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Introduction

Handbook of SAMPLE PREPARATION and HANDLING
Eleventh Edition Contributing Editors Ralph H. Obenauf, Ph.D. John Martin Richard Bostwick Tim Osborn-Jones Lea Anderson-Smith, Ph.D. Ben Murray Keith Tucker Dave Samuels Sandy Mangan Steve Siniscalco Sarah Geiger SPEX SamplePrep, LLC 15 Liberty St. Metuchen, NJ 08840 Phone: (732) 623-0465 Fax : (732) 906-2492 Email : sampleprep@spexcsp.com Web: www.spexsampleprep.com European Division: SPEX Ceriprep Ltd. 2 Dalston Gardens Stanmore Middlesex HA7 1BQ United Kingdom Phone: +44 (0) 208 204 6656 Fax : +44 (0) 208 204 6654 Email: sales@spexcertiprep.co.uk Web: www.spexsampleprep.com

Order Online 24/7: www.spexsampleprep.com

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Introduction

Introduction

Introduction
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. SPEX SamplePrep equipment is used to prepare samples for a wide range of analytical technologies including XRF, AA, and ICP. Much of our equipment is also used for cutting-edge research in pharmaceuticals, superconductors, polymers, forensics and genetics.

Our Customers
For the past five 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 Mining Geology and Mineralogy Polymers RoHS/WEEE Medicine and Genetics • • • • • Pharmaceuticals and Drug Testing Cosmetics Forensics and Crime Scene Investigation Environmental Protection and Remediation Food and Agriculture

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

How To Order
By Mail Mail your orders to: SPEX SamplePrep, LLC 15 Liberty St Metuchen, NJ 08840 By Phone (732) 623-0465 – US +44 (0) 208 204 6656 - UK By Fax (732) 906-2492 – US +44 (0) 208 204 6654 – UK Via email sampleprep@spexcsp.com – US sales@spexcertiprep.co.uk - UK By Web www.spexsampleprep.com

Our Quality
SPEX SamplePrep equipment has become the industry standard for reliability and durability in the laboratory and our products have been used in landmark studies such as those of NASA’s moon rocks and the identification of the remains of Czar Nicholas II and his family. Our expertise and products can help you achieve accurate, consistent results by ensuring reproducible samples, analysis after analysis. Let our five decades of sample preparation experience work to your advantage in the lab.

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Order Online 24/7: www.spexsampleprep.com

Order Online 24/7: www.spexsampleprep.com

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Introduction

Introduction

We are pleased to announce the launch of our brand new website to support the growing demand for our products and services. Our website offers a complete e-commerce solution to aid in your purchase of laboratory equipment and accessories for every sample size and application. Registering on our website is a simple process and gives you access to: • Product Offering and Pricing • Online Ordering • Order Status & Order History - Check your complete order history • Live Chat - For all the questions you need answered immediately, our sales staff can assist you • Newsletters - Register for our newsletters to receive all the latest updates on SPEX SamplePrep equipment and for exclusive offers and promotions

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 FCA Ex Works 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. All shipping charges are prepaid and the cost is 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.

Log on today to find out why SPEX SamplePrep is the better solution:
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When placing your order please include:
SPEX SamplePrep Account Number (if known) Purchase Order Number Billing Address Shipping Address Catalog number (in full as shown herein) Quantity (in units, not pieces) Item Description Preferred Shipping Method Payment Method Tax Exempt Number (if applicable) Copy of Tax Exempt Certificate (if applicable)

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 an authorized dealer in your country visit our website or contact SPEX SamplePrep via email at sampleprep@spexcsp.com. Orders from countries without authorized SPEX SamplePrep dealers may be placed directly with SPEX SamplePrep, 15 Liberty St., Metuchen, NJ 08840. However, export ordering terms, instructions, and quotations must be obtained in advance. Orders received without prior agreement may be returned to the purchaser.

Distributors
SPEX SamplePrep distributes products through a global distribution network. To find a distributor in your country please visit: www.spexsampleprep.com/purchase-options/distributors.aspx Alternatively you can contact our main office for more information on distributors in your country.

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Order Online 24/7: www.spexsampleprep.com

Order Online 24/7: www.spexsampleprep.com

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Minimum order for letter of credit payments is $2. negligence or misuse. the Geno/Grinder ball slide.spexsampleprep. specifications are subject to change without notice. but also pneumatic cylinders. alumina ceramic. The customer pays return freight for warranty claims. Metuchen NJ 08840. silicon nitride.com Order Online 24/7: www. Cost for all return transportation is the responsibility of the customer. but SPEX SamplePrep will pay return freight to the customer if the warranty claim is valid. MasterCard. The customer pays freight both ways for equipment to be serviced. LLC. The warranty excludes wear parts: parts that wear out through use and have to be replaced periodically for proper operation. New Jersey. Also excluded from the warranty are grinding vials and containers made from tungsten carbide. upgrade. Minimum Orders The minimum order is $100. or to wear.00. The SPEX SamplePrep Service Department is an integral part of our operation. Our trained service technicians can also advise you on the most likely cause of a problem. always include the RMA number. and include a purchase order with the return. and returns are subject to a 25% restocking fee up to a maximum of $200. and agate. Warranty SPEX SamplePrep LLC guarantees its products against defects of materials and workmanship for one year from the date of original shipment. To Arrange a Return Shipment We want you to be happy with your purchase from SPEX SamplePrep. Address all shipments to SPEX SamplePrep. repair. and the Mixer/Mill clamp retaining spring assembly. Hard ceramic parts may exhibit small cracks developed under heat.00. American Express). but DO NOT RETURN any item before contacting us for a RMA (Returned Materials Authorization) number. contact our technicians for an RMA number and cost estimate. or rebuild SPEX SamplePrep equipment with factory parts and the necessary expertise. grinding media. and prices are subject to change without notice.com 7 . SPEX SamplePrep does not recommend unattended operation of any of our laboratory equipment. Product Specifications Every effort has been made to provide complete and accurate product information in this catalog. Payment may be made by check. 6 Order Online 24/7: www. Before returning equipment for service. zirconia ceramic. drive belts. Repairs are subject to a minimum two-hour labor charge. Unauthorized returns will be refused. 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. and the like. and can be counted on to maintain. wire transfer. Precautions SPEX SamplePrep products are not for any household application. Wear parts include not only gaskets. and will not be considered defective unless this situation impairs functionality of the instruments.Introduction Introduction Payment Prepayment of merchandise cost and shipping charges is required for all export orders.spexsampleprep. Service The majority of our products are designed and built in our factory in Metuchen. All banking charges must be to buyer’s account. letter of credit. Repairs and replacements made under warranty are guaranteed for the remaining original warranty period. 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. Replacement parts and repair charges are excluded from this minimum. the Freezer/Mill coil..500. However. Out-ofwarranty repairs and parts are guaranteed for 30 days. or credit card (Visa. SPEX SamplePrep reserves the right to judge whether a malfunction is due to defects in materials or workmanship. Any letter of credit that states “banking charges are for the account of the beneficiary” WILL NOT BE ACCEPTED. and changes may be made from time to time to improve the performance of our products. Please bring any problem to our attention. and instructions. 15 Liberty St. Users are responsible for knowledge and understanding of the potential hazards of the material with which they are working. Address returns to our 15 Liberty St. address as described above. Heating elements are warranted for a period of six (6) months. Credit for returned merchandise is issued only after the goods have been received and inspected.

