurately and weigh Mix the sample thoroughly 15 for Seal the Mixer/Mill in mill and vial the n-hexane. of 25 mL and balls steel mm 6 two and 12mm the milled sample slurry paper in the funnel and filter and a clean a filter into Place vacuum mins. dry three of aid and the vial with milling cap steel the from oil residual the transfer flask. Quantitatively 10 mL portions three the sample with another oil from residual 10 mL portions and wash of hexane, Rinse 150 mL beaker. a dried and tared into miscella and oil hexane the filtered Transfer of hexane. with small portions the beaker of hexane. residue into flask the vacuum Feedstuffs Analysis – Crude Fat (Hexane Extractables) (Hexane Fat Crude – Analysis Feedstuffs extraction simultaneous milling and by in a sealed ball mill vial. with hexane recovered Lipids are the milling from derived components corn germ and other feedstuffs, method is applicable to The particle a uniform Grind a 50-100 g sample to (10 mesh) in a grinder or cuttingof corn. mill. size SP003: NANOTECHNOLOGY / APPLICATION: PRODUCTION OF NANO POWDERS PRODUCTION NANO OF APPLICATION: / NANOTECHNOLOGY SP003: The analyzed media were: Li2O, LiNbO3, LiBO2, B2O3, TiO2 and Li2O:B2O3 mixtures. The average average The and Li2O:B2O3 mixtures. TiO2 LiNbO3, LiBO2, B2O3, Li2O, media were: analyzed The means of X-ray by analyzed the grinding time and subsequently by particle determined was size materials containing The lithium (TEM). Electron Microscopy Transmission Diffraction and (XRD) its to with regard is interesting TiO2 use as solid electrolytes. selected because of their potential were filled in an argon vial was grinding the corundum materials hygroscopic For catalyst. use as a photo an airtight container. and put into stainless steel atmosphere Analyzing particle size effects in nanocrystalline materials requires a technique in which one technique in which can particleAnalyzing a effectsrequires in nanocrystalline size materials using a ball nano-crystallineadjust the particle In this study various produced size. were materials Ball vials). milling alumina and zirconia equipped with SPEX SamplePrep; mill (8000M Mixer/Mill®, large is particularly the grinding of a relatively use and allows this task as it is easy to suitable for materials. variety of different as a large as well of material amount Production of Nano-Crystalline Oxidized Ceramics with High- of Nano-CrystallineProduction Ceramics Oxidized Ball MillingEnergy The following are excerpts of application notes for the Mixer/Mill. To access our full library access and To the Mixer/Mill. for notes of application excerpts are following The visit www.spexsampleprep.com/appnotes. note application the complete download MIXER/MILL APPLICATION NOTES APPLICATION MIXER/MILL Grinding & Pulverizing

• 8500 ShatterBox® • 8530 ShatterBox®

THE SHATTERBOX® The ShatterBox is a ring & puck mill with soundproof enclosure that accommodates sample sizes ranging from 2 to 100 grams. Ideal for pulverizing dry, brittle samples and slurry grinding. It swings a dish-shaped grinding container, with a puck and (often) a ring inside, in a tight high speed circle. The sample is quickly crushed between the wall and floor of the container and the moving puck/ring grinding elements. Smaller grinding containers and those made with ceramics have a puck-shaped grinding element; larger containers have a ring and puck. Grinding containers are fitted with a gasket to prevent sample loss during grinding. The ShatterBox holds one large or three small grinding containers.

APPLICATIONS SAMPLE TYPES • Pharmaceuticals • Slag Rapid dry or wet grinding to • Ores • Ceramics analytical fineness of hard, brittle • Minerals • Dried Plant samples. • Rocks • Soil

TRY IT BEFORE YOU BUY IT! Demo and Sample Test Programs are available for this product. See pages 108-109 for more details

56 SHATTERBOX® Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 57 8530-115 8530-230 sampleprep For video, scan with video, For your smartyour phone or visit www.youtube.com/ 2 hp @ 835 RPM ⁄ 1 225 lbs. gross (102 kg) (102 gross 225 lbs. 3-prong grounded plug 115V, plug 115V, grounded 3-prong for cord European 60Hz. 2-prong 50 Hz. 230V, Part number: number: Part 4 5 Cam-action lever requires only moderate only moderate requires Cam-action lever the grinding dish secure to hand pressure and is adjustable for in the Shatterbox heights. of different containers in a dish-shaped grinding container Swings high-speed circle. a tight

4. 5. Cord Power Weight Weight Motor 3 2 19 in (48 cm) x 19 in (48 cm) x 40 in (102 cm) 115V/60Hz or 230V/50Hz Yes 1 Lockable casters enable easy movement of enable easy movement casters Lockable the mill. Lid locks down when mill is running. when mill is running. Lid locks down noise levels. reduces enclosure Soundproof Programmable, 10-minute electronic timer 10-minute Programmable, safe, environmentally and display with LCD switch. membrane push-button

Dimensions Voltage CE Approved Features & Specifications ShatterBox is a ring & puck mill with sound-proof enclosure. Accommodates sample sizes sample sizes Accommodates enclosure. is a ring & puck mill with sound-proof 8530 ShatterBox The brittle samples and slurry dry, grinding. pulverizing for Ideal 100 grams. 2 to from ranging 3. 2. 1. Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX SHATTERBOX® 58 and slurry grinding. and slurry accommodates samplesizes ranging from 2to 100grams. Ideal for pulverizing dry, brittlesamples 2. 1. The 8500 Features &Specifications Power Cord Dimensions Voltage

in atight high-speedcircle. Swings adish-shapedgrindingcontainer containers ofdifferent heights. in theShatterbox andisadjustablefor hand pressure to secure thegrindingdish leverCam-action requires onlymoderate ShatterBox isanunenclosedring&puckmillwithoutasoundproof enclosure that cm) x23 13 in.(33cm)xin.(33 3-prong grounded plug115V, 60Hz. 115V/60Hz 1 in.(60cm) 4 1 Motor Weight 4. 3.

2 not included. mount setofdrive andanextra belts. Timer Includes ananti-skid wood/rubber floor protects againstdust. for continuous operation, andarubber cover Perforated provides metalskirt ventilation 3 Part number:8500-115 1 135 lbs(61kg) ⁄ 2 hp@835RPM visit www.youtube.com/ your smart phoneor your smart For video, with scan sampleprep SHATTERBOX® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 59 Tungsten Carbide Tungsten Tungsten Carbide Tungsten Ceramic Zirconia Ceramic Small Grinding Container Includes puck, dish with O-ring x 6 in. diameter lid. and gasket (15.2 cm x 8 3.2 in. high, 13 lbs. Grinding load 15- cm, 6 kg). 170 mL. Volume 40 mL. 8506 Grinding Container 3.6 Includes puck, dish and lid. x 2.3 in. high, 7.7 in. diameter x 5.9 cm, 3.5 kg). (9.2 cm lbs. Volume Grinding load 2-20 mL. with 8507R rack. 80 mL. Used 8508 8504 Grinding Container Grinding O-ring dish, Includes puck, ring, 6.9 in. diameter and lid. gasket cm x (17.5 29 lbs. x 3.2 in. high, Grinding load 20- 8 cm, 12.5 kg). 240 mL. Volume 60 mL. Rack 8507R Holds one or three 8507 or 8508 grinding containers in Shatterbox. in Shatterbox. 8507 or 8508 grinding containers one or three Holds and or out of Shatterbox, lift Rack has handles to into Rack base plate grinding containers. positioning one or three pins for locating four and holds grinding containers clamp, Shatterbox to Rack lid is matched grinding 8507R RackWhen is used with three during operation. down either 8507 or 8508. should be the same kind, all three containers, Small Steel Hardened Prep-Aid Vertrel® XF Alumina Ceramic Alumina Ceramic Hardened Steel Grinding Steel Grinding Hardened Large Hardened Steel Large Hardened Liquid fluorocarbon grinding Liquid fluorocarbon reduces caking, Prevents aid. after evaporates contamination, One-quartgrinding. bottle. 3650 Grinding Container dish with Includes puck, ring, 8 in. and lid. O-ring gasket x 3.3 in. high, 29 lbs. diameter Volume (20.3 cm x 8.2 cm, 13 kg). 650 mL. Grinding load 30-100 mL. 8521 8507 Grinding Container Includes puck, dish with gasket, x 2.3 in in. diameter 3.6 and lid. (9 cm x 5.4 cm, 1.9 high, 4 lbs. 90 mL. Grinding load Volume kg). with 8507R rack. 2-20 mL. Used 8505 8501 Grinding Container Includes puck, dish with O-ring x 6.3 in. diameter lid. and gasket (15.2 cm x 8 3.2 in. high, 11 lbs. Grinding load 15- cm, 5 kg). 170 mL. Volume 40 mL. Container O-ring dish, Includes puck, ring, 6.9 in. diameter and lid. gasket (17.5 cm 17.5 lbs. x 2.9 in. high, Grinding load is x 7.5 cm, 8 kg). 270 mL. Volume 20-50 mL. Grinding Aids & Sample Grinding Aids Binders ® Prep-Aid Racks and Holders Grinding Containers Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX SHATTERBOX® TECHNICAL INFORMATION 60 *Sodium alkylarylsulfonate added, alkylarylsulfonate *Sodium 5%**Household detergent (Tide)added, 10% Grinding Tests Containers withthe8501and8504Grinding ContainersSuitable Grinding Number Oil Shale Oil Insulation Graphite Mineral Fiber Glass (synthetic)Garnet Fluorite Fiberglass Ferro-titanium Ferro-silicon Ferro-niobium Slag, blastfurnace Ferro-molybdenum Sand Iron Powder Ferro-manganese Phosphate, raw mix Pesticide Ferro-chromium Material (Portland raw mix) Cement Asbestos 8521 8507 8501 8506 8505 8508 8504 Part Part Tungsten Carbide Tungsten Carbide Alumina Ceramic Zirconia Ceramic Hardened Steel Hardened Steel Hardened Steel Material >100 mesh >200 mesh <100 mesh >100 mesh Thin sheets <80 mesh <80 mesh <80 mesh <80 mesh <10 mesh <80 mesh <60 mesh >60 mesh Received Fiborous Form as Chunks Chunks 6.4mm Chunks Fiber Fiber 30-100 mL 20-50 mL 15-40 mL 15-40 mL 20-60 mL Volume Sample 5-20 mL 5-20 mL (min) Time 2.5 2.5 10 15 12 4 2 6 2 3 2 6 4 3 1 4 6 3 3 5 Amount Typical Sample 200 100 19* 40* 8501 (g) 15 15 35 50 10 25 25 25 25 25 40 25 50 20 5 6 Weight 15 g 50 g 40 g 40 g 15 g 50 g 90 g 325 mesh Passing 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 15 68 % Suitable for Suitable Blending (min) Time Yes Yes Yes Yes Yes Yes Yes 10 2 2 4 ------Amount 8504 200 100 (g) 35 15 Slurry Grinding Slurry ------Suitable for Suitable Yes Yes Yes Yes Yes Yes Yes 325 mesh Passing 100 100 100 96 % ------SHATTERBOX® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 61 using the same the same using ® AFTER AFTER AFTER AFTER BEFORE & AFTER SAMPLES AFTER & BEFORE ® BEFORE BEFORE BEFORE BEFORE Glass Sandstone Garnet-bearing rock Zinc Ore The following samples were ground in the Shatterbox in the were ground samples The following protocol. protocol. 1/4 inch chunks to approximately 1. Crush sample grinding dish 8501 hardened steel grams of sample in 2. Add 30 for 3 minutes. Shatterbox 3. Run the SHATTERBOX Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX SHATTERBOX® TECHNICAL INFORMATION 62 samples can bereducedsamples can below 10microns. sizeresultant well particle below 200mesh(approximately 50microns). With grindingaids, smaller ring againstthecontainer floor.Grinding timesare two usuallybetween andfive minutes, with the container, reduced andring, puck, ofthepuckand by andfurther themillstone-like action elements swingfree insidethecontainer, thesampleisrapidly crushed between thewalls of Inside thecontainer are the sample, and(inmostcontainers) apuck, aring. thesegrinding As The Shatterbox swingsadish-shapedgrinding container inatight, high-speedhorizontal circle. Grinding Action a 150mLcapacity. This corresponds samplesize to of75-100grams. atypical size of10grams. An oversize steel grindingcontainer (8521)isalsoavailable andhasapproximately containers have ofthestandardcapacity thesample grinding typical aboutafifth containers anda berun(8508), whichcan eitheroneorthree at atimewiththe8507RRack. These grinding There are alsosmallgrindingcontainers madeofhardened steel (8507)andtungsten carbide container becomes more tightly packed. for aslittle as4grams andasmuch100grams. However, decreases asthe grindingefficiency ofthecontainers ismuchhigher,capacity and(for example) thesteel container hasbeenused and tungsten containers carbide and30grams for theceramic containers. Note that theactual (8506). Typical grindingloadsfor samplessuchascement, rock, orslagare 50grams for thesteel hardened steel (8501),tungsten (8504),alumina ceramic carbide (8505),andzirconia ceramic The standard grindingcontainers, withanominalvolume ofabout100mL,are available in Grinding Containers minimizing noiseandmaximizingsafety. environment requires arugged, simplemill. The 8530Shatterbox isidealfor labsconcerned with and steel millswithopen,noisylabconditions andisstillusedinmany locations where theworking The originalSPEXSamplePrep swingmill, the8500Shatterbox, was developed for cement plants for hundreds ofothermaterials includingsulfurpellets, driedmarsh-grass, andpharmaceuticals. Shatterboxes grindcement mix,rocks, typically slags, soils, ceramics, andores, buthave beenused Applications the 8530butwithouttimerandcabinet. 8530 Enclosed Shatterbox, as andtheoriginal8500,whichoffers thesamegrindingperformance 100 grams of brittlematerial to fineness. analytical There aretwo Shatterbox models, thefull-sized, popular “swing mill” intheUnited States. Now asthen,itisthemostefficient way topulverize up to Since itsintroduction over years ago, fifty SamplePrep theSPEX Shatterbox hasbecome themost Shatterbox TechnicalInformation 60 Years of Support to the Environmental Community Manufacturing Organic and Inorganic Certified Reference Materials

Quick turnaround based on your individual needs QuEChERS Kits & Internal Standards – Custom Kits also available LC/MS Single & Custom Standards New Inorganic Multi-Element Standards for the latest EPA methods Custom Blends & Daily Checks

MARKETS SERVED: Environmental • Industrial • Pharmaceutical • Consumer Safety • Academia • Food & Agriculture

For more information, contact us at: [email protected] www.spexcertiprep.com

63 Pressing & Pelletizing

3636

• 3636 X-Press®

THE X-PRESS® The 3636 X-Press is a 35-ton (31.8 metric ton) hydraulic laboratory pellet press that accepts 13 mm, 31 mm, 35 mm, and 40 mm pellet die sets. This automated laboratory press is created to press sample pellets for spec- troscopy. It is programmable, so that repetitive pellet preparations may be carried out with minimum operator workload and a maximum of uniformity. The X-Press can also be operated manually.

APPLICATIONS SAMPLE TYPES Pressing sample pellets for XRF/IR • Pharmaceuticals • Rocks • Cement • Slag • Minerals • Soil

TRY IT BEFORE YOU BUY IT! Demo and Sample Test Programs are available for this product. See pages 108-109 for more details

64 X-PRESS® Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 65 6 363 3636-230 sampleprep For video, scan with video, For your smartyour phone or visit www.youtube.com/ Adjustable 2.0 to 6.0 inches 2.0 to Adjustable 15 cm) (5 to 1.0 inch (2.5 cm) (8 cm) 3.25 inches diameter 3-prong grounded plug 115V, plug 115V, grounded 3-prong cord European 60Hz. 2-prong 50 Hz. 230V, for 1/3 hp Part number: 3636-115 number: Part 6 7 Manual pressure relief valve used to release the release used to valve relief Manual pressure in an emergency or pressure system hydraulic maintenance. system for Handle and handwheel moves the adjustment the adjustment Handle and handwheel moves the sample. secure to screw fill the oil to panel can be removed Access or check the oil level. reservoir

5 7. 5. 6. Daylight size Platen Cord Power Platen Movement Platen Motor Motor 2 in. (82 cm) ⁄ 1 4 3 121 Ibs. net (55 kg) 121 Ibs. 10–35 tons ram pressure pressure ram 10–35 tons or (9.1-31.8 metric tons 20,000 – 70,000 Ibs.) 23 in. (58 cm) x 11 in. (28 cm) x 32 1 Yes 115V/60Hz or 230V/50Hz 2 press that is automated and programmable. and programmable. is automated that laboratory press (31.8 metric ton) is a 35-ton Press Platen where die with sample is placed. where Platen enter user to allows display Touch-screen and release hold time, maximum pressure, start runs, press, and stop automated time for or select manual mode. Adjustment screw secures the loaded sample the loaded sample secures screw Adjustment the platen. of on top die placed Safety door and interlock with automatic Safety with automatic door and interlock pump shut-offvalve. safety

Force CE Approved Weight Dimensions Voltage Features & Specifications 3. 4. 2. 1. XRF, IR, and other analytical methods. Typical Typical IR, and other analytical methods. XRF, for of sample pellets pressing repetitive It is ideal for or less. minutes time is two pressing The 3636 X- The Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX X-PRESS® 66 CARVER CARVER Part number:3626 Part number:3621 Soils, Ceramics,Pharmaceuticals. extraordinary durability.Typicalsamplesinclude:Cement,Rocks,Minerals, for labswithasmallsampleload.Rugged,reliableandnotedtheir the mostprimitiveconditions.Economicalalternativetomotorizedpresses These manualhydrauliclaboratorypelletpresses Ideal for pressing samplepelletsfor IR.CEApproved. press that accepts 13mmpelletdiesets. Manuallycontrolled. topBench 12-ton (10.9metric ton) hydraulic pellet laboratory XRF, techniques. IR,andotheranalytical CEApproved. die sets. Manuallycontrolled. Ideal for pressing samplepelletsfor that accepts 10mm,133135 and40mmpellet Full-size 12-ton (10.9metricton) hydraulic pellet laboratory IR, and other analytical techniques.IR, andotheranalytical CEApproved.d. sets. Manuallycontrolled. Ideal for pressing samplepelletsfor XRF, that accepts 10mm,133135and40mmpelletdie Full-size 25-ton (22.7metricton) hydraulic pellet laboratory Part number:3622 MANUAL PRESSES 36 36 21 26 press press can beoperatedunder X-PRESS® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 67 Die Set – 35 mm Die Set – 13 mm DIE SET DIE Includes evacuable die body, die body, Includes evacuable 35 mm two plunger, base, O-ring pellets, polished steel seals knock-out ring vacuum sample disk extraction. for Load (45.4 metric tons). limit 50 tons Includes evacuable die body, die body, Includes evacuable 13 mm two plunger, base, O-ring pellets, polished steel knock-out ring seals, vacuum sample disk extraction. for Load (9.1 metric tons). limit 10 tons 3613 3616 For 3613 die, sold in pairs. 3613 die, For sold in pairs. 3623 die, For sold in pairs. 3623 die, For sold in pairs. 3616 die, For sold in pairs. 3616 die, For sold in pairs. 3614 die, For sold in pairs. 3614 die, For Replacement or spare steel pellets for die operation can be die operation pellets for steel or spare Replacement materials, of abrasive pressing routine For separately. purchased 31 mm, 35 mm and 40 mm tungsten offers SPEX SamplePrep polished steel for carbide pellets which can be substituted than steel, much harder carbide pellets are Tungsten pellets. All against breakage. not guaranteed and are brittle, but more sold in pairs. pellets are replacement Die Set – 40 mm Die Set – 10 mm Die Set – 31 mm Includes evacuable die body, die body, Includes evacuable 40 mm two plunger, base, O-ring pellets, polished steel knock-out ring for seals, vacuum sample disk extraction. limit Load (45.4 metric tons). 50 tons Includes evacuable die body, die body, Includes evacuable 10 mm two plunger, base, O-ring pellets, polished steel for knock-out ring seals, vacuum sample disk extraction. limit Load (4.5 metric tons). 5 tons 3614 3610 Includes evacuable die body, die body, Includes evacuable 31 mm two plunger, base, O-ring pellets, polished steel knock-out ring seals, vacuum sample disk extraction. for Load (45.4 metric tons). limit 50 tons 3623 Tungsten Carbide Pellets – 40 mm Carbide Pellets Tungsten PELLETS 3623ST Steel Pellets – 31 mm Pellets 3623ST Steel - 31 mm Carbide Pellets Tungsten 3623C – 35 mm Pellets 3616ST Steel – 35 mm Carbide Pellets Tungsten 3616C – 40 mm Pellets 3614ST Steel 3614C 3613ST Steel Pellets – 13 mm Pellets 3613ST Steel Replacement Pellets Replacement SPEX SamplePrep dies are designed to fit all SPEX SamplePrep presses, and they are equally equally are and they presses, fit all SPEX SamplePrep to designed dies are SPEX SamplePrep dies. using stand-alone laboratory presses other standard with compatible Pellet Die Sets Pellet Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX X-PRESS® ACCESSORIES 68 analyte. These bepurchased setscan separately ortogether withourdiesat adiscount. layer ofsample. Makes sturdy disks, prevents damageto die;idealfor smalleramounts (<1g)of setsallow Sleeve-and-Plunger easypreparationOur a ofXRFdiskswithbindermatrix supporting Sleeve and plunger sets SEE PAGES 90 AND 91 FOR DETAILS ABOUT THESE PRODUCTS. PrepAid® Binders more easilyhandled, marked, andstored thanuncladdisks. pellet. Thus reinforced, sampledisksare resistant to chippingandbreaking, andare other analyticaltechniques. The forms Spec-Cap thebottom and sidesofthefinished routinely ofpressed usedintheproduction powder sampledisksfor OES,XRF, and SPEX SamplePrep® are Spec-Caps® shallow, thin-walled aluminumcupswhichare Spec-Caps® Aid Sample Binder.Aid Sample Evacuable Pellet dieandPrep- Used with3623,31mm and PlungerSet 3623W 3614W Aid Sample Binder Aid Sample Evacuable Pellet andPrep- Die Used with3614,40mm and PlungerSet 31mm Die Sleeve 31mmDie 40mm Die Sleeve40mm Die sample disks. Plunger Set. Will bond200-250disksorprovide matrix for 25-35supported orusedundilutedform XRFsampledisk, assamplematrix withSleeve-and- SPEX PrepAid beblendedwithsampleat binderscan 10%by weight to Aid Sample Binder.Aid Sample Evacuable Pellet andPrep- Die Used with3616,35mm and PlungerSet 3616W 35 mm Die Sleeve 35mmDie X-PRESS® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 69 laboratory presses, pellet laboratory presses, X-Cell), compression of the compression X-Cell), pelletizing accessories are sophisticated sophisticated are pelletizing accessories Press There are many different procedures for preparing powdered samples for XRF analysis. Typically, Typically, for XRF analysis. samples powdered for preparing procedures different many are There to obtain enough then split quantity of the sample is first pulverized, a representative however, is blended with a binder if powder That 10 grams. an XRF sample disk, for usually 6 to powder a sample disk into be pressed to or without a Spec-Cap) in a pellet die (with and placed necessary, in This disk is then placed surface. compositionally uniform and has a flat, which will hold together the sample holder of the XRF spectrometer. powder in a pellet die yields a denser, flatter surface that provides greater analytical accuracy and greater surface provides flatter that in a pellet die yields a denser, powder length XRF. wave especially for sensitivity, Preparing Powder Samples XRF for Powder Preparing form to be in a homogeneous powdered the sample spectrometryrequires fluorescence often X-ray on the window the powder spreading by with a planar surface. this can Although be accomplished for liquid samples (such as a SPEX cell designed SamplePrep film of a While methods and mills for pulverizing are as varied as the samples themselves, pellet pressing pellet pressing as the samples themselves, as varied are pulverizing methods and mills for While and dies, presses, SPEX SamplePrep simpler tools. requires ensure dies and presses SPEX SamplePrep virtue is a cardinal Reproducibility in sample preparation. the sample or analytical technique. whatever sample disks, production of uniform For preparation of pellet samples, SPEX SamplePrep offers a full range of a full offers SPEX SamplePrep of pellet samples, preparation For SamplePrep-Carver SPEX and 25-ton manual include a 12-ton Presses and die accessories. die sets, of sizes in the standard available dies are Pellet X-Press. 3636 Automated and the 35-ton presses and form to include: aluminum Spec-Caps 10 mm,13 mm, 31 mm, 35 mm, and 40 mm. Accessories as SPEX as well binders, Prep-Aid and paraffin cellulose 31 mm, 35 mm, 40 mm pellets; protect thin layer sample pellets with a form and Sleeve-and-Plunger UltraBind; sets to own SamplePrep’s of sample on a binder matrix. in design, but functionally simple and very effective. XRF sample disks is dependent on the size of the spectrometer sample holder, sample holder, of the spectrometer on the size of XRF sample disks is dependent diameter The a binder or Spec-Cap require XRF disks do not larger. mm, 35 mm, 40 mm, or even be 31 which may The or both. use a binder or a Spec-Cap but most analysts under pressure, if the sample coheres XRF binders include impurities. it does not contribute is that an XRF binder for prime requirement proprietary products and polyvinyl with graphite, alcohol, orthoboric acid, paraffin, cellulose, Ultrabind. e.g. special properties, The following how-to suggestions apply chiefly to XRF sample preparation, but the basic principles preparation, to XRF sample suggestions apply chiefly how-to following The the are differences major The IR, etc. spark ablation, OES, the same for disks are sample of forming and across 13 mm IR disks are of the binders or additives. and the nature of the disks, diameters sample blended in; no Spec- (KBr) pulverized with the bromide potassium of pure largely consist OES and spark light. infrared transmit to as the sample disk must be able is used, Cap-type jacket Asthe disk must be electrically use 31 mm disks. these for generally conductive systems ablation in pressed and often blended with 50% pelletizing-grade graphite, most samples are techniques, an aluminum Spec-Cap. Pressing & Pelletizing Pelletizing & Pressing of in the form samples require and IR often OES, XRF, such as methods spectroscopic Analytical to section (refer melt, a fusion Although sample disks can be flat-surfacedcast from disks. round, and are beginning in Section Products as a powder begin 4), they often on Fusion 2, Chapter shape in a pellet die. to pressed Technical Information for the X- the for Information Technical Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX X-PRESS® TECHNICAL INFORMATION 70 changing the particle size shouldhavechanging theparticle littleornoeffect. sizes. B, Incase since theaverage penetration depthcovers of many components, many particles fluorescent intensity. This results from thefillingof voids by components withsmaller particle wouldlarge andachangeinthesize have particles, oftheseparticles onthe asubstantial effect page. A,theaverage Incase penetration oftheX-ray isofthesameorder ofmagnitudeasthe from different sample components approach stable values. This isshown graphically onthenext size becomes smallrelative particle As to thickness, thecritical fluorescence intensities emitted orinfinitecritical thickness. penetratecan andresult influorescence emitted from thesample. called the This depthisusually by thematrix.whole orinpart, Hence there isalimitto thedepthto whichtheexisting radiation withinthematrix absorbsradiation,a particle theresulting fluorescence isalsoabsorbed, in anX-rayAs enters apelletized sampledisktheexciting radiation isabsorbedby thematrix. When the intensities stabilize. on theirrelative absorptioncoefficients. Fortunately, size becomes smallenough, whentheparticle of bothcomponents isdecreased, theirrespective intensities may increase ordecrease depending yield ahigherintensity relative to thecomponent size. offixed particle Further, size iftheparticle By thesamereasoning, size ofonetwo samplecomponents asthe particle isdecreased, it will sample isdecreased. This isdueto inthesize thereduction andextent ofthevoids inthesample. years that theX-ray fluorescence intensity from size asamplewillincrease of the astheparticle It isimpossibleto say apriorihow fine to pulverize agiven sample. Ithasbeen known for many Effects Size Particle your chosenprocedure results inaccurate, reproducible data. requirements.analytical Runningaseriesofstandards orknown sampleswillhelpto confirm that andmustbeworkeddetails may vary outby theanalystto suithisorhersamples, equipment, and and what pressure to use, whetherto includeabinderorpress thediskinaSpec-Cap, allthese and theamount ofsampleto beground, ofmillandthegrindingtime, thetype what size ofdie In theend, procedure anexact mustbedeveloped ofsample. for eachtype The samplingmethod set, usedwiththeappropriate pelletdie, makes thisprocedure easy. incorporates athinlayer ofsampleonadiskbinder. The SPEXSamplePrep Sleeve-and-Plunger An alternate useful whenonlyasmallamount ofsampleisavailable, technique, particularly X-PRESS® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 71 Binders when properly Binders when properly Prep-Aid binders. Prep-Aid is Pressing SamplePressing Disks a mixture of often powder, quantity of homogeneous need a sufficient a sample disk, you make To including two binder; a pellet die set, and an appropriate material sample pulverized thoroughly and a the sample powder; sandwiching for smooth material or other hard, pellets of polished steel optional aluminum cup An such as the on the powder. exerting machine for the necessary pressure and samples during pressing, against abrasive bore the die protects the powder, contains Spec-Cap which yields technique, alternate An or breaking. the pellet against chipping protects subsequently the use of a sleeve- involves of sample on one side, disk of solid binder with a thin layer a durable and-plunger set with a pellet die. If the pulverized must be fine-grained case. in any be pressed to and homogeneous, powder The be necessary disk, it may add to cohesive a stable, into compressed is not readily sample material A binder can be uniformly or UltraBind. paraffin, such as cellulose, a binding/ briquetting agent of sample. a thin layer for blended with the sample or used as a backing distorting it from or analytical accuracyused enhance stabilizing the sample disk and keeping by during analysis and/ or storage. crumbling the analytical surface but also of the disk is not only flat XRF, for In an ideal sample disk pressed was whether the sample is true This of the original sample. representative and truly uniform, in a thin or pressed pressing, blended with a binder before Spec-Cap, without binder in a pressed by the use sample disks can be ensured and uniform stable, flat, Compact, on a binder matrix. layer and accessories, presses, dies, SPEX SamplePrep of reliable a fairly intricate in all its details, XRF analysis is, disks for into of powders the pressing While of follows A review analytical results. reliable yield consistent, to it can be routinized exercise, and anti-sticking binders, in the actual (pellet dies, pressing involved and tools the processes it is sampled (so that has been properly the analyte discussion that assumes The etc.). agents, particle minimize effects). (to size pulverized and adequately representative) In practice, the limiting particle size is often determined empirically by grinding the sample for a grinding the sample for limiting particle the empirically by In practice, determined is often size longer at then repeating measuring the particle analyzing the sample, length of time, given size, laboratory offers mills and SPEX SamplePrep a plateau. reach the intensities grinding times until procedure. this ideal for are grinding vials that Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX X-PRESS® TECHNICAL INFORMATION 72 good condition. evacuating adie, itisadvisableto make sure boththeupperandlower are O-rings inplace andin and quality.disk compaction Troublesome sampleswilloften benefitfrom this technique. When during pressing, thewithdrawal butinfact ofairandmoisture from improve thesamplecan out oftheKBr. MostXRFanalystsdonotbotherto evacuate their31mm,35mmor40dies to produce disksfor KBr infrared spectrometry, to draw theuseofavacuum isnecessary moisture of13 mmdies, Inthecase ofthe sampledisk. whichare anduniformity stability primarilyused contain gases, moisture, andpore space, the andremoval affect infact ofthesecan orreduction vacuum pumpto behooked upto thediebefore andduringapressing operation. Mostsamples All SPEXSamplePrep evacuable pelletdieshave avacuum hoseattachment, whichenablesa The Use ofthe Vacuum inPellet Pressing sample disks(andhence results) oftheanalytical willinevitablybegreater. programmed in, andwillremain thesame, sampleafter sample. The overall ofthe uniformity of the3636X-Press isthat lengthy holdtimesandprecisely controlled pressure release be can good ideato dumppressure abruptly inany pelletizingprocedure. Another significant advantage with manualpresses, asthepressure release control isoften notsensitive, butitisstillnever a well, several minutes may beappropriate. Aslow, careful bedifficult bleedperiodcan to accomplish holding time. Aminimumbleedtimeof15seconds isrecommended. For samplesthat donotbind A gradual release ofpressure after theholdperiodisperhapseven thanprolonged more important holding period. Automated X-Press isthat itturnsonthepump ifthepressure drops more than1ton duringthe holding timethepressure shouldbemaintained aswell aspossible. An advantage ofthe3636 at least30seconds isrecommended. analystsholdpressure Some for 5minutes ormore. During completely penetrate thesample, orfor otherreasons. Aholdingtimeat maximumpressure of may bedueto elasticrebound ofgasestrapped inthesample, abindermay because take time to pressure, andthepressure isabruptly released, thesamplediskoften doesnotholdtogether. This Holding timeandbleedare Ifasampleissimplybrought bothimportant. to maximum increases accuracy. analytical analysis ofmostelements, amatter ofmicrons, ofthesampledecreases compaction pore space and pressures, butuniform highpressure isrecommended. As “infinite depth” shallow for XRF is very 22 to 30tons; from andfor a40mmdisk, 25to 35tons. samplescohere Some adequately at low a sampledisk. Typical pressures for a31mmdiskare from 20to 25tons; from for a35mmdisk, usually have ofthepress loadlimitshigherthaneitherthecapacity orthepressure required to form die. The 13mmdiehasa10-ton limit, sosomecare mustbeexercised, but31mmandlarger dies the nature ofthesample. Obviously maximumpressures shouldnotexceed theloadlimitsof The maximumpressure for agiven taskvaries considerably, dependingonthesize ofthedieand lengthoftime, andthenreleasingcertain it, preferably slowly. A basicpressing sequence consists ofraising thepressure to aspecificlevel, holdingitthere for a X- offers 12-ton manualpresses and25-tonSamplePrep-Carver SPEX andthe35-ton 3636 Automated Manualandmotorizedsample disk. hydraulic presses are available for thistask:SPEXSamplePrep is raised to alevel that to thesampleorsample/bindermixture willcause cohere into astable In pressing samplesfor XRF, theloadedpelletdieisplaced inahydraulic Technique Disk for Pressing aSample Press. Any SPEXSamplePrep pelletdiewillfitthesepresses. press, andthepressure X-PRESS® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 73 The SPEX SamplePrep evacuable pellet die is a precision tool which must be handled carefully and which must be handled carefully tool precision pellet die is a evacuable SPEX SamplePrep The in design and function very Although such dies are operation. proper for maintained diligently A pellet die and easily jeopardized. partsworking necessary, fit of the is absolutely precise simple, difficulty; thousands of sample disks without a damaged or heavily will produce in good condition damage Any sample disks. and chipped or broken delays, frustration, produce to die is likely worn immediately. of a pellet die should be corrected or the bore the polished pellets to the die bore the polished pellets should pass smoothly through condition, In a pellet die in proper around “leak” sample will not the pulverized that but their fit should be so precise without binding, port seal the evacuation with a and base, assemble the die bore is to A good test the pellet edges. at or near the remain It should a polished pellet (polished side up) in the bore. and place fingertip, the of the air inside compression due to lightly, pushed down and spring back when of the bore, top the of the bottom smoothly to port the pellet should drop the evacuation When is unsealed, die. port it is either a loose fit, with the evacuation sealed, If the polished pellet sinks immediately bore. the die body and base is damaged. or the seal between will a sample powder and sharp edges so that close tolerances made with pellets are Polished (When the sample disk this happens, the pellet and the bore. the gap between into “feather” not remove to be difficult lip and the disk and upper polished pellet may crumbly a raised, have may part far the most vulnerable by as they can of a die, edges of these pellets are The the die). from surface. are a short Such a hard dents them even onto distance dropping or chipped by be dented bind in the only can cause they Not the pellets to the die. of the integrity to dangerous extremely edge of the pellet can spall off. the stressed of pelletizing, under the high pressures but also, die, jamming the and potentially scarring it deeply, bore, the through can chip be dragged resulting The the die. plunger and ruining with a fine- corrected should be immediately the polished pellets and die bore Minor damage to the die this the pellet will still pass smoothly through If after 600 grit) emery paper. (e.g. grained (A in service.continue the pellet and die can chipped, and its leading edge is not significantly bore, making chip, the left by the space into as sample can wedge badly chipped pellet should be retired, occur under In addition, further to to from the die. it difficult extract the pellet chipping is likely in use. can continue smoothed, properly die bore, scarred A lightly pressure). not affect the but will probably of the pellet should also be avoided, the polished face Damage to of 20–30 microns on the order Scratches functioning Analytical accuracy suffers. of the die. is what can of the polished pellet face abrasion can cause shielding effects in the sample disk,overall and very X-ray change the geometry between slightly in the critical relationship and distance Care and Maintenance of the SPEX SamplePrep Evacuable Pellet Die of the SPEX SamplePrepCare and Maintenance Pellet Evacuable Most evacuable pellet dies operate in the same way, by pressing the analytical sample between the analytical between sample pressing by way, in the same operate pellet dies Most evacuable assemble die is to loading the of way simplest The carbide. tungsten or steel pellets of polished two pour bore; the into side up, polished base; insert and die pellet, polished barrel the die the lower then down; polished side the upper polished pellet, and add it, level the bore, the sample into if the sample well works approach This die in the press. the assembled and place insert the plunger, it Once the sample disk is pressed, nor adhesive. abrasive and is neither under pressure well coheres use of the knock-out ring hand or with the either by die, the it from remove easy to should be fairly die. each SPEX SamplePrep supplied with it, die or scratches the or sticks to pressing, after well does not hold together the sample When Sleeve- binders, Prep-Aid Spec-Caps, include These pelletizing aids available. various are there and technique, application has its proper Each agents. anti-sticking and various and-Plunger sets, in this Chapter. detailed later Set-Up and Loading of the SPEX SamplePrep Evacuable Pellet Die Set-Up SamplePrepthe SPEX of Pellet Loading and Evacuable Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX X-PRESS® TECHNICAL INFORMATION 74 the sample weight will vary with the density ofthesample andthesize butthegeneralthe sample weight withthedensity ofthedisk, willvary sample isadded, thetop ofthesamplediskandedge Spec-Cap willcoincide. Obviously pressing,During thesample powder isforced insidetheSpec-Cap. When theproper amount of Then thesampleispoured into thedie, withthe upperpolishedpelletandtheplunger following. flaredSpec-Cap pusheddown against that lower pellet. this technique thediebore andbase are assembled, thelower andthe polishedpelletinserted, by theuserwith3625Edge-Flaring Tool, andthe3619ASpec-Cap isflared at thefactory. With 3617 Spec-Caps are flared by theuser withthe3618 Edge-Flaring Tool, 3615 3619A Pre-Flared Spec-Caps. Here the Spec-Cap isflared before beingplaced inthedie; 3619and Alternatively, theflaredSpec-Cap technique may beusedwitheitherthepaintedSpec-Caps orthe Cap requires somefinesse. Spec-Cap wall crumpling inward, andthetechnique ofassembling thediearound aloadedSpec- oflow-Zand possibly(inthecase elements) lessthan “infinitely thick.” There isalsoachance ofthe material is unusuallydenseorincompressible, thin,prone thesamplediskwillbe very to cracking successful isquite efficient, butthere perhapsthe are handicaps; greatest isthat unlessthesample Spec-Cap.filled This approach allows many samples to besetupandmarked inadvance, andwhen ways. The simpleristoSpec-Cap fillthe withsample, level itoff, and assemblethedie around the and 3617,38mm,makes 40mmdisks). The painted, straight-walled beusedin two Spec-Caps can painted withstraight walls (3619,30mm,makes 31mmdisks;3615,33mm, makes 35mmdisks; There are ofSpec-Caps, two types unpainted withflared walls (3619A,makes 31mmdisks)and remove thesample diskfrom thedie. die, asalubricant, andthepaint onthe3615,3617,and3619Spec-Caps acts making iteasierto also protects thebore ofthediefrom abrasive samples, enlarge whichwithtimecan ordamagethe allowing thediskto bewritten onandhandledwithoutcrumbling orcontamination. The Spec-Cap prepared by withaSpec-Cap willbeencased theSpec-Cap ononesideandaround itsedge, Spec-Caps are shallow inwhichasampleispressed. aluminumcups Asamplediskproperly Spec-Cap Proper Use oftheSPEXSamplePrep be taken immediately. pellet isplaced inthediebore, itshouldmove freely. Ifitdoesnot, careful corrective should action and rotate itgently inthemouthofbore to make sure itisproperly linedup. When apolished polished pelletinto thediebore isto holdthetrailing edgeofthepelletlightly withthefinger-tips, thepelletto cause can chip, andquite possiblyruinthe thedie. Asimpletechnique for inserting free thepelletgently. Above andmake all, thesituation donotpushitdown further worse, asthis do notjam;thefitissoprecise slightcause them that tiltwill to stick. a very When thishappens, damaged. thepolishedpelletsinto theboreWhen inserting ofthedie, take care extra that they ofthedie,Remember that andthemosteasily the polishedpelletsare parts themostcritical avoid scratching thepolishedsurface. you would for aglasslensormirror. Steel hasahardness similarto to glass, anditisimportant cleaning hepolishedpellets, treat themlike glass;inotherwords, usethesamecleaningtechnique cross-contamination ofdiskjammingorsticking from andthepossibility samplebuild-up. In treat itastheprecision tool itis. Pellet use, diesshouldbecleanedafterto every avoid bothsample In handlingthepelletdie, somesimplerules shouldbekept inmind:keep thedieclean,andalways the worn pellet, andcompare data. theanalytical press two sampledisksofidentical material, onewithapristinepolishedpelletandtheother considerablyis tolerable from willvary userto user. Asimpleway to checkpolishedpelletsisto condition of the polishedpellets, itistimeto replace them,butthedegree to whichsuchdistortion tube, anddetector. sampledisk, Obviously results ifanalytical are ofthe because beingdistorted Spec-Caps are flared X-PRESS® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 75 Prep-Aid Prep-Aid Binders after or ablate crumble which those samples pressure; under well analytical cohere samples Many and before pulverizing sample after usually blended with the Binders are a binder. require pressing can but also serve supporting of sample. as a pellet matrix, thin layer a pressing, name brand to reagents available commonly from and range Binders can be liquids or powders, crumble-proof disk achieved sample a stable, use should lead to Their formulas. products with secret and effort. of dilution, contamination, with a minimum cellulose and paraffin Of these, graphite. and boric acid, paraffin, Generic cellulose, binders include and for blending form, ideal finely powdered in extra-pure, SamplePrep SPEX through available are and blends quickly (3642) has a particle of less than 20 microns, Cellulose size Prep-Aid® pelletizing. as a sample matrix It can also be used undiluted weight. 10% by with samples at and completely and a sample, a die nor contaminate It will neither stick to with the sleeve-and-plunger technique. be kept however, should, with cellulose Disks stabilized storage. in the bottle during does not cake and swell and slowly as with time they can absorb moisture be retained, to if they are in a desiccator crack. our notions of the perfect satisfies product, SamplePrep SPEX all-around an exclusive UltraBind, and moisture- when palletized, strong and is self-lubricating, with samples, binder: it blends well of the manufacturing as a relic process. of NaCl amounts low have however, Most batches, resistant. remove yield a disk which is easy to blends easily with samples to Ultrabind A fine (20 μm) powder, and swelling cracking resists It also handling. rough withstand enough to and durable the die, from when used with the Sleeve-and-Plunger technique, disk matrix and is an excellent in storage, (3644) is described on page 200 along with other UltraBind® described in this chapter. binders. waxy as the seals the are air-stable, binder 20% paraffin Sample to with 10% disks formed As with by SPEX SamplePrep. offered (3646) is also Paraffin Powdered surface against moisture. them. contaminate does not with samples and blends evenly the fine (30 μm) powder cellulose, as in this technique, with the sleeve-and-plunger should not be used undiluted paraffin However, the die. to it will stick concentration a stable make to or undiluted and canbe used diluted form, in pure Boric available acid is commonly it typically and hence than cellulose supplied in hygroscopic it is much more sample disk. However, grinding in a mill or mortar-and a fine enough powder requiring become form, granular pestle to the sample during the final stage of Some analysts add boric acid to with a sample. blend evenly to if they are in a desiccator Sample bonded with boric acid must be kept disks this. achieve grinding to be preserved. to sample. any rapidly with and blends by moisture, sample disks unaffected makes powder Graphite for Its disadvantage the pellet die. disks from free it easy to making It also serves lubricant, a its own was Graphite weight. it must be used in a proportion least 50% of the sample disk by XRF is that of at because of its was sample-disk of but that in the development techniques, used extensively pressing most XRF manufacturers by size as the standard 31 mm sample disk accepted The high conductivity. optical spectroscopy, emission arc/spark in the point-to-plane technique for originated and users was are with graphite Sample disks pressed the sample. is passed through current a high-voltage where techniques. spark ablation also used for acrylic Liquid binders and others. pulverized plastic, wax, Solid also include powdered binders be a solution of Most appear to pressing. blended with a sample prior to also used; they are are all the sample particles blending, during is that advantage their reputed polymer(s) in solvent(s); range of sample weight is, for a 31 mm disk, 5 to 8 grams; for a 35 mm sample disk, 7 to 10 grams; grams; 10 disk, sample 35 mm a for 7 to grams; 8 disk, a 31 mm for 5 to is, weight sample of range 12 grams. mm disk, a 40 for 8 to and, Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX X-PRESS® TECHNICAL INFORMATION 76 XF (3650)isused, usuallybeaddedto thebindercan thesamplebefore grinding. size.grinding aidsare often neededto fineparticle attain very When agrindingaidsuchas Vertrel® likely to bindwell underpressure thanthesamesampleground to moderate fineness, andthat be noted finelyground that avery sample (e.g. cement-mix ground to below 10microns) ismore sample before grindingwillleadto caking inthegrindingcontainer. itshould Inthisconnection then caking whenthepressure isrelieved. Hence there isagoodchance that addingabinderto the isthat ofcaking underpressure,conspicuous property orat leastofflowing underpressure and binding tabletsavailable. theuseofbindersingeneral, Of itshouldberemarked that theirmost The classicexample ofthisgenre isaspirin,butthere are more sophisticated, grinding/ proprietary in tabletform, sothat auniform amount beeasilyaddedto can thesamplejustbefore grinding. There are alsomaterials whichare touted asaidsfor bothgrindingandbinding. Generally theseare possible samplediskrupture undervacuum-path conditions. evacuation ofgases, volatiles, andmoisture duringpressing, andpreventing assistingcompaction machined SPEXSamplePrep diesetalsoincorporates avacuum hoseattachment. This allows out ring” ofthesteel pelletsandsamplediskfrom allows easyextraction thedie. Each precision- samplediskreadyyielding acompact for thespectrometer’s sampleholder. Aconvenient “knock- two polished steel pellets. material Sample ispressed inthediebore between the polishedpellets, wear,and extra theSPEXSamplePrep dieincludesabody withdetachablebase, aplunger, and Each SPEXSamplePrep diesetisacomplete unit. Madeofhardened stainlesssteel for durability are clearlylabeledwithbore size andmaximumsafe load. mm for mostOESandXRFinstruments, and35mm40for newer XRFspectrometers. Dies SamplePrep offers dies to make four standard sizes ofsampledisks:13mm for IRspectrometers, 31 The choice ofdieisgenerally determined by therequirements instrument. oftheanalytical SPEX aPellet Die Selecting receive alight coating ofthepolymer, sothat subsequent pelletizing ismore andefficient. direct CONNECT WITH US ONLINE!