. . . . . . . . . . SPEX SamplePrep’s laboratory presses are ideal for preparing sample discs for these methods. . . . . . . . . . . . . . . . . 19 Titer Plates and Cap-Mats . . . . . SPEX SamplePrep’s Geno/Grinder and Freezer/Mills aid scientists by providing high-throughput sample preparation solutions at both ambient and cryogenic temperatures. . . . . . . . . 28 Mixing & Blending The non-homogeneity of materials in the real world presents a serious sampling problem for scientists. .spexsampleprep. . . . . . . . . . . . . . . . . . . . . . . Our vast line of equipment and accessories are used for a variety of common techniques as well as specialties. . . . . Table of Contents Introduction How to Use This Handbook . . . . . . . . . . . . . . . . . Good techniques are the foundation to ensuring high quality. . . . . . 37 Liquid Nitrogen Handling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . pharmaceuticals. . . . . . . . . . . . . . . . . . . . . . . . . . .spexsampleprep. . . . . . . . . . . . . . . . . . . . . . and cosmetics as well as samples that require mixing for effective extraction with a solvent or buffer. . . . . . . . . . . . . . . . . . . . . . . our automatic and air-actuated presses are designed to fit on the bench top. . . . . . . . . . . . . . . .com Chapter 3 SPEX SamplePrep 8000D Dual Mixer/Mill® . . . . . . . . . . . . . . . . . . . 35 Extractors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18 Accessories . . . . . . . . . . . 30 SPEX SamplePrep 6870 Freezer/Mill® . OES. . . . . . . . . . . . plant and animal tissue. . powders. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . AA. . . . . SPEX SamplePrep’s mills are effective at mixing and blending dry materials such as pigments. . . 27 Kryo-Tech® . . 32 Accessories . 40 SPEX SamplePrep 8000M Mixer/Mill® . . . . . . . . . . . . . . 19 Grinding Media . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15 Sample Preparation Techniques Reference Chart . . . . . . . . . . . . . difficult to dissolve in acid (zirconia and alumina). . . . . . . . . . . . . .com 9 . . . . . . . . . . . . . . SECTION 1 :: Products and Accessories Chapter 1 SPEX SamplePrep 2010 Geno/Grinder® . . . . . . . . . . . In addition. This versatility allows for grinding of a wide variety of samples. . . . . . . . . . . . . . . . 19 Clamps . . . . . . . . 28 Cryo-Blocks . . . 8 Grinding & Pulverizing SPEX SamplePrep’s laboratory mills and grinders are capable of pulverizing samples in both ambient and cryogenic environments. . . . pharmaceuticals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Below is a short description of each technique along with some insight into the use of our equipment. . . . Tissue Homgenization /Cell Lysis For Biotechnology and Forensic applications. . . . . . . . or both (metal ores and silicate rocks). . Chapter 2 SPEX SamplePrep 6970EFM Enclosed Freezer/Mill® . . . . . . . 35 Sample Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . plastics. . . . . . . . . . . and more. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38 Pressing & Pelletizing Analytical spectroscopic methods such as XRF. rocks. 36 Accessory Packages & Kits . flat-surfaced disc. . . . . and IR often require samples in the form of a round. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . and ICP. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . borate fusions are widely used. . . . . . requiring less space than standard floor model presses. . . . . . . . . . . . . . . . . . . 8 Order Online 24/7: www. such as cryogenic grinding. . . . . . . . . . . effective cell disruption and DNA/RNA extraction are critical. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Borate Fusion For samples that are difficult to prepare as homogeneous pressed powders (cement). . . . . . . . . . . . . . . . . . bone. . reliable analytical results. . . . . .Introduction Table of Contents Sample Preparation Techniques Sample preparation techniques are the building blocks used to prepare samples for specific scientific analyses. . . . . . . . . . . . . . 33 Vial Racks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . SPEX SamplePrep offers the full line of Katanax Electric Fusion Fluxers & SPEX CertiPrep Fusion Flux for preparation of samples for XRF. . . . . . . . . . . . 31 SPEX SamplePrep 6770 Freezer/Mill® . . . . . . . . . . . . . . . . . . . . . . . 41 Order Online 24/7: www. . . . . . . . . . . . . . 23 Racks and Holders . . . 33 Vials & Vial Sets . . . . . including metals. . . . . . . 22 Vials and Vial Sets . . . .