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77 Borate Fusion

®

• K1 Prime • K2 Prime

KATANAX® FUSION FLUXER

Katanax has been creating automated electric fusion equipment since 2002. Katanax fluxers combine exceptional fusion accuracy with all the advantages of electric power. Katanax fluxers allow you to save time and money while obtaining the best possible analytical data from fused samples.

The multi-lingual touch screen interface comes pre-loaded with various fusion programs that can be used as is, or customized for your particular protocol. Pre-loaded programs include: Oxide, Metal, Solution, Peroxide, Anneal and Ramping. Programs can be saved, renamed, deleted or copied, just like computer files. The interface also allows the user to control and monitor the temperature of the furnace.

APPLICATIONS SAMPLE TYPES • Prepares glass disks for XRF or • Ceramics • Clinker solutions for AA, ICP, and wet • Cement • Ores chemistry analysis • Minerals • Catalysts Rocks Refractories Peroxide or pyrosulfate fusions • • • • Slag • Metals • Liquid or solid oxidations • Soil • Alloys

78 KATANAX® FUSION FLUXER Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 79 com/sampleprep visit www.youtube. For video, scan with video, For your smartyour phone or Part number: number: Part K1P-115 K1P-230 XRF analysis and C ୦ 3-prong grounded plug, plug, grounded 3-prong French/ 115V 60Hz or 2-prong German style plug with an multi- IEC connector allowing cables. country power 19" (47 cm) x 11" (28 cm) x 26" (66 cm) 20 - 1150 Color LCD touch-screen interface pre-loaded touch-screen LCD Color languages. in multiple with fusion programs

1 3. Power Cord Power Operating Operating Temperature Dimensions 2 3 1300 W 66 lbs (30 kg) 115V/60Hz or 230V/50Hz Safety shield protects users from the heat. Safety users from shield protects and the crucible for heaters Independent mold.

Weight Power Power Consumption Voltage Features & Specifications 1. 2. K1 Prime is a single-position, fully automated, electrica maximum fusion machine with is a single-position, K1 Prime fully automated, The fused beads for preparing for Ideal samples per hour. of 5-7 sample throughput including of fusion parameters control chemistry and wet Automated analysis. AA, ICP, solutions for stirring time glass disks or time for cooling mixing time and rate, time and temperature, heating with 30 mm, 32 and K1P-40 K1P-35 K1P-32, K1P-30, Model numbers CE approved. solutions. for respectively. mm, 35 mm and 40 mm mold holders, Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX KATANAX® FUSION FLUXER 80 with 30mm,3235mmand40mmmoldholders, respectively. in15-20%lesstime.fusion cycles CEApproved. K2P5-Sisa5-positionunitbuiltfor solutionsonly solutions. high-throughput "HX" isavailable Optional package that allows K2Primes to complete heating timeandtemperature, mixingtimeandrate, cooling timefor glassdisksorstirringtimefor throughput of24-30samplesperhour. Features automated control offusionparameters including The 2. 1. Features &Specifications Power Cord Weight Consumption Power Voltage

K2 Prime isasix-position fullyautomated fusionmachinewithamaximumsample electric from theheat. Integrated shieldprotects locking safety users temperature. all crucibles andmoldsare at thesame furnace ensures electric High performance 1 (Single Phase) (Single 220-240V/50-60Hz 110 lbs(50kg) 4000W (HXversion) 3000W max 3-prong grounded plug. 4 Dimensions Temperature Holding Temperature Operating 4. 3. 3 2

connectivity alsoincluded. connectivity loaded withseveral fusionprograms. USB Color LCD touch-screen pre- interface and sixmoldsfor high-throughput. Crucible holderaccommodates sixcrucibles 20 -1100 20 -1200 x 27in(68cm) 36 in(91cm)x19(48 ୦ ୦ K2P-230 Part number: your smart phoneor your smart For video, with scan visit www.youtube. C C com/sampleprep KATANAX® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 81 Mold – 40 mm Heavy-Duty Mold – 35 mm Heavy-Duty Mold – 40 mm

platinumware lasts longer and lasts longer platinumware KP1009A KP1010A KP1008A 95% Pt/5% Au, 48 g. 95% Pt/5% Au, 95% Pt/5% Au, 34 g. 95% Pt/5% Au, 95% Pt/5% Au, 48 g. 95% Pt/5% Au, Zirconium Crucible Regular CrucibleRegular Heavy-Duty Crucible Mold – 35 mm Mold – 32 mm Heavy-Duty Mold – 32 mm Mold – 30 mm Heavy-Duty Mold – 30 mm

Molds KP0049A KP1002A KP1001A SPEX SamplePrep offers crucibles made of 95% platinum and 5% gold, the standard non-wetting non-wetting the standard 5% gold, and platinum made of 95% crucibles offers SPEX SamplePrep Pt/Au and crucibles fusions. peroxide for available are crucibles Zirconium fusions. borate for alloy and heavy-dutyregular in heavy-dutyversions; offered are molds is less likely to warp. All platinumware sold separately from the instrument. Price quotations are are quotations Price instrument. the from sold separately platinumware All warp. to is less likely Service prices that 623-0465. Please note (732) contacting Customer at by upon request available fluctuations. market change due to daily and may quoted are 100% Zirconium, 55 g. Straight-walled crucible. crucible. Straight-walled 55 g. 100% Zirconium, Capacity 30 mL. 95% Pt/5% Au, 26 g. Straight-walled crucibles. crucibles. Straight-walled g. 26 95% Pt/5% Au, Capacity 30 mL. with crucibles Straight-walled 30 g. 95% Pt/5% Au, durability. greater for and bottom rim a thicker Capacity 30 mL. KP1007A KP1005A KP1006A KP1004A KP1003A Crucibles & Molds for Katanax® Fluxers Molds & Crucibles for 95% Pt/5% Au, 25 g. 95% Pt/5% Au, 95% Pt/5% Au, 21 g. 95% Pt/5% Au, 36 g. 95% Pt/5% Au, 95% Pt/5% Au, 18 g. 95% Pt/5% Au, 30 g. 95% Pt/5% Au, Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX KATANAX® ACCESSORIES 82 Racks andHolders Racks Crucible Heater Lids 7151R high as1200°C. (nichrome) alloys usedfor rack withstandtemperatures as For holdingsix7152or7152HPgraphite crucibles. Ni-Cr HANDLING TOOLS PLATINUMWARE,LABWARE & For handlingcrucibles; 20in. For handlingcrucibles; 9in. 7151T 7154 KP0010A Unbreakable Teflon beaker used for preparing solutions. concerned withpossiblecontamination. is suppliedwiththeK1Pime. Recommended for users be usedinplace ofthealuminacrucible heater lidthat /5%Au,95% Pt 16g. Platinum crucible heater lidcan heatconserves duringfusionandaidsinpouring. withtheK1Prime.Supplied Itprotects thecrucible, KP5606A –Moldholder, 40mm, 6-position KP5605A –Moldholder, 35mm, 6-position KP5604A –Moldholder, 32mm, 6-position KP5603A –Moldholder, 30mm, 6-position available. All MoldPlates are designedto holdsixmolds. Custom sizes are Automated Fluxer Electric HoldersforMold theK2Prime KP0040A MoldHolder, for 40mmmolds KP0039A MoldHolder, for 35mmmolds KP0038A MoldHolder, for 32mmmolds KP0037A MoldHolder, for 30mmmolds Automated Fluxer. Electric HoldersforMold theK1Prime Beakers KP1011A KP5015A Short TongsShort

Rack and TongsRack Long Tongs

Teflon® Beaker Platinum Heater Crucible Lid HeaterAlumina Crucible Lid

KATANAX® ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX

83 7161, 7162 7153 Graphite Crucibles Graphite

Graphite Crucibles Graphite Graphite Crucibles Graphite Graphite Crucibles Graphite Graphite CruciblesGraphite

Graphite Crucibles Graphite

Micro, 9.5 mm O.D. x 19 mm, 0.6 mL capacity. x 19 mm, 0.6 mL capacity. 9.5 mm O.D. Micro, sold in units of 100. High-purity graphite; For casting 40 mm glass disks, 57.1 mm O.D. x 38.1 57.1 mm O.D. casting 40 mm glass disks, For bottom. flat 40 mm I.D. mm, 44.5 mL capacity, sold in units of 10. Highpurity graphite; 31.8 mm O.D. x 28.6 mm, 8.4 mL capacity. Regular Regular mL capacity. x 28.6 mm, 8.4 31.8 mm O.D. 100. sold in units of purity graphite; 31.8 mm O.D. x 28.6 mm, 8.4 mL capacity. x 28.6 mm, 8.4 mL capacity. 31.8 mm O.D. sold in units of 10. High purity graphite; 7162 7161 7160 7153 7152HP 7152, 7152 HP 7152 For casting 40 mm glass disks, 57.1 mm O.D. x 38.1 57.1 mm O.D. casting 40 mm glass disks, For bottom. flat 40 mm I.D. mm, 44.5 mL capacity, sold in units of 10. Regular-purity graphite; will crucibles Glass disks cast in graphite (NOTE: for which should be polished flat faces rough have analytical accuracy. For casting 33.7 mm glass disks, 50.8 mm O.D. x 50.8 mm O.D. casting 33.7 mm glass disks, For bottom. flat 33.7 mm I.D. 38.1 mm, 32 mL capacity, sold in units of 10. Regular-purity graphite; Graphite Crucibles for use with Muffle Furnaces Furnaces Muffle with use for Crucibles Graphite Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX KATANAX® ACCESSORIES 84 sample offlux,orinformationcustom ona flux. fusion, at 6-7mgper drop. SPEXSamplePrep Pleasecall for afree dropper bottleisaconvenient way to addnon-wetting agent to a so theentire meltistransferred to thebeaker. solutionina LiBr is added to the flux before making a solution for ICP/AA analysis, the meltfrom sticking to thecrucible ormold. Additional orLiI LiBr when making a “glass bead” (lithiumborate sampledisk),to keep non-wetting agent. Asmallamount orLiIisaddedto ofLiBr theflux ofthesefluxesSome includelithiumbromide orlithiumiodideasa andcoarseto glass-beadtexture. theirpurity Fluxes andadditives. These fluxes have exceptional qualitiesdue SPEX SamplePrep isproud to offer thefulllineofSPEX Fusion FUSION FLUX LiM/LiBr LiM/LiBr LiM LiT/LiM/LiBr LiT/LiM LiT/LiM/LiI LiT/LiM/LiBr LiT/LiM LiT/LiM/LiI LiT/LiM/LiBr LiT/LiM LiT/LiI LiT/LiBr LiT Mixture LiNO3 (500g) FFB-301-03 LiNO3 (250g)FFB-300-03 (125g)FFB-200-03 LiF crystals LiI –15mLsolution(10pk)FFB-115-03 LiI –15mLsolutionFFB-113-03 (125g)–trihydrateLiI crystal saltFFB-110-03 –15mLsolution(10pk)FFB-105-03 LiBr –15mLsolutionFFB-103-03 LiBr (125g)FFB-100-03 crystal LiBr Additive Description 35.00/65.00 (12/22) (11.94/21.89/0.17) Composition (%) 49.75/49.75/0.50 49.75/49.75/0.50 66.67/32.83/0.50 66.67/32.83/0.50 50.00/50.00 67.00/33.00 98.50/1.50 99.50/0.50 99.50/0.50 99.50/0.50 100.00 100.00 FFB-1005-02 FFB-0007-02 FFB-0005-02 FFB-0000-02 FFB-3505-02 FFB-3500-02 FFB-5007-02 FFB-5005-02 FFB-5000-02 FFB-6707-02 FFB-6705-02 FFB-6700-02 FFB-1007-02 FFB-1000-02 Pure Part Number Part FFB-5007-03 FFB-5005-03 FFB-5000-03 FFB-6707-03 FFB-6705-03 FFB-6700-03 FFB-1007-03 FFB-1005-03 FFB-1000-03 FFB-0007-03 FFB-0005-03 FFB-0000-03 FFB-3505-03 FFB-3500-03 FFB-5007-03 FFB-5005-03 FFB-5000-03 FFB-6707-03 FFB-6705-03 FFB-6700-03 FFB-1007-03 FFB-1005-03 FFB-1000-03 Ultra-Pure KATANAX® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 85

XRF. Each bead was measured ten times, with times, ten measured bead was Each XRF. www.spexsampleprep.com/appnotes. To download this application note in its entirety visit APPLICATION NOTE SP026: PREPARATION AND XRF ANALYSIS OF FLY ASH BEADS BEADS ASH FLY OF ANALYSIS XRF AND PREPARATION SP026: NOTE APPLICATION ASH FLY & SLAG, CEMENT, APPLICATION: Analysis ED by analyzed sets of glass beads were two The the results averaged for each bead. The results for the five beads within a set were then averaged averaged then were beads within a set the five for results The each bead. for averaged the results of & 2 as percentage 1 Tables in shown are results The set. the for results obtain overall again to being silica of iron, Oxides and alumina. with the major components each analyte, for composition lesser in present titanium, sodium, and sulfur were potassium, calcium, magnesium, phosphorus, of the fly ash. the remainder and comprised amounts was the fly ash sample that indicating consistency within a set, excellent show XRF results In addition, of reproducibility. level fused beads with a high the K1 prepares homogenous and that the that it is apparent Thus, nearly identical. 2 are Table 1 and Table from averages the overall clear glass produced fluxes both Since results. composition had no effect of flux choice on the XRF fly ash. to use with this either is appropriate beads with the fly ash sample, one bead for example An scans of each bead. the ten for also consistent were results Measured scans of the other repetitive obtained from of results 1 and is indicative in Appendix is shown nine beads. Fusion Method Fusion residual carbon to eliminate at 750° C for 2 hr. crucible in a porcelain roasted was fly ash The into a Pt/Au weighed were ratio of 8:1) 0.80 g of fly ash (a flux/sample (~0.2%). 6.40 g of flux and a 32 mm glass bead and fused into a plastic laboratory hand with spatula, by mixed gently crucible, program, OXIDE fixed version of the K1’s a modified used was fusion program The using the K1. 1035° C. at 15 minutes 4) set for with the main fusion stage (Step CertiPrep FFB-5005-02 (1:1 SPEX fluxes: each of two in this manner for prepared beads were Five and agent) as a non-wetting with 0.5% lithium bromide lithium metaborate lithium tetraborate: with 0.5% lithium bromide). metaborate FFB-6705-02 (2:1 lithium tetraborate:lithium ABSTRACT particles of the mineral is comprised and of coal the combustion product from ash is a waste Fly and certain in mixes component cement is used as a fly ash Recovered gases. rise with the flue that of concrete. the durability and strength improves sets of glass two and then fused into and blended, was pulverized a sample of fly ash In this study, SPEX from fusion fluxes lithium borate different Two K1 electricbeads using a Katanax fusion fluxer. by energy then analyzed were The beads beads with each flux. five prepare to used were CertiPrep both within a set compared were results and the (EDXRF) spectroscopy flourescence X-ray dispersive using the K1 and effect of flux consistency of beads produced evaulate sets to the two and between on the XRF measurements. composition Preparation and XRF Analysis of Fly Ash Fused Beads Fused Ash of Fly and XRF Analysis Preparation Katanax Application Note Katanax Application Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX KATANAX® TECHNICAL INFORMATION 86 improving offusionsfor trace analysis. the performance in trace analysis, since thesampleisdiluted during fusion. There have beenrecent advances in but noteliminate them.Borate fusionmay notbethemethodofchoice iftheanalyst isinterested X-ray fluorescence analysis isthemethodofchoice. The fusionmethod will reduce matrix effects sample, ithasproven to bethebestmethodfor materials that have when these characteristics size andproduces fusioneliminates andmineralogical effects Because ahomogeneous particle Borate fusionhasbecome increasingly popularasapreparation technique for XRFsampledisks. bounds for thetechnique. borate fusionsofsulfides,carbides andsome ferro-alloy materials formerly considered out-of- to borate fusions. However, hybrid oxidation/fusion techniques have beendeveloped for reliable Most ofthesesamplesare naturally oxygen-rich anddonotrequire transformation chemical prior pigments suchas TiO2, andslagsfrom smelters, blastfurnaces, refineries andglassplants. as cement, buildingmaterials andminingconcentrates. Additional industrialsamplesinclude like dolomite, sand, basaltandiron ore, andby-products butalsotheirindustrialproducts such cement, glass, ceramics, miningandminerals. analyzed Samples includenotonlyraw materials Many Automated usersoftheK1andK2Prime Series Fluxers Electric are inthefollowing industries: and damageordestroy them. not onlyremaincan alsoalloy insolubleinthefluxbut withthe95%platinum/5% goldcrucibles befusedwithboratescannot thesecompounds because reduce duringfusionandthemetalswill asaglassdiskorpouredbe cast into adilute acidsolutionanddissolved. Platinum-group metals in theprocess and therefore bemeasured). sulfurcannot Oncefusioniscomplete, themeltcan coal. The coal samplemustbeashedandtheashisthenfused. The sulfurinthecoal willvolatilize be oxidized. Organic compounds mustbeashed. (An example ofthisistheanalysismetallurgical sulfides,carbides, chlorides, etc, mustbe oxidized before beingfused. Reduced metalsmustalso silicates; zirconia and aluminaare Compounds oxides; withoutoxygen andsoforth. suchas be intheform ofanoxidized, inorganic compound. Cement isusuallyablendofcarbonates and metal ores andsilicate rocks). For borate fusionsto besuccessful, thesamplewhenfusedmust pressed powder (e.g. cement), hard to dissolve inacid(e.g. zirconia andalumina),orboth(e.g. Borate fusionsare widelyusedfor sampleswhichare eitherdifficult to prepare ashomogenous When to Employ Borate Fusion operations withmufflefurnaces. SamplePrep SPEX also provides thefulllineofSPEX Fusion Flux. Automated Fluxers Electric for rapid, reproducible fusions, andgraphite crucibles for smaller-scale SPEX SamplePreptwo offers approaches to borate fusion. KatanaxThe Series K1andK2 Prime hazardous acids(e.g. HF)isavoided. borate bequicker fusioncan overall thanmicrowave dissolutioninpressure vessels, andtheuseof minutes to make glassdisksorsolutionswithautomated fluxers. For samplesprepared asliquids, oftheadvantagesOne preparation ofborate fusionistheshort ten time, to typically fifteen samples containing sulfides, ferroalloys, etc. hydrochloric acidfor analysisinsolutionby AAorICP. Recent advances alsoallow borate fusionof XRF analysis. The asaglassdiskfor becast XRF, meltcan orquicklydissolved indilute nitricacidor mineralogical effects. The useofborate fusionswillalsominimize which matrix effects are seenin it, yieldingahomogenousmelt. The sampleforms borate size saltsandthiseliminates and particle lithium metaborate. The isheated samplemixture until thefluxmeltsandsampledissolves in powdered form withaflux,eitherlithium tetraborate oflithium oramixture tetraborate and rock, andsimilarmaterials for elemental analysisby XRF, AA,andICP. The samplesare mixed in Borate fusionisanextremely effective methodofpreparing cement, refractories, ceramics, Borate Fusion Technical information for Fusion Katanax Fluxers KATANAX® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 87 Fusions are accomplished in several steps. First the sample is mixed with a flux in an appropriate ratio ratio with a flux in an appropriate the sample is mixed First steps. in several accomplished are Fusions the flux from prevent to agent 1:2 and 1:10), with the addition of a non-wetting (usually between for to 7 grams 6 of flux/sample mixture are amounts Typical and the mold. the crucible to sticking of past the melting point sample is heated The a solution. for 2 grams a 31 mm glass disk, and 1 to performed fusions are made of in crucibles Most borate crucible. the flux in an inert, heat-resistant in graphite done fusions are Some borate alloy. non-wetting a standard and 5% gold, 95% platinum crucibles. the sample has until agitated regularly and the crucible is maintained During the fusion, heating a mold and into the melt is either poured At this point flux. in the molten dissolved completely stirred 10% HNO3) and acid (e.g. mineral dilute into or poured XRF, a glass disk for form annealed to to harden is left fusions) the melt pyrosulfate In some cases (notably the glass flux dissolves. until the dissolve in an acid solution to placed are and the glass together and the crucible in the crucible, glass. The fluxer. programmable with an automated, sample throughput great achieve It is possible to fused glass disks seven up to can produce samples, cement for when programmed K1 Prime, Katanax of LiBr, a percent of flux and about half with 6 grams mixed of cement using 0.6 grams in an hour, similar samples can for when programmed K2 Prime, 6-position Katanax The agent. a non-wetting 30 fused disks per hour. up to produce can with SPEX be carriedfurnace out manually in a muffle fusion procedures same borate The crucibles can be used SPEX SamplePrep flat-bottomed larger The crucibles. graphite SamplePrep with handled and agitated as perform are cast while the crucibles well glass disks as to fusions, is usually much longer than time per sample with the muffle furnaces The tongs. SPEX SamplePrep contact Again, please our applications has its advantages. Each approach fluxer. with an automated requirements. your for the optimum equipment determine specialists to How to Prepare a Fused Sample a Fused Prepare to How The pressed powder method can be highly accurate when carefully done with multi-phase samples samples multi-phase with done carefully when can method accurate be highly powder pressed The and during grinding subject segregation are but such samples to ore sand and rock, cements, such as are Particle disks glass effects). and mineralogical size Borate effects(e.g. matrix and to pressing, in desiccators. stored if carefully stable because disks are they powder than pressed preserve to easier as fusion method, borate with the oxides pure XRF can be made from for also standards Synthetic problems. matrix-matching a solid solution with few glass is essentially borate of the major advantage techniques, and other liquid-analyzing AA, ICP, for samples In preparing pressure with acid in a microwave than dissolution simpler and quicker it is often fusion is that borate of a decanting to elements ignition of the heating from procedure, fusion/solution A complete vessel. require fusions do While borate fluxer. an automated or less in minutes fifteen cansolution, clear take the melt, dissolve HNO3 to or HCl the use of dilute and and fumes, heat some caution in evacuating not necessary. acids are mineral other concentrated such as HF and reagents hazardous materials. for all not be suitable but may of applications range a wide fusion methods offer Borate should be so structural and molecular information of the sample, the original form destroys Fusion 1150˚ C) drives fusion (1000˚ to of borate high temperature The made. the fusion is before measured during fusion. form compounds while other Sn, and Sb, metals such as Hg, volatile compounds of off fusion can for extend inorganics and reduced materials organic Extra necessary steps prepare to samples borate many For choose. method to accurate be the most time but still may turnaround analytical approach. and most accurate quickest, fusion is the simplest, methods, important are and widely used sample preparation Both fusion and pulverizing/pressing either approach. for of equipment has a full range SPEX SamplePrep advantages. each with their own your suitable for which method is more help determine specialists to our applications Please consult laboratory. Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX KATANAX® TECHNICAL INFORMATION 88 NWA. The ideal amount ofNWA for aspecific procedure is usuallydetermined by experiment. fusion, somewhat longerfusions(asfor some technical ceramics) may alsoneedgreater amounts of “stickiness” ofamelt, require additionalNWA. non-wetting As agents gradually volatize duringa e.g. 12mgofNWA for 6gramssamplessuchasiron offlux. ores,Certain which greatly increase the sample before fusionstarts. Typically theamount ofNWA isabout0.2%oftheweight oftheflux, When glassdisksfor XRFare beingmade, anon-wetting agent ismixed withthefluxand with excessive NWA willballupwhenpoured andnotform acomplete disk. concave andmay bedifficult to uppersurface remove from themold, whereas amolten fluxbead agent isto tension increase ofthemelt. thesurface Afuseddiskwithtoo littleNWA willhave a fusion sothemolten fluxwillnotstick to thecrucible ormold. ofanon-wettingThe visibleeffect Non-wetting agents (NWA) are iodidesandbromides beadded insmallquantities whichcan to a Additives for Fusions: Non-Wetting Agents, Fluidizers, andOxidizers our customers. SPEX SamplePrep guaranteesofthefluxes andthequality andadditives boththepurity supplied to All fusionfluxesSamplePrep sold by SPEX are manufactured to thehigheststandards available. physical superiorfor characteristics theirapplication. andlessdensethantheis fine-grained “glass bead” fluxes, butis available forthosewhofindits borate/carbonate flux(aphysical andso-called mixture) “fluffy” lithium tetraborate. The latter andeaseofuse,homogeneity andminimumabsorptionofmoisture. The exceptions are the Most SPEXFusion Flux are ofthe “glass bead” for maximum andcoarse-grained type,pre-fused agent to aflux. for greater convenience. solutionisavailable LiBr separately for quickadditionofanon-wetting The mostpopularblendedflux,2:1 “tet:met,” isalso available non-wetting withaddedLiBr agent grades. All are ofanalysis for trace suppliedwithacertificate metalimpurities. tetraborate/lithium carbonate mixture. Many ofthesefluxes are available inpure andultra-pure metaborate, several lithiumtetraborate/metaborate blends, sodiumtetraborate, andalithium SPEX SamplePrep offers thefull lineofSPEX Fusion Flux. This includeslithium tetraborate, lithium with thesefluxes at temperatures between 1000˚and1150˚C. lithium tetraborate/metaborate issogreat mixtures that fusionsare mostanalytical out carried a fusion,thegreater thedegree ofvolatilization. However oflithiumtetraborate theutility and ofaflux,asthehigher Meltingpointtemperature mayHandbook. intheselection beafactor of (1979)andinSulcek andPovondraBock (1989),bothcited inthebibliography at thebackofthis and more specialized applications. Alternative fluxes andfluxing techniques in are discussed potassium pyrosulfate (K2S2O7). These have lower meltingpoints thanlithiumborate fluxes fluxesOther includesodium tetraborate (Na2B4O7),sodiummetaphosphate (NaPO3),and proceedthe fusioncan asnormalwithoutany lossofsulfurfrom thefusion. lithium orsodiumnitrate andpreheated to oxidize thesulfide to sulfate. When thishasbeendone have material beendeveloped for suchas fusingsulfide-rich copper ore. The sampleismixed with materials befirst can oxidized withstandard techniques andthensuccessfully fused. Methods fluxes, andwilloften crucibles,attack platinum-gold oralloy withthem. However, many ofthese etc. Metals, sulfides, nitrates,carbides, phosphides, etc. inlithiumboratecannot befuseddirectly Individually ortogether, theselithiumborates willdissolve oxides, carbonates, silicates, sulfates, tet” are mixtures more suitablefor acidicoxides suchassilicate rocks refractories. andsilica-alumina dissolution ofbasicoxides, andispreferred for cement andmostores. Lithiummetaborate or “met/ (LiBO4, M.P. ofthetwo. oramixture 845˚C), arule As lithiumtetraborate isbetter suited for the Most fusionsinvolve theuseoflithiumtetraborate (Li2B4O7,M.P. lithiummetaborate 920˚C), aFusionHow Flux to Select lithium KATANAX® TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 89 When making solutions by pouring the molten flux into a dilute mineral acid, it is desired to have have to desired it is acid, mineral dilute a into flux the molten pouring by solutions making When proportion much higher a can require This beaker. the to crucible the from transfer complete is necessary than agent disk. pour a glass A quantity to sample not of flux plus of nonwetting popular are bromide iodide and Lithium of NWA. 100 mg to 50 require might grams 2 exceeding is lithium bromide becauseHowever do not add an impurity they the flux. agents to non-wetting a dropper flux from the and added to solution saturated a so it is usually made into hydroscopic, and easier air-stable, more somewhat iodide are and cesium sodium iodide, Lithium iodide, bottle. out 10 or 20 mg weigh than it is to of NWA or two add a drop to it is simpler While use as solids. to non- that Note while a fusion is in progress. a hot crucible cannot added to be liquid NWA of a solid, as copper being fused, samples are when copper-bearing care should be used with agents wetting the melting lowering Lithium fluoride can be used as a fluidizer, volatile. extremely halides are melting point a flux’s lowers it weight, by At 10% easily. far more it flow of a flux and making point C. about 100˚ by unoxidized can be useful in eliminating and sodium nitrate such as lithium nitrate Oxidizers mix, is relatively in cement present often Graphite, will not fuse. a sample that from components oxidized can be crack.to Graphite cause it a black film on a glass disk or even harmless but can leave to enough corrosive be may such as phosphides and sulfides Other sample components CO2. to they and sulfates phosphates to oxidized in a single fusion. If they are a crucible damage or wreck analysis. in the fused glass disk for will be present and their cations harmless, will be comparatively fusion including them should any fluxes, then borate melting points lower much have As oxidizers is complete. oxidation until temperature a low at proceed ACCESSORIES FOR XRF ANALYSIS

The XRF spectroscopist is confronted with an almost infinite variety of samples. Liquid samples, from water to oil, require virtually no preparation. Many solid samples, if homogeneous, can be machined to the proper shape and run directly. Others, such as refractories, ores, and biological materials, are too inhomogeneous, and must be pulverized or fused. Then the homogenized material can be dissolved for analysis as a liquid sample, pressed into pellet form, or cast as a glass like solid. SPEX SamplePrep manufactures disposable sample-handling accessories for powder and liquid XRF samples. Over the last twenty years, millions of powder samples for XRF have been pressed and protected in the SPEX SamplePrep Spec-Cap, an aluminum cap for reinforcing pellets. Millions more liquid XRF samples have been run in SPEX SamplePrep X-Cells. These and the related products listed here will save you time and money, and assure you of reproducible, contamination-free results. Spec-Caps® SPEX SamplePrep® Spec-Caps® are shallow, thin-walled aluminum cups which are routinely used in the production of pressed powder sample disks for OES, XRF, and other analytical techniques. The Spec-Cap forms the bottom and sides of the finished pellet. Thus reinforced, sample disks are resistant to chipping and breaking, and are more easily handled, marked, and stored than unclad disks.