. . . . . . . . . . . . . . . . . . .com 11 . . . . . . 82 Chapter 4 SPEX SamplePrep 8530 Enclosed Shatterbox® . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92 Limits of Cryogenic Grinding . . . . . . . . . . . . . . . . . . . . . . . . . . 67 10 Order Online 24/7: www. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43 Small Vials and Vial Sets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43 Large Vials and Vial Sets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47 Grinding Media . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54 PrepAid® Grinding Aids & Sample Binders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67 Molds & Mold Holders . 62 SECTION 2 :: Technical Information Chapter 1 Tissue Homogenization / Cell Lysis . . . . . . . 67 Accessory Packages & Kits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94 Grinding Tests with the Freezer/Mill . . . . . . . . . 81 Services available from the CRM Division . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97 Grinding Container Materials . . . . . . . . .spexsampleprep. . . . . . 44 Comparison of Grinding Vials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .com Chapter 6 Katanax® K1 Prime Automated Electric Fluxer . . . 50 SPEX SamplePrep 8500 Shatterbox® . . . . . . . . . . . . . . . . 72 Chapter 7 XRF Accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69 Fusion Flux and Additives . . . . . . . . . . . . . . 51 Accessories . . . . . Labware & Handling Tools . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93 Guide to Freezer/Mill Sample Capacity . . . . . . . . . . . . . . . . . . . .Table of Contents Table of Contents SPEX SamplePrep 5100 Mixer/Mill® . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66 Accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43 Vials & Vial Sets . . . . . . . . . 49 Platinumware. . . . . . . . . . . . . 49 SPEX SamplePrep PrepAid® Grinding Aids . . . . . . . . . . . . . . . . . . . . . . . . . . 59 Replacement Pellets . . . . . 58 Accessories . . . . . . . . . . . . 91 Key Points About Cryogenic Grinding . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88 SPEX SamplePrep Container Materials Selection Chart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42 Accessories . 93 Cryogenic Grinding for RoHS/WEEE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52 Racks and Holders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52 Grinding Dishes . . . . . . . . . . . . . . . . . . . . . . . 81 Products available from the CRM Division . . . . . . . . . . . 66 Racks & Holders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75 X-Cells . 66 Crucibles . . . . . . . . . . . . . . 60 Sleeve-and-Plunger Sets . . . . . . . . . . . . . . . . . . . . . . . . . 96 Key Points About Grinding . . . . . . . . 74 PrepAid Binders . . . . . . . . . . . . . . . . . . . 61 SPEX SamplePrep PrepAid® Binders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59 Pellet Die Sets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86 Chapter 2 Grinding & Pulverizing / Mixing & Blending . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88 How to Select a Laboratory Mill and Grinding Container . . . . . . . . . . . . . . . . . . . . . . . . . . . . .spexsampleprep. . . . . 86 Cryogenic Grinding . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65 Crucibles and Molds for Katanax K1 and K2 Automated Electric Fluxers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57 3626 SPEX SamplePrep-Carver 12-ton Press . 90 Composition of Standard Steels Used in SPEX SamplePrep Equipment & Accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97 Order Online 24/7: www. . . . . . . . . . . . . . . . 76 Thin Film . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86 Bead Milling . . . . . . . . . . . . . . . . . . . . 64 Katanax® K2 Prime Automated Electric Fluxer . . . . . . . . . . . . . . . . . . . . 88 When to Pulverize . . . . . . . . . . . . 68 Graphite Crucibles for muffle furnaces . . . . . . . . . . . . . . . . . 60 Spec-Caps® for Reinforcing XRF Sample Disks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78 Certified Reference Materials for Organic and Inorganic Spectroscopy and Chromatography . . . . . . . . . . . . . . . . . . . . . . . . . . 74 Spec-Caps® . 55 SPEX SamplePrep 3628 Air-Actuated Bench-Press® . . . . . . 68 Mold Holders and Plates for the K2 Prime Automated Electric Fluxer . . . . . . . . . . . . . . . . 54 Chapter 5 SPEX SamplePrep 3635 Automated X-Press® . . . . . . . . . . . . . . 67 Mold Holders for the K1 Prime Automated Electric Fluxer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58 3622 SPEX SamplePrep-Carver Model M . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56 3621 SPEX SamplePrep-Carver Model C . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48 Sample Adapters . . . .

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134 Chemical Resistance of Kapton® . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114 Set-Up and Loading of the SPEX SamplePrep Evacuable Pellet Die . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126 Additives for Fusions: Non-Wetting Agents. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 121 Trouble Shooting . . . 105 SPEX SamplePrep Shatterbox . . . . . . . . 122 Selecting a Pellet Die . . . 158 SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126 12 Order Online 24/7: www. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131 Selecting Thin Film Windows for XRF . . . 151 SP019: Comparison of Methods for the Isolation of DNA from Soybeans . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .com 13 . . . . . 111 Pressing Sample Disks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 124 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123 SECTION 3 :: Application Notes Geno Grinder . . . . . . . . . . . . . . . 145 SP014: RNA Extraction from Aspergillus parasiticus mycelium . . . . . . . . . . . . . . . . 148 SP017: Lysis Time and Other Variables on DNA Extraction . . . . . . . . . . . . . . . . . . . . . . 142 SP001: Cell Disruption . . . . . . . . 183 Chapter 4 Fusion . . . . . . . . . 130 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .spexsampleprep. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100 Pelletizing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119 Sample Disk Removal . . . . . . . . . .com Order Online 24/7: www. . . . . . . . . . . 99 Respiritory Protection . . . 100 SPEX SamplePrep Mixer/Mills . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109 How to Select a Fusion Flux . . . . . . . . . . . . . . . . . . . 156 SP021: Extraction of RNA/cDNA and Genomic DNA from Tissue with Real-Time PCR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153 SP020: Lysing of Bacterial Cells in the Geno/Grinder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 175 SP025: Lysing / Homogenization . . . . . . . . . . . . . . . . . 136 Chemical Resistance of Polypropylene . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .Table of Contents Table of Contents Contamination . . 107 Grinding Tests with the 8501 and 8504 Grinding Containers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 124 When to Employ Borate Fusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 146 SP016: Lysing / Homogenization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 127 Graphite Crucibles and Handling Equipment . . . . . . . . 117 Sleeve-and-Plunger Technique: Binder as Sample Disk Matrix . . . . . . . . 130 Bubble-Free Cell Insert . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102 Pulverizing and Blending Grinding Tests with 8000 Series Mixer/Mills . . . . . . . 98 Cleaning Containers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130 Reinforcing XRF Pellets with Spec-Caps . . . . . . . . . . . . . . . . . . . . . . 116 Binders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130 X-Cells for XRF Liquid Samples . . . . . . . . . . . . 114 The Use of the Vacuum in Pellet Pressing . . . . 119 Anti-Sticking Agents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 110 Particle Size Effects . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 162 SP023: Comparison of Pesticide Extraction in Agricultural Products . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139 Chapter 3 Pressing and Pelletizing . .spexsampleprep. . . . . . . . . . . . . . 110 Preparing Powder Samples for XRF . . . . . . . 98 Grinding Aids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . and Oxidizers . . . . . . . . . . . . . 120 Sample Disk Handling and Care . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100 Infrared Mulls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100 Mechanical Alloying . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 142 SP011: DNA Extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115 Proper Use of the SPEX SamplePrep Spec-Cap . . . . . . . . . . . . . . . . . . . . . . 128 Chapter 5 XRF Accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143 SP013: Grinding / Disruption . . Fluidizers. . . . . . . . . . . . 135 Chemical Resistance of Mylar® . . . . . . . . . . . . . . 149 SP018: High-Throughput Disruption of Yeast in a 96-Well Format . . . . 172 SP024: Pesticide Anaylsis: Standard QuEChERS vs Modified Method . . . . . . . . . 110 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . 124 How to Prepare a Fused Sample . . 132 Thin Film Transmission Characteristics . . . . . . . . . . . . . . 137 Chemical Elements and Their Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115 Care and Maintenance of the SPEX SamplePrep Evacuable Pellet Die . . . . . . . . . . . . . . . . . . . . . . 113 Technique for Pressing a Sample Disk . . . .

. . . . . . . . . . . . . . 208) makes it easy to locate information about particular products. . . . . . . . . . . . . . . . . . . . . . . . . . 207 Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . or analytical methods. . . . . . . . . . .Product information such as descriptions and catalog numbers for ordering • Section 2 . . . . . . . . . . . . . . . . . . . . . . . . . 216 How to Use the SPEX SamplePrep Handbook of Sample Preparation and Handling The SPEX SamplePrep Handbook can help you get the most from your analyses by increasing the reliability and reproducibility of your prepared samples. . . . . . . . A subject index (pg. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . and product comparison charts. . . . . . .com 15 . . . . . . . . . . fused glass disks. . .com Order Online 24/7: www. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 193 SP015: RNA Extraction . . . . 203 XRF Sample Preparation: Selected References . . . . . . . . . . . . . . .spexsampleprep. . . . . 208 Product Index . . . . . . . . . . . . . . .Our Application Notes library regarding the use of our equipment for your specific application Each chapter within these sections pertains to a particular product. 198 Katanax . . . . . . . 196 HT002: Crude Fat (Hexane Extractables) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . It suggests how the most heterogeneous. . . . . . . . . . . . as well as the sample preparation technique as it relates to a particular product. . . . . . . . . . . . 14 Order Online 24/7: www. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 196 SP003: Nano Technology . . . . . . . . . . . . . . . . samples. . . . . 203 Periodic table . . . . . . . . . . . . . . . . . . . . . . . . . 187 SP006: Milling/Blending (Homogenizing) . . . . . . . . . . . . . . . . . . or solutions. . . . . . . . . . . . . . . . . . . . . . . . . . . . 184 SP002: Ginding/Homogenization . . . . . . . . . . . . . . . . The Handbook is divided into 3 sections: • Section 1 . . . . .Table of Contents Introduction Freezer Mill . . . . . unmanageable materials can be transformed into samples ideal for your analysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . 189 SP007: Grinding/Homogenization . . . . . . . . . . 208 Subject Index . . . . . . . . . . . . . . . . . . . . 205 Trademark References . . . . . Procedural tips and applications-oriented product descriptions are supported by photographs. . . . . . . . . . . . . . . . . . . . protecting sample disks against breakage. . . . . . . . . . . . . . . . . . . . . . . . . . Margin tabs have been included to differentiate these areas. . . . . 206 Questionnaire for test grinding of Samples . . . . . . . . . .spexsampleprep. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A numerical product index (pg. . . . . . . inhibiting caking during pulverization. . . . . . . . . . . . . . 200 Appendix . . 216) helps you find product descriptions for SPEX SamplePrep laboratory equipment and supplies by model or catalog number. The sample preparation techniques are discussed in further detail at the end of this introduction. . . . . 194 Mixer Mill . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . homogeneous powders. . . . . . . . . . . . . 192 SP009: Reduction/Homogenization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 184 HT 001: Grinding Bone in the Freezer/Mill . . . . . . 190 SP008: Structural Changes in Polymers . 200 SP026: Preparation and XRF Analysis of Fly Ash Fused Beads . . . . The Handbook also includes a complete listing of reliable sample preparation products to make the analyst’s life easier. . . . . . . . . . . . . . . . . and copying with many other sample preparation difficulties. . . . . . . . . . . . . . . diagrams. . . . . . . . compressed powder sample disks. . . . . . . . . 185 SP005: DNA/RNA Extraction . . . . . . . sample preparation techniques. . . The Handbook also includes a complete listing of reliable sample preparation products to make the analyst’s life easier. . . . There are techniques for avoiding sample contamination. . . . . . . . . . . . . . . . . . . . . . . . . whether as fine. . . . . . . . . . . . . . . . . . . . . .Technical information associated with these products along with sample preparation techniques and application • Section 3. . . . . . . . . . . . . . . . . . . . . . . . . . . .