3619 30 mm Spec-Cap® 30 mm wide x 8 mm deep, for 3623 die. Produces 3615 33 mm Spec-Cap® pellets 31 mm x 5 mm. Outside painted to prevent 33 mm wide x 8 mm deep, for 3616 die. Produces seizure in die and to facilitate labelling. Sold in units of pellets 35 mm x 5 mm. Outside painted to prevent 100 and 1000 (3619M). seizure in die and to facilitate labelling. Sold in units of 100 or 1000 (3615M). 3619A 31 mm Pre-Flared Spec-Cap® 31 mm wide x 8 mm deep, for 3623 die. Produces 3617 38 mm Spec-Cap® pellets 31 mm x 5 mm. The 3619A has been preflared 38 mm wide x 9 mm deep, for 3614 die. Produces for a snug fit in the 3623 31 mm Evacuable Pellet Die, pellets 40 mm x 5 mm. Outside is painted to prevent and has an unpainted surface. It may be substituted seizure in die and to facilitate labelling. Sold in units of for the 3619 30 mm Spec-Cap in all applications 100 or 1000 (3617M). where flaring is recommended. Eliminates need for 3618 Edge-Flaring Tool. Sold in units of 100 and 1000 (3619AM).

90 XRF ACCESSORIES Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 91 . . . Edge-Flaring Tool Edge-Flaring Bubble-Free Cell InsertBubble-Free Cell

X-Cell )n

5 ) (3642-450) (3644-450) (3646-450) O 10 2n+2 For 3615 Spec-caps. This tool tool This Spec-caps. 3615 For to rim the Spec-Cap widens the a snug fit against ensure thus preventing of the die, walls pellet sample loss and jamming. 3625 H Polyethylene snap-ring, collar, collar, snap-ring, Polyethylene and and cup with snap-post vent film. window Requires reservoir. Sold in units of 100. 3527I 3561 Patented insert the 3527 40 for Patented air trapped Prevents mm X-cell. a bubble under the forming from X-cell film when the is window position. Soldused in the upright in units of 100. 6 H n Prep-Aid UltraBind® Prep-Aid Binder – (C Cellulose (C Binder – Paraffin Prep-Aid

≤ 20 μm powder, 150 g bottle. Can be blended with sample at 10% by weight weight 10% by be blended with sample at Can g bottle. 150 ≤ 20 μm powder, with Sleeve-and- as sample matrix XRF sample disk, form or used undiluted to 25-35 supported for matrix bond 200-250 disks or provide Will Plunger Set. 600-750 disks or will bond as 450 g bottle that available Also sample disks. supported 72-105 for matrix sample disks provide ≤ 20 μm powder, 150 g bottle. Can be blended with sample at 10% by weight weight 10% by be blended with sample at Can 150 g bottle. ≤ 20 μm powder, with Sleeve-and- as sample matrix XRF sample disk, form or used undiluted to 25-35 supported for matrix bond 200-250 disks or provide Will Plunger Set. will bond 600-750 disks or as 450 g bottle that available Also sample disks. 72-105 supported for matrix sample disks provide 3646-150 3644-150 3642-150 < 20 μm powder, 150 g bottle. Can be blended with sample at 10% by weight weight 10% by be blended with sample at Can g bottle. 150 < 20 μm powder, with Sleeve- matrix as sample or used undiluted XRF sample disks, form to Binder with the of Paraffin resistance the moisture Combines and-Plunger Set. with Cellulose is associated the die that disk from a prepared ease of removing 25–35 supported- for matrix bond 200–250 disks or provide Will Binder. will bond 600-750 disks or as a 450 g bottle that available Also sample disks. 75-105 supported for matrix sample disks provide Edge-Flaring Tool Edge-Flaring

X-Cell X-Cell Spec-Caps. and 3619 Spec-Caps. 3617 For rim widens the Spec-Cap tool This a snug fit against the ensure to thus preventing of the die, walls pellet jamming. sample loss and 3625 Tool Edge-Flaring 3618 31 mm Closed X-Ray cell cell X-Ray 31 mm Closed snap-ring and polyethylene and cup with snap-post vent film. window Requires reservoir. Sold in units of 100. 3529 40 mm Closed X-Ray cell with cell X-Ray 40 mm Closed snap-ring and polyethylene and cup with snap-post vent film. window Requires reservoir. Sold in units of 100 3527 ® X-Cells ® BInders PrepAid Edge Edge Tools Flaring Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX XRF ACCESSORIES 92 Thin Film Note: noted All measurements inmmunlessotherwise SPEX SamplePrep X-Cells details dictate the type andsizedictate thetype ofX-Cell andwhichwindow material to use. PANalytical, Rigaku, Bruker, and Thermo Instruments. The requirements oftheapplication will SPEX SamplePrep X-Cells are designedto fitthemajorbrands ofXRFspectrometers suchas Number X-Cell X-Cell 3577 3565 3527 3571 3529 356T 31mmUniversal X-Cell 31 mm Open End X-Cell31 mmOpen 43 mmX-Cell 40 mmX-Cell 31 mmX-Cell Description 3511 film to desired length.(Polyimide) with serrated edgefor tearing wide, 50ft. (15m)long, inbox continuous roll 2 as Supplied 0.3 mil(8μm)thick. (Roll) Micro X-Cell 3515 diameter, 500sheetsperbox. circles 3 pre-cut as Supplied 0.25 mil(6μm)thick. (Large) 3565 units of100. Requires windowSoldin film. withventand cup andreservoir. Polyethylene collar snap-on for Analyzers. Horiba Sulfur 43 mmClosed X-Ray Cell 3577 units of100. Requires windowSold in film. sensitive orhazardous samples. body. Uniquecell for small, air- collar,snap-rings, andopen Collar. Twopolyethylene 31 mmMicro X-ray Cell with

Kapton® WindowFilmKapton® Mylar® Pre-Cut Circles Circles Mylar® Pre-Cut X-Cell X-Cell 1 7 / 4 / 8 in.(82.6mm) in.(73mm) Overall Height 22.0 22.0 22.0 22 19 22 Overall O.D. 31.6 39.5 31.6 31.6 48 32 Plane O.D. Window 31.6 31.6 43.0 38.0 31.6 30.5 3512 per box. mm) diameter, 500sheets as pre-cut circles 2 as pre-cut Supplied 0.3 mil(8μm)thick. desired length.(Polyester) with serrated edgefor tearing to wide, 300ft. (92m)long, inbox continuous roll 2 as Supplied 0.12 mil(3μm)thick. (Roll) 3516 3571 Sold inunitsof100. Sold body. Requires window film. collar,snap-rings, andopen Cell withCollar two polyethylene End X-Ray Open 31 mmDouble Kapton Pre-Cut Circles Pre-Cut Kapton

Aperture Mylar WindowFilm X-Cell 38.8 31.5 24.5 24.5 24.5 6.3 7 / 1 8 in.(73mm) / 2 in.(63.5 Capacity 11.5* (mL) 0.5 1.0 8.0 8.0 13 XRF ACCESSORIES TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 93 in. in. in. in. in. - - - - - 2 2 2 2 4 / / / / / 1 1 1 1 1 2 2 2 2 3 in. (63.5 in. (63.5 in. (63.5 in. (63.5 (63.5mm) (63.5mm) (82.6mm) (63.5mm) (63.5mm) 2 Diameter / 1 1 1 Mylar Pre-CutMylar Circles Ultralene® Pre-Cut Polypropylene Pre-Cut Polypropylene

Quantity 500 Circles 500 Circles 500 Circles 500 Circles 500 Circles 300 ft (92m) 300 ft (92m) 300 ft (92m) 300 ft (92m) 50 ft (15mm) Circles 0.16 mil (4 μm) thick. Supplied as pre-cut 2 circles with 500 per box mm) diameter, paper interleaving. 3526 3518 3518 0.25 mil (6 μm) thick.0.25 mil Supplied as pre-cut 2 circles 500 sheets mm) diameter, per box. 3521 as pre-cut 2 circles 500 sheets mm) diameter, per box. Circles thick.0.2 mil (5 μm) Supplied Roll Roll Roll Roll Roll Type Precut Precut Precut Precut Precut 4 8 8 6 4 3 6 6 5 5 (micron) Thickness Thickness .3 .3 in. (70 .15 .25 .15 .12 .25 .25 .20 .20 4 (mil) / 3 Thickness Thickness Ultralene® Window Ultralene® Window Polypropylene Polypropylene Mylar Window Film Window Mylar