16 Order Online 24/7: www. Best of all.com 17 . Products Available For Demo: Katanax K1 Prime Electric Fluxer 8000D & 8000M Mixer/Mill 6770/6870/6970EFM Freezer/Mill 2010 Geno/Grinder 8530 Shatterbox 3635 X-Press Contact (732) 623-0465 Email: SamplePrep@spexcsp.com Katanax K1 Prime is only available for local demos.Would you like to test our sample preparation equipment with your own samples? Section 1 Products & Accessories Now You Can With SPEX SamplePrep’s Demo Program Contact SPEX SamplePrep to arrange a test grind in our labs by our experts. our demo program is complimentary! You only pay shipping and handling to and from your facility.spexsampleprep. Or try out our sample preparation equipment in your laboratory for one week. We recommend test samples be sent to us directly to be processed in our demo lab. Once you try our quality products you’ll ask yourself how you ever lived without them.

(9. vertical pulverizing motion • Handles two standard deep-well titer plates or multiple vials from 0. (39 kg) net 115V/60Hz or 230V/50Hz 3-prong standard North American plug for 115V/60Hz version 2-prong European CEE 7/7 plug for 230V/50Hz version 18 Order Online 24/7: www. or removes balls from magnets after balls are pulled out of wells or vials. and 3116PC vials in 2190 Vial Rack. racks. CE Approved • Versatile high-throughput plant and animal tissue homogenizer/cell lyser with a unique. Rubber mat for positioning between stacked titer plates is included. height • LCD screen displays the full timer setting along with the time. in minutes and seconds. 2100 Grinding Ball Dispenser Simultaneously dispenses one 5/32 in.spexsampleprep. Works with 2230 titer plate. enzymes. Specifications: Dimensions: Weight: Voltage: Power Cord: 25 ¼ in. the Large Capacity Clamp Assembly is available 2199 Large Capacity Clamp Assembly An oversized clamp that accommodates centrifuge tubes or a double load of titer plates. (36 cm) x 20½ in. vials. Grinding Media Grinding Balls & Magnets Stainless steel balls are useful for grinding large or tough samples.6 to 50 mL Patented and Patent Pending Accessories Clamps The 2010 Geno/Grinder is supplied with the Standard Size Clamp Assembly. (4 mm) steel grinding ball (2150) into each well of a standard 96-well titer plate.5 mm) steel grinding balls (2155) from 2110M 24-pin magnet.5 mm) steel grinding balls (2155) from titer plates and vial sets. including 2200 and 2210 titer plates. The choice of ball size should be determined based on the sample material and the size of the grinding vial. remaining in the grinding cycle Typical Samples and Applications • Plant materials such as seeds. Inserts or removes 3/8 in. stems.com 19 . and other configurations up to 2¼ in. (52 cm) 87 lbs. fruits. stacked two per side. Used with 2110S Separator. which is designed to accommodate two standard deep-well titer plates or a variety of small vials with a maximum height of 2¼ in (57 mm).Section 1 Chapter 1 Section 1 Chapter 1 SPEX SamplePrep 2010 Geno/Grinder® 2010-115 Geno/Grinder – For 115V/60Hz operation 2010-230 Geno/Grinder – For 230V/50Hz operation. or twenty-four standard 15 mL centrifuge tubes (119 mm length) with 2197 Holder. 2110S Separator for 24-Pin Magnet Separates 3/8 in. For taller vials or to stack titer plates. (9.spexsampleprep. (64 cm) x 15 in. 2110M 24-Pin Magnet 24 magnet-tipped pins on plate with handle. 2240-PC and 2240-PE Vial Sets. 2240-PC and 2240-PE Vial Sets. bacteria.com Order Online 24/7: www. roots. the grinding balls can be discarded or cleaned for re-use. Clamp also holds four deep-well titer plates. and yeast • Extraction of pesticide residue using QuEChERS Method • Extraction of oil from fish and seafood. Drops balls into 2230 24-well titer plates. • Optional large clamp assembly (2199) enables processing of up to four deep-well titer plates or sixteen 50 mL vials simultaneously • Controls allow the operator to set the run time in 5 second increments and precise vertical grinding speed between 500 and 1750 strokes per minute (SPM) • Sample preparation is completed in as little as 2 minutes with the addition of 1-2 grinding balls to the sample with a buffer solution • Safety interlocks and pneumatic cylinder stabilize the lid for safe operation • Supplied with height-adjustment spacers to handle titer plates. Designed to hold up to sixteen standard 50 mL centrifuge tubes (115 mm length) with 2196-16-PE Holder. After use. vegetables • Animal tissue • Isolation of nucleic acids (DNA/RNA). leaves. vigorous. proteins.