Mylar Mylar Mylar Mylar Kapton Kapton Film (Roll) Film 0.16 mil (4 μm) thick. Supplied 2 7/8 in. (73 roll as continuous (92 m) long, 300 ft. mm) wide, edge for serrated with in box length. to desired cutting film 3525 Window Film Window thick.0.2 mil (5 µm) Supplied 2-7/8 in. (73 roll as continuous (92 m) long. 300 ft. mm) wide, 3520 3517 3517 (Roll) (6 μm) thick.0.25 mil Supplied 2 roll as continuous (92 m) long, 300 ft. mm) wide, edge for with serrated in box length. to desired film tearing Ultralene Ultralene Description Polypropylene Polypropylene 3511 3512 3515 3526 3516 3517 3518 3520 3521 3525 Film P/N Film Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX XRF ACCESSORIES TECHNICAL INFORMATION 94 the snap-post on therear bepushedtothe snap-post can break thesealandto permitventing oftrapped bubbles pushed down over to thecup form aflat drum-like window. The cell isturned over and, ifdesired, samples, isfilledwithliquid, thecup apiece offilmisspread over the top, is thenthesnap-ring facilitatescup labeling. ring. Each closedX-Cell For consists andsnap-on ofacup routine liquid guards spectrometers. againstspillageininverted-optic withinthereservoir Aroughened surface through thevent. This assures theanalystofasmooth,flat window for improved precision, yet sealfor venting volatilesnap-open for samples andareservoircatching cup any liquidsthat expand and a43mmClosed Cell for Analyzers. Horiba Sulfur The patented closedX-Cell designfeatures a most spectrometers. For specialapplications there areEnd and Open 31mmDouble contaminant-free polyethylene, closedX-Cells are available inboth31mmand40sizes to fit ofX-Cellof theapplication willdictate thetype andwhichwindow material to use. Madeof spectrometers suchasPANalytical, Rigaku, Bruker, and Thermo Instruments. The requirements of liquidsamplesinXRFspectrometers. They are designedto fitinto themajorsuppliersofXRF SPEX SamplePrep X-Cells are usedthroughout theworld for fast, dependable, reproducible running forX-Cells XRFLiquidSamples recommend 3615 and3617Spec-Caps, respectively. havemanufacturers shifted toward 35mmand40 mm sampledisks, andfor theselarger sizes we sample disks. For theseinstruments, 3619and3619ASpec-Caps are ideal. Several spectrometer than uncladdisks.The sample holdersofmostX-ray spectrometers willaccept 31mm(1 the disksare resistant to chippingandbreaking andare more easilyhandled, marked andstored sides ofthecompleted pellet, sampledisk(alsocalled briquette, orplanchet). Thus reinforced, ofpressed-powderthe production sampledisksfor XRF. The Spec-Cap forms thebottom andpartial SPEX SamplePrep Spec-Caps are shallow, thin-walled whichare aluminumcups routinely usedin Reinforcing XRFPellets withSpec-Caps application. our samplepreparation specialiststo determine theoptimumequipment andtechniques for your and oxidants. These are products describedelsewhere inthishandbook;pleasefeel free to consult lines ofgraphite crucibles, borate fusionfluxes, andfusionadditives suchasnon-wetting agents yielding XRFglassdisks, orsolutionsfor AA,ICP, etc. fusionwork For there further are alsofull also theKatanax K1andK2Prime Automated Fluxers Electric for rapid, automated borate fusions, of compressing thosepowders into flat, uniform sampledisks, ready for XRFanalysis. There are converting mostsolidsamplesinto homogeneouspowders, aswell asdiesandpresses capable suited for XRFspectroscopy. There are millsandgrindingcontainers laboratory of capable SPEX SamplePrep alsoprovides anextensive lineofsamplepreparation equipment particularly assure you ofreproducible, contamination-free results. SamplePrep X-Cells. These andtherelated listed products here willsave you timeandmoney, and protected inSPEXSamplePrep Spec-Caps. more Millions liquidXRFsampleshave beenrun inSPEX samples. Over years, thelasttwenty millionsofpowder samplesfor XRFhave beenpressed and accessoriesSPEX SamplePrep for powder disposablesample-handling manufactures andliquidXRF pellet form,asaglasslike orcast solid. fused. Then thehomogenized material bedissolved can for analysisasaliquidsample, pressed into as refractories, ores, materials, andbiological are too inhomogeneousandmustbepulverized or solid samples, ifhomogeneous, bemachinedto can theproper shapeandrun directly. Others, such flat Liquidsamples, disk. from water to oil, are run insample cells covered withathinfilm.Many common isthat theymustallbepresented to theXRFspectrometer intheform ofahomogeneous, The XRFspectroscopist isconfronted withanalmostinfinite ofsamples. variety What theyhave in to XRFaccessories Introduction Micro X-Cells, 1 in.) XRF ACCESSORIES TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 95 he Bubble-Free Cell Insert is a simple, patented insert (3527) which Insert XRF liquid cell the 40mm for patented Cell he Bubble-Free is a simple, prevents trapped air from forming a bubble under the window film when the cell is used in the film when the a bubble under the window forming air from trapped prevents the sample is added, Insert before a cell Cell 3527I Bubble-Free is pushed into The position. upright is filled the cell an inverted-coneand forms once shelf under which air bubbles can trapped be bubbles rise to position, so any in an inverted run are liquid cells XRF systems, In many and sealed. optics” “inverted of this drawback The with the analysis. and do not interfere the back of the cell contaminate the sample can spill and potentially ruptures, film if the window is that configuration in so-called being run number of samples are an increasing However, or damage the spectrometer. of underneath. instead the cell is above source the X-ray where XRF spectrometers, optics” “normal displacing the sample can collect during assembly of the cell Bubbles trapped against the window, with a fitted use an X-Cell To it. by the sample and emitted reaching the X-rays and attenuating bubbles should Any and tap it. invert it, Insert, assemble the cell, Cell Bubble-Free SPEX SamplePrep insert, the hole in the is turned right-side-up and when the cell rise through the bubbles will be an Most but not all bubbles get into film. the window from away shelf, the insert’s below trapped shown have Tests beam. the X-ray by when heated some samples outgas during assembly; X-Cell to escape without bulging such gases film will allow pinhole near the edge of the window a that will fit normal Cell InsertX-Cell coupled with the 3527 3527I Bubble-Free the film.The or rupturing Inc. Rigaku Scientific and Shimadzu Instruments, Diano, made by optics XRF spectrometers Selecting Thin Film Windows for XRF for Windows Selecting Film Thin a thin film which serves by as the sample window. must be covered liquid sample cell X-Cell An X-rays of the transmission uniform the liquid while allowing contain film must effectively The your analytical priorities and the nature film depends on of a window choice Your the sample. to there Are versa? or vice transmission, important more than X-ray strength Is of the sample. capable of Is the sample chemically in the film? aggressive, certain cannot tolerate impurities you up or will it heat X-Cell, the certainyou pour it into or penetrating Is it hot when films? weakening on the film and put pressure volatiles release Will it the film? during analysis and perhaps soften inside the cell? from T Bubble-Free Cell InsertBubble-Free Cell X-Cell is then positioned in the spectrometer spectrometer in the positioned is then X-Cell filled The is run. sample the while liquid or expanded mask. For or powders. of pastes small quantities and residues solution run canto be used also X-Cells the with slightly then dished for solutions, as prepared is window the film residues, solution to under an IR lamp dries warmed and there of solution placed A drop a glass rod. end of rounded the surface on of film is spread piece and another or paste If powder situ analysis. in a smudge for 3527 The analysis. X-ray for sample is ready the sandwiched on the ring, snapping before overlaid 31 mm sample disks. hold crumbling canalso be used to 40 mm X-Cell unusual many ideal for which are Double Open X-Cells End supplies versatile also SPEX SamplePrep or RTV tar, glue, such as materials viscous pastes, sludges, samples: slurries, or hard-to-handle two at both ends, has a body open X-Cell The 3571 and machine parts, metal films etc. sealant, film window After while the ring is being applied. snap-on hold film in place to and a collar rings, dabbed, poured, and the sample placed, it can inverted, be one end of the cell, to has been attached can then be of the 3571 X-Cell top The directly against the window. or otherwise in the cell, located left or sealed with film. open is the solution X-Cell then the 3577 Micro samples, or hazardous air-sensitive deal with small If you mm in is 6.3 the window holder, 31 mm sample standard it fits in the While problems. your to ready you’re and scatter reduce to your beam down Collimate up. and only 0.5 mL fills it diameter, a 7 x 13 mm back,open or window but it will also accept can with an be run X-Cell Micro The go. to of special samples. or the isolation injection, for purging, bottle closure serum Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX XRF ACCESSORIES TECHNICAL INFORMATION 96 well asthewindow film. temperatures well below 100°C, soifyou are working with hotsamples, pre-test the are likely to perforatelongbefore theX-Cell isaffected. However, polyethylene beginssoftening at exceptchemicals halogenated hydrocarbons. Window films, being muchthinnerthan X-Cell bodies, X-Cells are madeofpolyethylene, whichisgenerally resistant to acids, bases, andmostorganic to attack. chemical essentially impervious attacked by strong oxidizing agents. Microporous Teflon isnotusedasawindow filmassuch,butis chemicals, beattacked butcan by aromatic andhalogenated hydrocarbons. All ofthesefilmsare chemicals. Polypropylene andUltralene are reasonably resistant to acids, bases, andmany organic except strong bases. Mylarisvulnerable to strong acidsandstrong basesandresistant to organic In general, Kapton ishighlyresistant to acidsandorganic andalmosteverything chemicals follow buttheyare may notmeant beof somehelpinselection, to replace testing. actual exposure to thesamplefor several timesyour longestanticipated running time. The tableswhich the window leaks. For eachnewsample, we strongly recommend that you test thewindow film by Some samplessimply film. attack somefilms, exposingthespectrometer topossibledamageif Attack: Your5. Chemical sample’s may characteristics chemical dictate your choice ofwindow SamplePrep beheldresponsible cannot for variation infilm composition. differenttypes offilmbutalsobetween different notonlybetween lotsofthesame material. SPEX best advice isthat you run ablankfrom newroll every orbox you opensince be impuritiescan coatingbut now to surface includesaphosphate-based improve itshandlingcharacteristics. Our Zr, P, Fe, Cu, Zn, Ti, andAl. cleanestfilm overall Our isUltralene.Kapton iscleaninmost respects (ppm) ofCa, P, Fe, Cu, orSb. Zn, Polypropylene filmhasbeen known to contain trace levels of Ca, others. While Mylarfilmmakes asuitablewindow for mostanalyses, itmay contain trace levels 4. Purity: No XRFwindow filmisabsolutely free ofmetallicimpurities, butsomeare cleanerthan SamplePrep filmsare for uniform thickness selected so your results are reproducible. the thickness ofthefilm. Thus you willgetuneven fluorescent withanunevenintensity film.SPEX Uniform Thickness:3. considered for lightelement analysisinparticular. (4 μmUltralene, and3μmMylar)have thegreatest degree ofX-ray transmission, andshouldbe transparent to X-rays; 6μmMylarismore transparent, asis5μmpolypropylene. The thinnestfilms as well theSPEXSamplePrep asitscomposition. Of XRFwindow films,Kapton 8μm istheleast 2. Transmission: X-ray transmission through polymerfilmsisaffected bythethickness ofthefilm SamplePrep XRFwindow films exceptKapton are weakened by heating muchabove 100°C. our bestfilminitsbalance of X-ray transmission, chemical resistivity, strength, andpurity. All SPEX roughly comparable strengths, mechanical butdiffer inother key properties. Ultralene remains for its thickness. The remaining films(5μmPolypropylene, 4μmUltralene, and3μmMylar)have exceptalmost everything strong solutions. alkali micron Six (6μm)Mylarisalsounusuallystrong any otherSPEXSamplePrep film,heat-resistant to to over impervious 300°C,andchemically durability. Kapton istheclosestthingto abombproof XRFwindow film.Itismuchstronger than window leakage, thefilmsoffered SamplePrep bySPEX have fortheirstrength beenselected and with inverted optics. While SPEXSamplePrep accepts noresponsibility for damageresulting from Leakage1. Strength: orrupture ofthewindow duringarun could damageto cause spectrometers film characteristics: When choosingathinfilmwindow for considerthe your application, following X-Cells, you test themtogether outsidethespectrometer. strongly that ifthere filmsand/or isany questionaboutthecompatibility ofasamplewithcertain and for that purposewe supplyonrequest can samplesofSPEXfilmsand X-Cells. We alsosuggest thefinalchoiceOften offilmbalances several requirements. We recommend comparingfilms, The absorptionofX-rays at agiven wavelength to proportional isdirectly X-Cell body as XRF ACCESSORIES TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 97 - 96 84 97 160 100 100 140 100 100 102 102 100 100 100 100 Tensile Modulus Tensile X-Cell, window film, window X-Cell, 74 92 66 73 62 82 89 10 20 30 20 62 77 30 100 Degrades Elongation - 93 86 94 67 97 60 65 65 65 85 65 100 100 100 100 PERCENT RETAINED TYPICAL PERCENT RETAINED Tensile Strength Tensile C C C C C C C 0 0 C 0 0 0 0 0 0 5 days, R.T. 5 days, Conditions 4 days, 100 4 days, 365 days, R.T. R.T. 365 days, R.T. 365 days, 365 days, R.T. 365 days, R.T. 365 days, R.T. 190 days, 365 days, R.T. 365 days, R.T. 365 days, 22 days, 200 22 days, 14 days, 100 14 days, 14 days, 100 14 days, 14 days, 100 14 days, 36 days, 110 36 days, 180 days, 150 180 days, 166 days, 100 166 days, p-Cresol Methanol Toluene Oil Transformer Benzene Chloroform Jet Fuel 10% Sodium Hydroxide, pH = 8.9 Acetone Hexane pH = 4.2 Oil Shale pH = 10.0 Water: pH = 1 Acetic Acid, Glacial Acid, Acetic Substance Reprinted by permission of E.l. du Pont de Nemours & Co., Kapton, Summary E-50533. of Properties Kapton, & Co., de Nemours du Pont permission of E.l. by Reprinted Chemical of Kapton® Resistance Thin Film Transmission Characteristics Transmission Film Thin SPEX SamplePrep window films and X-Cells are not intended to be used in vacuum-path vacuum-path in be used to intended not are X-Cells and films window SamplePrep SPEX CAUTION: or cansample chamber stretch in an XRF spectrometer’s change pressure abrupt An XRF systems. come apart. leak or to or otherwise film, also be noted It should burst window X-Cell the cause and can stretch an X-Cell, inside pressure the ability generate to chemicals have some volatile that the film between the joint through by migrating leakage cause slow bursting or (rarely) to a film a SPEX SamplePrep a question about whether is there Whenever and the cell. or combination thereof is likely to perform to in a particular likely properly is the analyst analytical thereof situation, or combination the spectrometer. contaminating does not risk which way test these products in a should first Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX XRF ACCESSORIES TECHNICAL INFORMATION 98 Chemical Resistance ofMylar Chemical Glacial AceticGlacial Acid Acids Substance Sodium Hydroxide,Sodium 10% Hydroxide,Sodium 2% Silcone ResinGESR28 Silicone ResinGESR80 Phenolic ResinGE1678 ResinGE2480 Glyptal Hydrocarbon Oil, low. vis. Dimethyl Formamide Ethyl Acetate Hydrochloric Acid, 10% Dioxane (1.4) Solvents Asphalt Base GE9466 Base Asphalt Varnishes Silicone, DC200 Tricresyl Phosphate Sulfide, 4% Sodium Ethanol Hydrofluoric Acid, Con. Hydrocarbon Oil, hi.vis. Impregnants Methyl Ethyl Ketone Sulfuric Acid,Sulfuric 30% Nitric Acid, 40% Nitric Acid, 10% Toluene Ammonium Hydroxide, 2% Bases Trichoroethylene Detergent, 25% Miscellaneous 168 hours, 150 900 hours, 150 24 hours, 75 24 hours, 75 24 hours, 75 24 hours, 75 (immersion) Conditions (baked) O O O O C C C C O O C C Tensile Strength Percent Retainedtypical 100 100 100 100 100 100 100 100 100 100 100 100 100 92 92 90 85 58 92 90 96 79 72 75 80 0 0 Elongation 230 100 100 100 141 100 100 100 100 100 100 100 100 100 18 18 65 65 54 80 67 45 50 50 3 0 0 Tensile Strength 100 113 113 125 100 100 123 100 100 100 100 100 100 40 40 97 60 73 97 40 75 75 50 0 0 - - XRF ACCESSORIES TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 99 C C C C C C B B B B B B B B B B B A A A A A A A A A A D B,E A,E Effect C) O 80 60 20 60 20 60 20 60 20 60 20 20 20 80 60 20 60 20 20 20 20 60 60 20 20 80 60 20 80 100 Temperature ( Temperature Ethanol Glycol Ethylene Ether Ethyl Ethyl Acetate Ethyl Ammonia, 30% Ammonia, 10% Hydroxide, Ammonium Acetate Amyl Alcohol Amyl Chloride Amyl Aniline Regia Aqua Fuel Aviation Benzene Benzyl Alcohol Brine Aqueous Bromine, 20% Hypochlorite, Calcium Disulfide Carbon Tetrachloride Carbon GasChlorine Chloroform 50% Acid, Chromic Cyclohexanol Decaline 2% Detergents, Chlorobenzene Acetic Acid, 50% Acid, Acetic Acetone Acetophenone Acetic Acid, Glacial Acid, Acetic Substance Chemical Polypropylene of Resistance Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX XRF ACCESSORIES TECHNICAL INFORMATION 100 -Extensive Absorption -Extensive orPermeation Reprinted by permissionofHercules Inc., PPD-32E Bulletin -Limited Absorption or Attack Code: Chemical Resistance ofPolypropyleneChemical cont'd Substance Hexane Gasoline Formaldehyde Nitric Acid, 10% Nitric Acid, 70% Lubricating Oil/Motor Oil Linseed Oil Ketones Iodine Tincture Hydrogen Peroxide Hydrochloric Acid, 20% Hydrochloric Acid, 30% Sulfuric Acid,Sulfuric 10% Acid,Sulfuric 50% Acid,Sulfuric 98% AcidSulfamic andSyrupsSugars Silicone Oil Pyridine Plating Solutions Phenol Petroleum Ether Paraffin Whisky Turpentine Trichloroethylene Toluene Wine

E-Ma D-Ex C B A-N egligible Effect tensive Attack y Produce Cracking UnderStress Temperature ( 100 100 100 60 60 60 20 60 60 20 20 60 60 60 60 20 80 60 60 20 60 60 20 60 20 20 20 60 O C) Effect B,E C,E A A A A A A A A A A A A A A B B B B B C C C C C C C XRF ACCESSORIES TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 101 S Y V Ti Tl Si Tc Zr U Sr W Ta Sc Se Xe Tb Tb Pa Th Zn Sn Yb Ra Ru Rn Rh Ag Na Tm Re Rb Sm Pm Symbol Xenon Vanadium Ytterbium Yttrium Zinc Zirconium Uranium Thulium Titanium Tin Tungsten Thorium Selenium Silicon Silver Sodium Element Ruthenium Radon Rhenium Sulfur Terbium Scandium Strontium Tellurium Thallium Technetium Promethium Radium Rubidium Samarium Rhodium Tantalum Protactinium I P K O Ir N H Li Lr In Pr Ni Kr Pt Fe Hf La Lu Os Po Pd Pu Pb Ne He No Ho Nd Np Hg Mo Mg Md Mn Nb Symbol Palladium Oxygen Phosphorus Platinum Plutonium Polonium Potassium Osmium Praseodymium Nickel Nitrogen Niobium Nobelium Neptunium Lead Lutetium Lawrencium Lithium Element Iron Hydrogen Indium Manganese Magnesium Molybdenum Neodymium Neon Lanthanum Hafnium Krypton Mercury Indium Holmium Iodine Mendelevium Helium F C B Cl Fr Er Cf Cr Al Es Cs Br At Ar Ce Ca Ac As Eu Co Cu Cd Bi Sb Bk Ba Be Ge Dy Ga Au Fm Cm Gd Am Symbol Fluorine Gadolinium Gallium Europium Fermium Francium Germanium Gold Curium Erbium Einsteinium Copper Dysprosium Bromine Element Californium Bismuth Boron Cadmium Calcium Chlorine Chromium Cobalt Actinium Berkelium Beryllium Antimony Argon Arsenic Barium Carbon Cesium Aluminum Cerium Americium Astatine Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX TECHNICAL INFORMATION 102 analytical resultsanalytical berefined can accordingly. of contamination andcontrolling them. When thecontaminants are known be quantified, andcan Processing asamplealways contaminates it. Successful analysisdependsonrecognizing thesources Contamination zirconia ceramic doescontribute to theanalyst. isoften notimportant low percentages ofmagnesium oxide andhafniumoxide, the contamination SPEXSamplePrep as densealumina,grindingalmost fastassteel. Anditismostly because hard andtough itwearsslowly, very addinglittlecontamination. times Itisaboutoneandone-half isaceramicZirconia whichinmany ways approaches theidealgrindingmedium.Since itisboth low. to agate, andwhileitcontains someyttriaandalumina,overall contamination levels willbevery contaminant issilicon, consider SPEXSamplePrep silicon nitride. Itisextremely durable compared hardness superiorto agate andzirconia. to have Ifitisimportant acontainer whoseonlymajor resistant. material Silicon nitrideisatough space-age withremarkable wear characteristics, and and metalliccontamination isequallyundesirable. Agate and isextremely is99.9%silica wear- must behandledwithcare. Agate vialsare for thegrindingandmixingofsampleswhenorganic Agate isharder to thansteel, almostanything except inert andchemically HF. It’s alsobrittleand are ahelpfuladditionto any lab’s grindingarmory. ofsamples, abrasion-resistant. minority aluminaceramicbut very forvials animportant Necessary aluminum oxide, withsomesilicon, andmagnesiumpresent. calcium, Itislightweight andbrittle contaminants are All SPEXSamplePrep objectionable. aluminacomponents are 99.5%pure Alumina ceramic isidealfor extremely hard where samplesorincases steel andtungsten carbide will lastindefinitely. They’re recommended asalong-term“best buy” for grinding almostanything. than tungsten, cobalt (abinder)isthemajorcontaminant. Ifcared for, tungsten containers carbide substantially harder andheavier thansteel, grindingisfaster andcontamination isminimal. Other Tungsten vialsanddishesare themosteffective carbide and versatile ofall. Tungstencarbide is containers. corrode steel andshouldbeground intungsten carbide, alumina,agate, zirconia, orsilicon nitride rusts beusedto easily butcan grindsamplesfor RoHS/WEEEtesting. compounds Halide-releasing expected. to Stainless attack, steelbutcontributes chemical islesssubject Niaswell. Cr-free steel the lab. When hard substances are ground insteel containers, someFe andCr contamination be can Hardened steel isdurable andtough, suitablefor general-purpose grinding;it’s theworkhorse of sample. for mixing andstoring powders. With thesevialsonlytraces oforganic impuritiesare addedto your andpolystyrene vialsandballsareMethacrylate idealfor pulverizing soft, brittlematerials and withcareselected inthelab. to offercapability optimum presence inthesamplewillnotinterfere withanalysis. SPEXSamplePrep’s containers have been container isgenerally harder thanthematerial to beground andshouldbeofasubstance whose a mill. The proper grindingvialordishwillgreatly enhance accuracy. analytical The grinding Your ofappropriate selection asyour grindingandmixingcontainers choice isasimportant of Grinding Container Materials KEY POINTS ABOUT GRINDING zirconium oxide with TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 103 Shatterbox, Shatterbox, Howard Kanare of Construction Technology Laboratories, Inc. has publicized the use of propylene the use of propylene has publicized Inc. Laboratories, Technology of Construction Kanare Howard laboratory for fine grinding of 0.3 wt.%) roughly of sample, grams ten up to for drop (one glycol mill such as the SPEX SamplePrep In a swing minerals. and many cement Portland or without agglomeration microns less than ten quickly to samples canoven-dried be ground Dry grinding is simpler and quicker, but requires much more careful matching of the technique to to of the technique matching careful much more but requires Dry grinding is simpler and quicker, the sample can be dried soils and cements, as in many moisture, is due to If the caking the sample. Dry with a variety of additives. soaps/ ground Other samples can be successfully grinding. before as well agent is an anti-static graphite and some also include an abrasive; lubricants, are detergents a an abrasive, contain which may proprietary many grinding aids as well, are there as a lubricant; and acetate Other phenyl grinding aids include polyvinyl and a binding agent. alcohol, lubricant aspirin. Slurry grinding is an obvious approach; if particles remain in suspension during grinding, they Slurry if particles in suspension during grinding, approach; grinding is an obvious remain and grinding, the sample before to added or other liquids are alcohol, Water, cake. to unlikely are of grinding a sample to way slurry Although reliable afterwards. grinding is a reasonably removed grinding container, a leak-proof particles, and time-consuming, it is sloppy requires micron-sized procedure. sample preparation one’s to and adds extra steps Grinding Aids further during grinding, particle reduction is clearly size “cake” or samples agglomerate When the fusing of particles accumulation, charge static heat, moisture, from can result Caking inhibited. “art” an preparation sample which make of the techniques Many and other causes. under pressure, the possibilities. at can only hint and we caking, getting around to devoted are Because of these variations in grinding container composition, we strongly recommend recommend strongly we composition, in grinding container Because of these variations your with preferably containers, individual grinding your of the exact profile determining elemental grind samples of known is to simplest approach The and techniques. analytical equipment own grind portions may one samples, known Lacking grinding. by is added and see what composition in increase which elements see and check to lengths of time, increasing of a single sample for for known impurities and their proportions are Once the contributed proportion grinding time. to of the regardless results, to the analytical can be fitted profile the resulting a grinding container, (While is important, it clearly will vary this level with the composition level. actual contamination and of the sample, and toughness hardness, the size, of the grinding container, and condition grinding time). Major, minor, and trace elements predictably found in SPEX SamplePrep grinding containers containers grinding in SPEX SamplePrep predictably found elements and trace minor, Major, grinding almost no two strictly speaking, Chart in listed A, Sectionare 2. However, 2, Chapter carbides, steels, different many are There exactly profile. the same elemental will have containers a so that type proprietary, formulas are the Often compositions. each with specific and ceramics, two from makeup a different specific properties will have have to carbide engineered of tungsten of the same to batch batch from variations inevitable are In addition, there manufacturers. different composition. element both in the exact proportions and in trace of the major elements material, As the grinding container is the major source of contamination, its selection is critical. In general, its selection In general, is critical. contamination, of source major is the As container the grinding will which elements avoiding while levels contamination minimize objective should be to one’s carbide container: slags in a tungsten of steel is the grinding example An analysis. with interfere carbon, of tungsten, contaminants low-level and the expected carbide grinds rapidly, tungsten selection of grinding SPEX SamplePrep’s in these slags. for looked generally not are and cobalt your samples for flexibility maximum the best approach in choosing you gives materials container and analytical aims. Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX TECHNICAL INFORMATION 104 homogeneous powder. Inevitably, some ofthispowder isreleased into theenvironment, usually The general ofsample grindingis, objective ofcourse, to convert aninhomogeneoussolid to afine, Protection Respiratory agent. containers bethoroughly driedafter cleaningand, ifstored, kept inaplasticbagwithdesiccating removed by warm dilute oxalic acidsolutionorabrasive cleaning, we recommend that steel Hardened steel andeven stainlesssteel containers rust. can While iron oxide coatings be can scratching ofthegrindingsurfaces. that grindingcontainers become more difficult of tocleanwithagebecause progressive pittingand checking theimpuritiesappearing insuccessive batches sand. ofground Itshouldbenoted quartz A cleaningprocedure iseasilyevaluated by grindingandanalyzingaknown sample, oreven by controls respirable airbornedust. orsimilar appliance. advantage Asafety the useofablow-dryer ofthiscleaningmethod isthat it sand together withhotwater anddetergent, thecontainer. thenrinseanddry isspeededby Drying grindingprocedureAn effective single-step for mostgrinding containers is to grindpure quartz may benecessary.metal, cleaningormultiplegrindswith quartz chemical the container thoroughly. Inextreme cases, such astheplating of container walls withamalleable For more thorough cleaning onemay grindoneormore batches sand, ofpure andthenwash quartz out acontainer, sampleanddiscard ofthenext it. thenbrieflygrindan expendable portion applications asimplewipedown withethanolmay approach suffice; another ispractical to brush the procedure beassimpleorcomplex can asyour warrant. objectives analytical Insome containersGrinding shouldbecleanedbetween sampleruns to avoid cross contamination, and Containers Cleaning Square PA. Advances inX-ray Analysis, Vol. 44,JCPDS–International Centre Data, forNewtown Diffraction Approaching aUniversal Preparation Sample Methodfor XRFAnalysis ofPowder Materials. Anzelmo, Alexander; (2001). andArias, Larry John;Seyfarth, Reference X-Press. transfer theground sample/binderpowder to thedie. Press at 20tons for 0.3minutes ina3636 the Vertrel XF. inan8530Shatterbox Grind for 2.0minutes, openthegrindingcontainer inahooduntil together 10grams ofsample, 2.5grams of3642Cellulose or3644Ultrabind binder, and7mLof here adapted for SPEXSamplePrep equipment: inan8501Hardened Steel Container Grinding load The technique that follows was pioneered by JohnAnzelmo andcolleagues at Bruker AXS andis grinding container, andisavailable asaPrep-Aid product. beroutinelycan ground below 10microns. Vertrel XFalsolowers contamination levels from the container iseasierto clean. Typical XRFsamplessuchascement, rock, clinker, andsimilarmaterial almost any sample isenhanced by theuseof Vertrel XF, contamination islowered, andthegrinding an opengrindingcontainer withoutleaving any residue. experience Our isthat the “grindability” of aid. Afluorocarbon fluid, it prevents caking sample duringgrinding, andquickly evaporates from Vertrel® XF, aDuPont soldasacleaningfluid, product isfindingincreased acceptance asagrinding data sheet;itisavailable asaPrep-Aid product. sticking to themillwalls. Propylene glycol mustbeusedsafely, after consulting thematerial safety Vertrel XFhasevaporated. Prepare a361440mmPellet withaflared Die Spec-Cap, 3617 and TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 105 How to Select to How a Laboratory Mill and Grinding Container or production batch not for are They the analytical for laboratory. intended mills are SamplePrep from less than ranging in amounts grinding of analytical samples efficient rapid, but for milling, Mixer/ Freezer/Mills, hallmark SPEX SamplePrep The 100 grams. approximately up to one gram use the so after samples, individual for grinding containers separate all have Mills and Shatterbox spectroscopists designed for were mills SPEX SamplePrep is cleaned and not the mill. container but also homogeneous powders, uniform samples to about reducing not only concerned who were during processing. the samples added to was about what select SPEX to proper the and can help you these concerns addresses follows that information The application. your for mill and grinding container SamplePrep of several a choice have you temperature, impact room by at samples can be pulverized If your are mills that ring-and-puck are and 8530 Shatterboxes 8500 The mills. SPEX SamplePrep proven 8000M The or less. in 5 minutes 100 grams, approximately grinding of samples up to rapid ideal for samples in the 10 gram not only pulverize high-energy ball mills that are and 8000D Mixer/Mills 60 mL. approximately emulsions up to and making blending powders suitable for but are range with about 10% the sample capacity high-energy is a smaller ball mill, of the 5100 Mixer/Mill The multiple-sample and capacity these mills have All with smaller samples, 8000-series Mixer/Mills. maximum on-the-job a for over flexibility and materials, sizes of grinding container a wide choice of applications. wide range unique cryogenic can grind Mills mills that are Freezer 6770, 6870 , 6870D and 6970 EFM The and most polymers, and animal tissue, including all plant sample, “ungrindable” almost any require Freezer/Mills milling. room-temperature to resistant are other samples that countless in the vial during cryogenic and maintaining temperatures sample, chillingthe for liquid nitrogen the most widely used and most remains the Freezer/Mill its introduction Forty after years grinding. cryogenicworld. effective mill in the When to Pulverize When to to a serious sampling dilemma: how presents world in the real nonhomogeneity of materials The Often approach the best analytical whole with a small sample. nonuniform often a large, represent and representative compositionally to be enough large a quantity of the material to take is first to a particular Then the sample can be adapted analytical powder. a fine homogeneous it to reduce has SPEX SamplePrep etc. dissolved, a sample disk, fused, into pressed and used as is, technique, of samples, all kinds and blending capable of pulverizing laboratory containers mills and grinding pharmaceuticals. to and pesticides living tissue, to rocks plastis, metals to from Pelletizing Samples Pelletizing and dies. presses analysis with SPEX SamplePrep and IR X-ray for pellets can be turned into Powder X-Press. Automated 3636 and the 35-ton manual presses and 25-ton 12-ton offer We Infrared Mulls Infrared using small Mixer/Mills with SPEX SamplePrep prepared quickly KBr and Nujol mulls are pellets spectrum polystyrene appears as a constant The (3114). vials (3118) and steel agate plastic (3111), background. no IR produce and agate Steel and can be subtracted. easily background during the emptying or cleaning of the grinding container. We strongly recommend the wearing of of wearing the recommend strongly We emptying the during container. grinding of the or cleaning Even laboratorythe use of a and suggest fume hood. this procedure, dust-mask during an approved when system the respiratory harmful to potentially can samples become and cement rock harmless pulverized. finely Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX TECHNICAL INFORMATION 106 choose theproper weight for hissample,andothercharacteristics. based onitsdensity approximately 1.3g/mL,inavolume conducive to efficient grinding. Clearlytheanalystmust the middleofvolume range. The grindingsample”“typical sand, of withadensity isquartz volume, isachieved withsamples grindingefficiency for blending40–50%.Optimum toward The recommended maximumsamplevolume for grindingisapproximately 20%ofacontainer’s need to getdone. know aboutSPEXSamplePrep mills, themore confident can bethatyou theywilldothejob you in ourapplications lab, orwe loanyoutrialsinyour can amillforown short-term lab. The more you applications, feel free to specialists. ourproduct contact We of alsooffer your samples test-grinding and Accessories To any discuss SPEXSamplePrep millsandcontainers, for your andtheirsuitability showsThe thecomposition ofStandard following chart Steels usedinSPEXSamplePrep Equipment Chart B: Composition of Standard Steels Used in SPEX SamplePrep Equipment & Accessories Compositions are theoretical, actual lot analyses are not available. The major element is iron, minor elements listed below will vary. Additional trace elements may be present and will change from lot to lot. Actual composition of individual grinding vials should be determined by analyzing known samples ground in those containers, and determining which element(s) were added during the sample grinding.