250 gram bottle. 2162 Low Binding Silica Beads. size ranges from 800-1000 µm. 2241-PC and 2241-PE Vials to grind extra large or tough samples. 100-400 µm Acid washed RNase/DNase-free treated irregular silica resin. 2171 Silica Grinding Resin. SPEX SamplePrep offers all three grades in a variety of sizes.spexsampleprep. size ranges from 400-600 µm. 5/32 in. 400 µm Acid washed and chemically treated to keep samples from binding to titer plate wells.Section 1 Chapter 1 Section 1 Chapter 1 2110M-12 Pack of 12 Magnetic Tips Each Magnetic Tip is a micropipette tip with a strong magnet. 200 gram bottle. 2161 Silica Grinding Beads. 5/32 in. (11 mm) Made of 440C stainless steel. x 5/8 in. Typically. 200 gram bottle. 250 gram bottle. They are suitable for most basic applications. 2180 Zirconium Grinding Beads. 2 cylinders are used per sample vial. Converts micropipette dispensers into pin magnets for removing 2150 grinding balls from 96-well titer plates. 3/8 in. Molecular Biology Grade. For use in 2230 titer plate or in 2190 Vial Rack with 3116PC. 5/16 in. Pack of 96 Magnetic Tips. Sold in bags of 100. 2167 Low Binding Silica Beads. 200 µm Acid washed and chemically treated to keep samples from binding to titer plate wells. 3/8 in. 2150 Grinding Balls. For grinding large or tough samples in 2230 titer plates and 2250 Vial Sets. Sold in bags of 5. 2185 Ceramic Grinding Cylinder. 2155 Grinding Balls. Grinding Beads Molecular Biology Grade Grinding Beads are treated to inactivate contaminating enzymes and have been tested accordingly. Sold in bags of 100. 2168 Low Binding Silica Beads. Large size ceramic grinding cylinder with angle-cut ends for use with standard 50 mL centrifuge tubes. 400-600 µm Acid washed RNase/DNase-free treated silica beads. x 5/16 in. 800-1000 µm Acid washed silica beads. Converts micropipette dispensers into pin magnets for removing 2150 grinding balls from 96-well titer plates. Order Online 24/7: www.spexsampleprep. 250 gram bottle. size ranges from 100-400 µm. 2156 Grinding Balls. 400-600 µm Acid washed silica beads. 20 Order Online 24/7: www. Sold in bags of 100. size ranges from 400-600 µm. 800 µm Acid washed and chemically treated to keep samples from binding to titer plate wells.com Grinding Cylinders Our ceramic cylinders are chemically inert and are useful when mixing samples for extraction methods such as pesticide residue analysis and extraction of oil from fish and seafood. 2166 Silica Grinding Beads. Medium size ceramic grinding cylinder with angle-cut ends for use with standard 15 mL centrifuge tubes. (9. The angle-cut ends help the cylinders to shear the sample matrix during processing.com 21 . 200 gram bottle. 200 gram bottle. 200 gram bottle. Used with 2100 Grinding Ball Dispenser and all 96-well titer plates. 200 gram bottle. (4 mm) Made of 440C stainless steel. Acid Washed Grinding Beads are treated to remove fine particles and contaminants. Pack of 12 Magnetic Tips. Molecular Biology Grade. 100 µm Acid washed and chemically treated to keep samples from binding to titer plate wells. 2182 Low Binding Zirconium Beads. size ranges from 800-1000 µm. Sold in bags of 100. 2110M-96 Pack of 96 Magnetic Tips Each Magnetic Tip is a micropipette tip with a strong magnet. 200 gram bottle. 200-400 µm Acid washed RNase/DNase-free treated zirconium beads. 2165 Silica Grinding Beads. 200 gram bottle. 2184 Ceramic Grinding Cylinder. 800-1000 µm Acid washed RNase/DNase-free treated silica beads. 200 gram bottle. Molecular Biology Grade. size ranges from 200-400 µm. Low Binding Grinding Beads are coated to reduce non-specific binding of nucleic acids and proteins and are used for lysing dilute samples of cells.000. resulting in a thorough extraction of analyte into the solvent. size ranges from 100-400 µm. Small size ceramic grinding cylinder with angle-cut ends for use with standard 5 or 15 mL centrifuge tubes. 100-400 µm Acid washed irregular silica resin. 100 µm Acid washed and chemically treated to keep samples from binding to titer plate wells. 2183 Ceramic Grinding Cylinder. 7/16 in. 2181 Low Binding Zirconium Beads. x 7/8 in. 2160 Silica Grinding Beads. Molecular Biology Grade. 2170 Silica Grinding Resin.5 mm) Made of 440C stainless steel. Sold in bags of 100.