Type Carbon Manganese Phosphorus Sulfur Silicon Chromium Nickel Molybdenum Zirconium Where Number % % % % % % % % % Used 0.15 0.15 1.00 303 2.00 max 0.20 max 17-19 8-10 0.60 max 0.60 max 3114 max min max 0.030 1.00 304 .08 max 2.00 max 0.045 max 18-20 8-12 - - 6781S, 6757, 8004SS max max 0.030 410 0.42 0.40 0.040 max 0.60 14.25 - - - 5200, 3127 max

2150, 3114SB, 3127, 3610, 3613, 3614, 440C 1.10 0.60 0.040 0.030 1.00 16-18 - 0.50 - 3616, 3623, 6751, 6757, 6781S, 6801, 6881, 8007, 8007B

0.95- 3117B, 8001, 8009, 52-100 0.20-0.35 0.03 0.03 - 1.3-1.6 - - - 1.1 8501, 8507, 8521

ASTM 06 1.45 1.00 - - 0.90 - - 0.25 - 6771, 6871, 6883

Tool 0.90 1.10 - - 0.30 0.50 - - - 3117 Steel TECHNICAL INFORMATION Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 107 G Press ini M Ultrabind X- X-Cell ShaQer • • • • • Mixer/Mill PrepAid Spec-Cap Shatterbox Ultralene • • • • • iton V

• DNeasy

Kapton Vertrel XF Vertrel

• •

Kryo-Tech Freezer/Mill Geno/Grinder Katanax Auto-Extractor • • • • • PCR QIAshredder • Delrin W T

TRADEMARK REFERENCES TRADEMARK • izard • Corporation: of Promega Trademark Registered Registered Trademark of Roche Molecular Systems and Hoffman of Roche Molecular Systems Trademark Registered LaRoche: Registered Trademarks of Qiagen: Trademarks Registered • Registered Trademark of Katanax Inc: Trademark Registered Katanax Registered Trademark of DuPont Teijin Films: Teijin of DuPont Trademark Registered Mylar Registered Trademarks of E.I. DuPont de Nemours & Company: de DuPont of E.I. Trademarks Registered • • eflon Registered Trademark of Applied Biosystems: of Applied Trademark Registered TaqMan ICDD Registered Trademark of International Centre for Diffraction for Centre of International Trademark Registered Data®: Registered Trademarks of SPEX SamplePrep, LLC SamplePrep, of SPEX Trademarks Registered SAMPLE GRIND / FUSION / PRESSED PELLET REQUEST FORM

Send samples to SPEX SamplePrep at 65 Liberty Street, Metuchen NJ 08840, USA. Fax form to +1 (732) 906-2492 or submit the form online at www.spexsampleprep.com. Please contact us before sending in your test sample. Call (732) 623-0465: or email [email protected]. Samples are required to be sent on customers account, excess sample that is considered to be hazardous will be returned. Up to three samples will be ground at no charge. A report and recommendations will be returned within three weeks. SELECT A SPEX SAMPLEPREP PRODUCT TO DEMO, OR RECEIVE A QUOTE: 2010 Geno/Grinder 6870 Freezer/Mill 8000D Mixer/Mill 2020 Geno/Grinder 6870D Freezer/Mill 3636 X-Press 1600 MiniG 6970EFM Freezer/Mill 8530 Shatterbox 1500 ShaQer 5100 Mixer/Mill K1 Prime Fluxer 6770 Freezer/Mill 8000M Mixer/Mill K2 Prime Fluxer SPEX SamplePrep grinding or mixing container: ______Sample description and composition: ______If sample is incompatible with any grinding container or considered hazardous in any way please include MSDS. Purpose for Grinding: ______Emission Spectroscopy: ______X-Ray Spectroscopy: ______Extraction: ______Other: Desired Particle Size after Grinding, if known: ______If contamination with certain metals or plastics is objectionable, please list them along with the approximate ppm level(s) of concern: ______Notes or Comments: ______

For Return of Sample and Report Name and Title: ______Company Name: ______Mailing Address: ______Phone: ______Date mailed: ______Shipping Account numer: ______

108 DEMO REQUEST FORM

First Name:

Last Name:

Title:

Company Name:

Address: address 2:

City: State/Province/Region:

Country: Zip/Postal Code:

Phone: E-mail:

Select a SPEX SamplePrep product to demo, or receive a quote:

2010 Geno/Grinder 6870D Freezer/Mill 3636 X-Press 2020 Geno/Grinder 6970EFM Freezer/Mill 8530 Shatterbox 1600 MiniG 5100 Mixer/Mill K1 Prime Fluxer 1500 ShaQer 8000M Mixer/Mill K2 Prime Fluxer 6770 Freezer/Mill 8000D Mixer/Mill 6870 Freezer/Mill

Fax form to +1 (732) 906-2492 or submit the form online at www.spexsampleprep.com. Demo Equipment is required to be sent on the customer's shipping account.

109 ORDERING INFORMATION Prices and Quotations Prices are subject to change without notice. We will gladly quote current prices on request. Verbal and written quotes are valid for 30 days unless otherwise stated. Acceptance by the seller is expressly limited to the Standard Terms of SPEX SamplePrep, LLC. Confirming Orders Mark confirming orders clearly. Failure to do so will result in a 25% restocking charge for duplicate shipments. DOMESTIC ORDERS (US) Payment Payment terms are net 30, days based on credit approval. If you do not have an established account with SPEX SamplePrep, LLC, you may provide credit information, three commercial references, Dun and Bradstreet Number, or remit payment including freight charges with order. Payment may also be made by credit card (Visa, MasterCard or American Express), or wire transfer. Shipping Our shipping terms are EXW/FCA Metuchen, NJ. Any other terms are by special arrangement only. Most items are shipped by UPS or motor freight, depending on the size and weight of the shipment. Various express/overnight services are also available. Shipping charges can be pre-paid and the cost will be added to the invoice. If you are sending payment with the order, consult us first for shipping charges. Minimum Orders The minimum order is $100. Replacement parts and repair charges are excluded from this minimum. Export Orders SPEX SamplePrep maintains authorized dealers in many countries around the world. In Europe we are represented by our subsidiary, SPEX CertiPrep, Ltd. To find a distributor in your country please visit our website or contact our main office via email at [email protected]. Orders from countries without authorized dealers may be placed directly through SPEX SamplePrep. However, export ordering terms, instructions, and quotations must be obtained in advance. Orders received without prior agreement may be returned to the purchaser. Payment Prepayment of merchandise cost and shipping charges is required for all export orders. Payment may be made by check, wire transfer, letter of credit, or credit card (Visa, MasterCard, American Express). Minimum order for letter of credit payments is $2,500.00. All banking charges must be to buyer’s account. Any letter of credit that states “banking charges are for the account of the beneficiary” WILL NOT BE ACCEPTED. Warranty SPEX SamplePrep LLC guarantees its products against defects of materials and workmanship for one year from the date of original shipment. Repairs and replacements made under warranty are guaranteed for the remaining original warranty period. The warranty excludes wear parts: that wear out through use and have to be replaced periodically for proper operation. Wear parts include not only gaskets, drive belts, grinding media, and the like, but also pneumatic cylinders, the Geno/Grinder ball slide, the Freezer/Mill coil, and the Mixer/Mill clamp retaining spring assembly. Also excluded from the warranty are grinding vials and containers made from tungsten carbide, alumina ceramic, zirconia ceramic, silicon nitride, and agate. The customer pays return freight for warranty claims, but SPEX SamplePrep will pay return freight 110 to the customer if the warranty claim is valid. SPEX SamplePrep reserves the right to judge whether a malfunction is due to defects in materials or workmanship, or to wear, negligence or misuse. All Katanax instruments have been carefully inspected and tested before shipping and are warranted to be free from defects in workmanship and material for a period of one year from date of shipment. Hard ceramic parts may exhibit small cracks developed under heat, and will not be considered defective unless this situation impairs functionality of the instruments. Heating elements are warranted for a period of six (6) months. To Arrange a Return Shipment We want you to be happy with your purchase from SPEX SamplePrep. Please bring any problem to our attention, but DO NOT RETURN any item before contacting us for a RMA (Returned Materials Authorization)number, and instructions. Unauthorized returns will be refused. Cost for all return transportation is the responsibility of the customer. Credit for returned merchandise is issued only after the goods have been received and inspected, and returns are subject to a 25% restocking fee up to a maximum of $200.00. Address all shipments to SPEX SamplePrep, LLC, 65 Liberty St., Metuchen NJ 08840; always include the RMA number. Service The majority of our products are designed and built in our factory in Metuchen, New Jersey. The SPEX SamplePrep Service Department is an integral part of our operation, and can be counted on to maintain, upgrade, repair, or rebuild SPEX SamplePrep equipment with factory parts and the necessary expertise. Our trained service technicians can also advise you on the most likely cause of a problem. Repairs are subject to a minimum two-hour labor charge, and prices are subject to change without notice. Out-of- warranty repairs and parts are guaranteed for 30 days. Before returning equipment for service, contact our technicians for an RMA number and cost estimate, and include a purchase order with the return. Address returns to our 65 Liberty St., Metuchen, NJ 08840. The customer pays freight both ways for equipment to be serviced. Product Specifications Every effort has been made to provide complete and accurate product information in this catalog. However, specifications are subject to change without notice, and changes may be made from time to time to improve the performance of our products. Precautions SPEX SamplePrep products are not for any household application. Our acceptance of a purchase order is made with the assumption that our products will be used only by qualified individuals who are trained in appropriate procedures. Users are responsible for knowledge and understanding of the potential hazards of the material with which they are working. SPEX SamplePrep does not recommend unattended operation of any of our laboratory equipment.