but a single Cap-Mat. in a polyethylene carrier with foam vial holder. Round Wells. 2240-PC Pre-Cleaned Polycarbonate Vial Set. each set containing 24 vials pre-loaded with steel balls. but a single titer plate. Case of 10 sets. Case of 100 titer plates. 2230-100 24-Well Titer Plate.5 mm) steel grinding ball (2155). 2221 Cap-Mat for 2220 Titer Plate Same as above. Order Online 24/7: www. Case of 100 Rectangular 5 mL wells with a working capacity of 2 mL per well. Use with 2221 Cap-Mat and multiple 5/32 in. 2201 Cap-Mat for 2200 Titer Plate Same as above. Case of 10 Cap-Mats seal 2220 48-Well Titer Plates. 2220-100 48-Well Titer Plate. Case of 10 Cap-Mats. Square Wells. Grinding load per vial 1. Sold singly or in cases of 100. (4 mm) steel grinding balls (2150) per well. prevents leaks and cross-well contamination. used in pairs. Replacement vials and steel balls can be purchased separately.5 mm) steel grinding ball (2155) or 7/16 in. (9. but a single titer plate. each set containing 24 vials. Suitable for RNA extraction when used with 2600 Cryo-Station. 2221-10 Cap-Mat for 2220 Titer Plate. 5 mL. 2231-10 Cap-Mat for 2230 Titer Plate. Carrier fits Geno/Grinder clamp.4 mL wells with a working capacity of 2. 2231 Cap-Mat for 2230 Titer Plate Same as above. and one 3/8 in. Case of 10 Sealing mats for the 2200 Titer Plates. Case of 10 Cap-Mats. Case of 10 Cap-Mats seal 2230 24-Well Titer Plates. mother-to-daughter automated plate pipetting. Ready to use. 2210-100 96-Well Titer Plate. Cap-Mats seal titer plate wells. 2220 48-Well Titer Plate Same as above. which is inserted in gaps between wells to keep plates and samples chilled to preserve RNA for extraction. but a single Cap-Mat. Carrier fits Geno/Grinder clamp. Sold singly or in cases of 10. Case of 10 Each set includes 24 pre-cleaned 2241-PC vials. with alphanumeric marks for well identification. Round Wells Same as above. Case of 10 sets. (9. Vials can be filled and sealed individually. Case of 100 Square 10 mL wells with a working capacity of 4 mL per well. 2201-10 Cap-Mats for 2200 Titer Plates. in a polyethylene carrier with foam vial holder. used in pairs. rugged polypropylene. (9. 2211-10 Cap-Mat for 2210 Titer Plate. Titer plates are made of polypropylene. 2210 96-Well Titer Plate.0 mL. but a single Cap-Mat. Case of 10 Sealing mats for 2210 Titer Plates. above. For use with the 2650 Cryo-Block. but a single titer plate. 2200-100 96-Well Titer Plate. Case of 100 titer plates. but a single Cap-Mat. but a single titer plate. They can be used for many applications including sample libraries. Holds one 3/8 in. 2200 96-Well Titer Plate.5 mL.com 23 .5 mL. these sturdy titer plates have been tested extensively with various samples. alphanumeric marks for well identification. (11 mm) steel grinding ball (2156) per well. Case of 100 titer plates. Case of 10 Cap-Mats. Tough silicone rubber.com 22 Order Online 24/7: www. Vials can also be used with 2662 CryoBlock or 2190 Vial Rack. preventing spills and well-to-well contamination. Vials can also be used with 2662 Cryo-Block or 2190 Vial Rack. and resist perforation by steel grinding balls even at high clamp speeds. and the larger vials can hold bigger samples than titer plates. Case of 10 Each set includes 24 vials with screw-cap.5 mm) steel grinding ball (2155).0 mL wells. Vials and Vial Sets Vial sets are an alternative to titer plates. may be sterilized and re-used. Case of 100 Square 2. Case of 100 Round 2. 5 mL. 2211 Cap-Mat for 2210 Titer Plate Same as above. large sample dilutions and cell suspensions. Ready to use. Use with 2231 Cap-Mat. Can be sterilized and re-used.spexsampleprep. each with a 3/8 in. Sold in cases of 10 mats. Rugged silicone rubber. Grinding load per vial 1.Section 1 Chapter 1 Section 1 Chapter 1 Titer Plates and Cap-Mats While most titer plates can be used in the Geno/Grinder.spexsampleprep. 2240-PEF Pre-Cleaned Frosted Polyethylene Vial Set. Square Wells Same as above. 2230 24-Well Titer Plate Same as above.

2255C20 Polycarbonate Center Cylinder. Package of 100. 2255 Cryogenic Grinding Vial Pack Used to grind tough materials (e.com Order Online 24/7: www. bone) at cryogenic temperatures. 2 end plugs. 2253C-48 Cap for 2253-PC-48 Extra caps for the 50 mL Polycarbonate Vial. 2255C4 Polycarbonate Center Cylinder. (2. 5/8 in. Holds one 3/8 in. Sold in units of 240. long (12. each set containing 5 vials pre-loaded with steel balls. 2301-800MB 2 mL Tube with 800 µm Molecular Biology Grade Silica Beads Self-standing 2 mL microfuge tube with screw-cap. long (2. diameter x 2 in. Package of 100.1 cm). (11 mm) steel grinding ball (2156). Fits 2197 Holder and 2661 Cryo-Block.8 mm). 2302-100LB 2 mL Tube with 100 µm Low Binding Zirconium Beads Self-standing 2 mL microfuge tube with screw-cap.9 cm x 4. 2302-100AW2 2 mL Tube with 100 µm Acid Washed Zirconium Beads Self-standing 2 mL microfuge tube with screw-cap. diameter x 4 ¾ in. each with 1 cylinder.7 mm x 50.g. 2241-PEF-200 Frosted Polyethylene Vial. 6754 extractor required for end plug removal. diameter x 4 ½ in.4 cm). 15 mL. Ready to use. For use with 2199 Large Clamp Assembly.5 mm) steel grinding ball (2155). fits 2240-PC Vial Set. (11 mm) steel grinding balls (2156). Holds grinding media up to 1/2 in. diameter x 4 ½ in.9 cm x 11. 1 1/8 in. Grinding load per vial 6 mL.com 25 . Sold as a pack of 48 Vials. Grinding load per vial 6 mL.spexsampleprep. pack of 20 Pack of 20 replacement cylinders for 2255 Grinding Vial Set. diameter x 2 in. 2251PC Polycarbonate Vial. Grinding load per vial 6 mL. Not precleaned or pre-loaded with grinding ball. (2. 2250 Pre-Cleaned Polycarbonate Vial Set. Short Polycarbonate vial with screw-on cap. (9. and 2190 Vial Rack. 1/2 in. prefilled with 100 µm Low Binding Zirconium Beads. (9.7 mm x 50. Grinding load per vial 1. 1 1/8 in.4 cm). Tall Polycarbonate vial with screw-on cap. Fits 2196-16-PE Holder and 2664 Cryo-Block. Can be used with 2662 Cryo-Block or 2190 Vial Rack. Package includes four sets of cryogenic vials. prefilled with 800 µm Molecular Biology Grade Silica Beads. Holds grinding media up to 1/2 in. 1 1/8 in. 5 mL Polycarbonate vial with screw-on polyethylene cap. Holds one 3/8 in. prefilled with 1275 mg of 100 µm Acid Washed Zirconium Beads. 2253-PC-48 Polycarbonate Vial. Vials can also be used with 2660 CryoBlock. 50 mL Polycarbonate vial with screw-on cap. Grinding load per vial 20 mL. Holds all sizes of grinding media up to 7/16 in. Sold in units of 200.spexsampleprep. long (12. Package of 100. Grinding load per vial 1. 2660 Cryo-Block. each with a 7/16 in. 2301-400MB 2 mL Tube with 400 µm Molecular Biology Grade Silica Beads Self-standing 2 mL microfuge tube with screw-cap. long (1. Package of 100. Holds grinding media up to 3/8 in. Sold as a pack of 30 Vials. 2252-PC-30 Polycarbonate Vial.9 cm x 11. prefilled with 600 mg of 100 µm Acid Washed Zirconium Beads. in a polyethylene carrier with foam vial holder. 5 Ml Frosted Polyethylene vial with screw-cap. 50 mL Low density polyethylene vial with screw-on cap. Package of 100. 2302-100AW1 2 mL Tube with 100 µm Acid Washed Zirconium Beads Self-standing 2 mL microfuge tube with screw-cap.5 mL. prefilled with 400 µm Molecular Biology Grade Silica Beads. 15 mL. prefilled with 100 µm Molecular Biology Grade Silica Beads. Fits 2250 Vial Set.5 mL. Sold in units of 100. Not pre-cleaned or pre-loaded with grinding ball. 2254-PE-48 LDPE Vial. 2662 Cryo-Block. Grinding load per vial 20 mL. Carrier fits Geno/Grinder clamp.Section 1 Chapter 1 Section 1 Chapter 1 2241-PC Polycarbonate Vial. Sold as a pack of 48 Vials. Fits 2196-16-PE Holder and 2664 Cryo-Block. pack of 4 Pack of 4 replacement cylinders for 2255 Grinding Vial Set.5 mm) steel grinding ball (2155). Sold as a pack of 48. and 2 tungsten carbide balls. Package of 100.2 cm). diameter x 1 2/3 in. Case of 10 sets. 15 mL Each set includes 5 pre-cleaned 2251PC vials. 24 Order Online 24/7: www. used in pairs. For use with 2199 Large Capacity Clamp Assembly and 2260 Cryo-Block. 2301-100MB 2 mL Tube with 100 µm Molecular Biology Grade Silica Beads Self-standing 2 mL microfuge tube with screw-cap. 1/2 in. Pre-cleaned.8 mm).6 cm x 12.