111 Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX SUBJECT INDEX 112 D C B A SUBJECT INDEX DNA Extraction 21,2223 DNA Extraction Die Sleeve andPlunger 69 Dies, Evacuable, for Pelletizing 68,73 Dewar 34 Cryogenic Transfer Hose34 36,383940 Grinding Cryogenic glovesCryogenic 34 18 Cryo-Block Zirconium Crucible 81 Graphite Crucibles 82,83 Crucible 81 71 thickness critical Cr-Free Vial Contamination Chemical Attack on Window Film 96 Ceramic 14,254759 Media Grinding Cellulose Binder 69,91 14,15 Cap-Mats Bubble-Free 91,95 Borate Fusion 86 Binders 59,7276 PressBench 66 13,16 Silica Beads Beads PressBench 22,6465666771 73, 7475 Ball Dispenser12,22 Automated Press 64 Auto-Fill System 34 Auto 32 Extractor 21 Geno/Grinder Application Notes Alumina Ceramic 47,48505960 Agate Vial 46 Set AgateSet Vial Agate ball46,4748495054102 Agate for 12 Geno/Grinder Adjustable Clamp Adapters for 49 Mixer/Mills Adapters for Freezer/Mills Zirconium 13,16 Beads Freezer/mill 40 Agate, samplespecifications 46,4748495054102 for 12 MiniG 31, 38 102 SUBJECT INDEX Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 113 77 46, 47, 53 5100 45, 105 6970EFM Freezer/Mill 30 Freezer/Mill 6970EFM 8000D 44 K2 Prime 80 K2 Prime MiniG 10 6870 Freezer/Mill 28 Freezer/Mill 6870 Paraffin Binder 70, 72, 76 Paraffin Effects 71 Size Particle dies 70, 75 Pellet 70, 73, 74, 76, Pelletizing Ordering Information 110 Information Ordering Nonwetting agent 89 agent Nonwetting Accessories 49 Accessories Samples & After 52 Mixer/Mill Before Molds 81, 82 Mulls 105 92, 93 Film Window Mylar Manual presses 67 Manual presses 42, 51 Mechanical Alloying Methacrylate 46, 47 set 27, 28, 29, 31, 33 Microvial 94 Micro X-Cells Minimum 110 Orders Mixer/Mill 42 8000M 43 , 68, 70 Laboratory 7 presses 84, 85, 88 Lithium borate Kryo-Tech 17 Kryo-Tech Kapton Window Film 92 Film Window Kapton Katanax 78 79 K1 Prime Grinding Containers, Shatterbox 59, 60, 62 Shatterbox Grinding Containers, Grinding, 22, 111 media 19 Geno/Grinder 8 2020 Geno/Grinder 11 Freezer/Mill 26 Freezer/Mill 27 Freezer/Mill 6770 platinumware 81 platinumware cylinder center 31, 32 Polycarbonate Geno/Grinder 15 for Vial Polycarbonate Mixer/Mill 15, 48 for Vial Polyethylene 37, 93, 96 Polypropylene Vial Polystyrene P O N M L K G F Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX PRODUCT INDEX 114 T S R Z Y X W V U Tungsten Carbide 46,474850 Titer Plates 14 Thin Film 92 70,74759194 Spec-Caps 95 rings Snap-on 69,7071747691 Sleeve-and-Plunger 47,495054 Silicon Nitride 13,1622 Beads Silica Grinding Shipping 110 Shatterbox 52,565758596162103104105 24 ShaQer 26,3139102 RoHS/WEEE Shipment 111 Return 17,325981 Racks Press 64,65667073104105107 Prep-Aid 49,59697072747691 Pre-Flared 75 Spec-Caps Zirconium 13,1682102 Zirconia 47,48505459102 Yeast 19 XRF 3,7396465666769707273 X-Press 5,64657073105107 X-Cell 70,919294959697107 Warranty 110 Vertrel 104,107 Ultralene 93,96107 Ultrabind 70,76104107 , 5354596068 , 85 -79 - 97, 104 PRODUCT INDEX Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 115 age Number P

Tray for MiniG ...... 12 for Tray or 50 mL Centrifuge Tubes ...... 17 Tubes or 50 mL Centrifuge ...... 17 Tubes or 15 mL Centrifuge inding Resin, 100-400 μm ...... 13 inding Beads, 400-600 μm ...... 13 inding Beads, 400-600 μm ...... 13 inding Beads, inding Resin, 100-400 μm ...... 13 er...... 24 in Magnet ...... 12 ack of 12 Magnetic Tips...... 12 ack of 12 Magnetic Well Titer Plate, Case of 100 ...... 15 Case Plate, Titer Well Well Titer Plate, Case of 100 ...... 14 Case Plate, Titer Well Well Titer Plate, Square Wells ...... 14 Wells Square Plate, Titer Well of 100 ...... 14 Case Wells, Square Plate, Titer Well Wells...... 14 Round Plate, Titer Well of 100 ...... 14 Case Wells, Round Plate, Titer Well ...... 14 Plate Titer Well conium Grinding Beads, 200-400 μm ...... 13 Grinding Beads, conium inding Balls, 7/16 in. (11 mm ...... 12 7/16 inding Balls, inding Ball Dispenser...... 12 in. (4 mm ...... 12 5/32 inding Balls, in. (9.5 mm ...... 12 3/8 inding Balls, iniG...... 10 eno-Grinder...... 8 djustable Clamp for MiniG ...... 12 for djustable Clamp ap-Mat for 2230 Titer Plate ...... 15 Plate Titer ap-Mat 2230 for of 10 ...... 15 Case Plate, Titer ap-Mat 2230 for ap-Mat for 2220 Titer Plate ...... 14 Plate Titer ap-Mat 2220 for of 10 ...... 14 Case Plate, Titer ap-Mat 2220 for ap-Mat for 2200 Titer Plate...... 14 of 10 ...... 14 Case Plates, Titer ap-Mats 2200 for ...... 14 Plate Titer ap-Mat 2210 for of 10 ...... 14 Case Plate, Titer ap-Mat 2210 for roduct Name eramic Grinding Cylinder, 3/8 in. x 7/8 in ...... 14 Grinding Cylinder, eramic 5/16 in. x 5/8 in ...... 14 Grinding Cylinder, eramic 5/32 in. x 5/16 in ...... 14 Grinding Cylinder, eramic ial Rack ...... 17 eparator for 24-Pin Magnet ...... 12 24-Pin for eparator ow Binding Zirconium Beads, 200 μm ...... 13 Beads, Binding Zirconium ow ow Binding Zirconium Beads, 100 μm ...... 13 Beads, Binding Zirconium ow ow Binding Silica Beads, 800 μm...... 13 Binding Silica Beads, ow 400 μm...... 13 Binding Silica Beads, ow 100 μm ...... 13 Binding Silica Beads, ow oam holder for MiniG ...... 17 for oam holder C 48- 48- C C 24- C 96- C C 96- 96- C C C C V Holder f Holder f 96- L Silica Gr Silica Gr Zir L L C Gr Gr L Silica Gr Silica Gr L Nesting G Gr 24-P 12 P S Gr P ShaQ M F A

PRODUCT INDEX 2230-100 2231 2231-10 2220-100 2221 2221-10 2211 2211-10 2220 2201-10 2210 2210-100 2200 2200-100 2201 2185 2190 2196-16-PE 2197 2182 2183 2184 2171 2180 2181 2167 2168 2170 2156 2162 2165 2166 2110S 2150 2155 2100 2110M 2110M-12 1690 1690T 2010 Product Number 1500 1600 1680 Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX PRODUCT INDEX 116 3118A 3118 3117B 3117 3116PC 3116 3114SB 3112 3111 2666 2665 2664 2663 2662 2661 2660 2650 2600 2305-2800SS 2304-800AW 2304-400AW 2304-100AW 2303-MM3 2303-MM2 2302-3000AW 2302-200AW 2302-1700AW 2302-1400AW 2302-100AW1 2302-1000AW 2301-100MB 2300 2260 2255 2253-PC-48 2253C-48 2252-PC-30 2251PC 2250 2241-PEF-200 2241-PC 2240-PEF 2240-PC 2231-10 Number Product

A A Har Har 5 mLP P S M P C C C C C C C C C 2 mL 2 mL 2 mL 2 mL 2 mL 2 mL 2 mL 2 mL 2 mL 2 mL 2 mL 2 mL 2 mL Holder f C C P C P P P F P P P C P rosted Polyethylene Vial, 5mL...... 15 tainless Steel ...... 48 BallSet olystyrene Vial ...... 46 olystyrene Vial ...... 46 olycarbonate Vial, 50mL...... 15 olycarbonate Vial, 15mL, Tall ...... 15 olycarbonate Vial, ...... 15 15mL,Short olycarbonate Vial, 5mL...... 15 re-Cleaned Polycarbonatere-Cleaned Vial 15mL...... 15 Set, Frostedre-Cleaned Polyethylene Vial 5mL...... 15 Set, Polycarbonatere-Cleaned Vial 5mL...... 15 Set, roduct Name roduct ap for 2253-PC-48...... 15 for 2230 ap-Mat Titer Plate ...... 15 ryo-Block for 48 Micro-centrifuge orPCR for 48Micro-centrifuge Tubesryo-Block ...... 18 orPCR for Micro-centrifuge Tubesryo-Block ...... 18 for 50mLCentrifuge ryo-Block Tubes ...... 18 for 4mLPolyethyleneryo-Block Vials ...... 18 for 4mLPolycarbonateryo-Block Vials ...... 18 for 15mLCentrifuge ryo-Block Tubes ...... 18 for 15mLPolycarbonateryo-Block Vials ...... 18 forryo-Adapter Titer Plates ...... 18 ...... 17 ryo-Station for 2255 ryo-Block Vial ...... 18 Grinding ryogenic Vial Pack ...... 17 gate Ball ...... 48 gate Vial ...... 46 Set ethacrylate Balls ...... 48 ethacrylate dened Tool Steel ...... 48 BallSet dened Tool Steel Vial ...... 46 Set Tube with2.8mmStainless Steel Balls...... 17 Tube ...... 16 with800μmSilicaBeads Tube ...... 16 with400μmSilicaBeads Tube ...... 16 with100μmSilicaBeads Tube 3...... 16 withMixed Matrix Tube 2...... 16 withMixed Matrix Tube with3mmZirconium ...... 16 Beads Tube with200μmZirconium ...... 16 Beads Tube with1.7mmZirconium ...... 16 Beads Tube with1.4mmZirconium ...... 16 Beads Tube with100μmZirconium ...... 16 Beads Tube with1.0mmZirconium ...... 16 Beads Tube ...... 16 with100μmSilicaBeads olycarbonate Vial ...... 46 or 2mLmicrofuge Tube ...... 17

P age Number PRODUCT INDEX Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 117 age Numberage P

amplePrep-Carver Model C ...... 67 amplePrep-Carver Model M ...... 67 e-and-Plunger Set – 31 mm ...... 69 e-and-Plunger Set – 40 mm ...... 69 e-and-Plunger Set – 35 mm ...... 69 -Free Cell Insert Cell ...... 91 -Free et – 35 mm ...... 68 et – 13 mm ...... 68 et – 40 mm ...... 68 et – 10 mm ...... 68 -Cap – 30 mm ...... 90 -Cap – 38 mm ...... 90 -Cap® - 30 mm ...... 90 -Cap – 33 mm ...... 90 -Cap – 33 mm ...... 90 -Cap – 38 mm ...... 90 teel Pellets – 31 mm ...... 68 Pellets teel alene® Pre-Cut Circles ...... 93 alene® Pre-Cut Circles alene® Window Film (Roll ...... 93 Film Window alene® dened Tool Steel Vial Set ...... 46 Vial Steel Tool dened ylar® Pre-Cut Circles (Large ...... 92 (Large ylar® Pre-Cut Circles (Roll ...... 92 Film Window ylar (Roll ...... 93 Film Window ylar ...... 93 ylar Pre-Cut Circles ethacrylate Balls ...... 48 roductName apton Pre-Cut Circles ...... 92 Pre-Cut Circles apton apton® Window Film (Roll ...... 92 Film Window apton® -Cell, 31 mm Double Open End X-Ray Cell ...... 92 Cell 31 mm Double End X-Ray Open -Cell, ...... 92 Cell 31 mm Micro X-ray -Cell, -Cell, 31 mm Closed X-Ray Cell ...... 91 Cell 31 mm Closed X-Ray -Cell, ...... 91 Cell Closed X-Ray 31 mm Universal -Cell, ...... 92 Cell 43 mm Closed X-Ray -Cell, -Cell, 40 mm Closed X-Ray Cell ...... 91 Cell 40 mm Closed X-Ray -Cell, re-Flared Spec-Capre-Flared – 31 mm ...... 90 re-Flared Spec-Capre-Flared – 31 mm ...... 90 olypropylene Pre-Cut Circles ...... 93 Pre-Cut Circles olypropylene teel Pellets – 40 mm ...... 68 Pellets teel – 35 mm ...... 68 Pellets teel teel Pellets – 13 mm ...... 68 Pellets teel dge-Flaring Tool ...... 91 Tool dge-Flaring dge-Flaring Tool ...... 91 Tool dge-Flaring ungsten Carbide Pellets – 35 mm ...... 68 – 35 mm Pellets Carbide ungsten ungsten Carbide Pellets – 40 mm ...... 68 – 40 mm Pellets Carbide ungsten Spec 3621 SPEX S 3622 SPEX S ST S Die Sleev E Spec Spec E Spec P P Die Sleev Spec Spec Die S T S Die Sleev Die S Die S S Die S T S X Bubble X X X X X M M M P Ultr Ultr P M Har K K M

3625 3622 3623 3623W 3619AM 3619AM 3619M 3621 3617M 3618 3619 3619A 3616ST 3616W 3617 3615M 3616 3616C 3614ST 3614W 3615 3613 3613ST 3614 3614C 3571 3577 3610 3529 3561 3565 3526 3527 3527I 3518 3521 3525 3512 3515 3516 3517 3119 3127 3511 Product Number Page Number Page

Product Name Product Number Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX PRODUCT INDEX 118 Product Number Number Product 6883 6881C4 6881C20 6881 6871 6870S 6870M 6870L 6870D 6870 6820 6814 6807 6805 6804 6802 6801C4 6801 6781S 6771 6770 6761 6757 6755 6754 6753C 6751C20 6751C4 6751 6135 6134 6133PC 5100 5004C 5004A 5004 3650 3646-450 3646-150 3644-450 3644-150 3642-150 3636

P M M M M Lar Small M Lar 6870D F 6870 F A A M V Ex Lar Lar Lar Small S Small C 6770 F Small P M V Ex M Small P Small P Small Gr P P P SPEX S M T T P P P P P P A ungsten ...... 48 Carbide BallSet ungsten Carbide-Lined Vial ...... 46 Set roduct Name roduct olyethylene Vial ...... 48 olystyrene Vial ...... 48 olycarbonate Vial ...... 46 repAid Vertrel® XF...... 49 repAid Paraffin Binder – (CnH2n+2 ...... 91 repAid Paraffin Binder – (CnH2n+2 ...... 91 repAid UltraBind® ...... 91 repAid UltraBind® ...... 91 repAid Cellulose Binder...... 91 ial Rack forial Rack Large Vials ...... 32 forial Rack Small Vials ...... 32 uto-Fill System for the6870Freezer/Mill ...... 34 forutoExtractor™ Freezer/Mill® Vial ...... 32 Sets utomated X-Press® ...... 65 ulti-Vial Adapter ...... 32 ethacrylate Centerethacrylate Cylinder ...... 46 id-Size Cr-Free Vial ...... 32 id-Size Polycarbonate Center Cylinder ...... 32 id-Size Polycarbonate Center Cylinder ...... 32 id-Size Vial ...... 32 Set id-Size Vial Package Accessory ...... 33 icrovial ...... 31 Set icrovial Extraction Sample Tool ...... 33 tractor/Vial Openerfor Large andMid-Sized Vials ...... 32 tractor/Vial Openerfor Small Vials ...... 32 ge Cr-Free Vial ...... 31 Set ge Vial Package Accessory ...... 33 ge Steel Center Cylinder ...... 31 ge Polycarbonate Center Cylinder ...... 31 ge Grinding Vial ...... 31 Set Vial Package Accessory ...... 33 reezer/Mill® ...... 28 reezer/Mill® ...... 27 amplePrep ...... 45 5100Mixer/Mill® tainless Steel Grinding Vial ...... 31 Set oly-Vial ...... 31 Set olycarbonate Center Cylinder ...... 31 olycarbonate Center Cylinder ...... 31 r-Free Vial ...... 31 Set reezer/Mill® ...... 29 inding Vial ...... 31 Set

P age Number PRODUCT INDEX Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX 119 age Numberage P

reezer/Mill® ...... 30 reezer/Mill® or 8003 Vial Set ...... 47 Vial or 8003 Vial Mixer/Mill® ...... 43 Vial t Tongs ...... 81 Tongs t t Cryogenic Transfer Hose ...... 34 Transfer t Cryogenic on Nitride Vial Set ...... 47 Vial on Nitride on Nitride Ball ...... 49 tterbox® ...... 56 tterbox® dened Steel Grinding Container ...... 59 Grinding Container dened Steel dened Steel Vial Set ...... 47 Vial dened Steel conia Ceramic Vial Set ...... 47 Vial Ceramic conia Ball ...... 48 Ceramic conia aphite Crucibles ...... 82 Crucibles aphite ...... 82 Crucibles aphite aphite Crucibles ...... 82 Crucibles aphite ...... 82 Crucibles aphite id-Size Vial Adapter ...... 33 Adapter Vial id-Size ...... 32 Poly-Vial id-Size ...... 33 Adapter Vial id-Size ethacrylate Vial Set ...... 47 Vial ethacrylate ultiple-Sample ...... 49 Adapter ultiple-Sample ...... 49 Adapter ual Mixer/Mill® ...... 42 lumina Ceramic Ball ...... 48 lumina Ceramic lumina Ceramic Vial Set ...... 47 Vial lumina Ceramic gate Ball ...... 47 gate Ball ...... 49 gate Set ...... 49 Vial 6133 for dapter ryogenic Gloves ...... 34 ryogenic Gloves roductName ack ...... 81 ial Clamp Adapter for the 8000D Mixer/Mill the 8000D ...... 49 for ial Clamp Adapter ound-Ended Hardened Steel Vial Set ...... 47 Vial Steel ound-Ended Hardened olystyrene Vial ...... 47 Vial olystyrene ortable Pressurized Cryogenic Cylinder ...... 34 Cryogenicortable Cylinder Pressurized ortable Cryogenic Dewar, 25 L Capacity 25 ...... 34 ortable Cryogenic Dewar, teel-Jacketed Tungsten Carbide Vial Set ...... 47 Vial Carbide Tungsten teel-Jacketed Set ...... 47 Vial tainless Steel Ball Set ...... 49 tainless Steel teel Ball Setteel ...... 48 ong Tongs ...... 81 Tongs ong ong Cryogenic Transfer Hose ...... 34 Transfer ong Cryogenic ungsten Carbide Grinding Container ...... 59 Grinding Carbide Container ungsten ungsten Carbide Vial Set ...... 47 Vial Carbide ungsten Ball ...... 48 Carbide ungsten T A A Clamp f A Sha Har Silic Silic R M M V T S Zir Zir M S S Har S P A A T Gr Gr Shor Gr Gr D Single Shor L P Enclosed F R L P M M M C P

8501 8504 8015 8017 8500 8011 8012 8014 8014A 8008A 8009 8010 8007 8007B 8008 8005 8005A 8006 8003A 8004 8004A 8004SS 8001B 8002 8003 8000D 8000M 8001 7154 7160 7162 7151T 7152 7152HP 6907 6910 6970EFM 7151R 6900 6905 6906 6884 6885 6886 Product Number Page Number Page

Product Name Product Number Order 24/7 online: www.spex.com. Call: 1-855-GET-SPEX PRODUCT INDEX 120 Product Number Number Product KP5606A KP5605A KP5604A KP5603A KP1015A KP1011A KP1010A KP1009A KP1008A KP1007A KP1006A KP1005A KP1004A KP1003A KP1002A KP1001A KP0049A KP0040A KP0039A KP0038A KP0037A KP0010A K2P K1P 8530 8521 8508 8507R 8507 8506 8505

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