1/2 in.8 mm Stainless Steel Balls Self-standing 2 mL microfuge tube with screw-cap. 2302-1000AW 2 mL Tube with 1. Package of 100. prefilled with 2. prefilled with 800 μm and 1. Sold in units of 100. For use with 2199 Large Capacity Clamp Assembly. 2197 Holder for 15 mL Centrifuge Tubes Thick.Section 1 Chapter 1 Section 1 Chapter 1 2302-200AW 2 mL Tube with 200 µm Acid Washed Zirconium Beads Self-standing 2 mL microfuge tube with screw-cap. 3116PC 5 mL Polycarbonate Vial Polycarbonate vial with slip-on polyethylene cap. Package of 100. 2302-1400AW 2 mL Tube with 1.7 mm Acid Washed Zirconium Beads. 2198-24-PE Holder for 6133PC Vial Thick. Racks and Holders These Racks and Holders are designed to hold vials securely in place on the Geno/Grinder during processing. Racks 2190 Vial Rack Holds 24 3116PC vials. prefilled with 1. prefilled with 1.5 mL. ¾” x 2”.4 mm Acid Washed Zirconium Beads. prefilled with 800 µm Acid Washed Silica Beads. Acid Washed.5 mm) steel grinding ball (2155). diameter x 2 in. rugged foam block holds 16 standard 50 mL centrifuge tubes.spexsampleprep. Package of 100. 119 mm length. Grinding load per vial 1. Package of 50. Package of 50. Order Online 24/7: www.4 mm Acid Washed Zirconium Beads Self-standing 2 mL microfuge tube with screw-cap. All three vials hold a single 3/8 in. Package of 100. Package of 100. prefilled with 500 μm Garnet and a 6 mm Zirconium Grinding Satellite. or 24 2241-PEF-200 vials. 2304-800AW 2 mL Tube with 800 µm Acid Washed Silica Beads Self-standing 2 mL microfuge tube with screw-cap.0 mm Acid Washed Zirconium Beads Self-standing 2 mL microfuge tube with screw-cap. prefilled with 400 µm Acid Washed Silica Beads.spexsampleprep. Package of 100. For use with 2199 Large Capacity Clamp Assembly. rugged foam block holds 24 standard 15 mL centrifuge tubes. Package of 100. prefilled with 100 μm Silica Beads. 1.7 mm x 50. 26 Order Online 24/7: www. Package of 100.4 mm Acid Washed Zirconium Beads. 2302-3000AW 2 mL Tube with 3 mm Acid Washed Zirconium Beads Self-standing 2 mL microfuge tube with screw-cap.4 mm Zirconium Beads and a 4 mm silica bead. rugged foam block holds 48 microfuge Tubes. They are lightweight and can also be used on the benchtop and to transport samples within the laboratory.5 mm) steel grinding ball (2155) to grind unusually large or tough samples. (9. prefilled with 200 µm Acid Washed Zirconium Beads. rugged foam block holds 24 vials. Holds one 3/8 in. 2303-MM2 2 mL Tube with Mixed Matrix 2 Self-standing 2 mL microfuge tube with screw-cap. 24 2241-PC vials. 2303-MM3 2 mL Tube with Mixed Matrix 3 Self-standing 2 mL microfuge tube with screw-cap. long (12.com 27 . 2304-100AW 2 mL Tube with 100 µm Acid Washed Silica Beads Self-standing 2 mL microfuge tube with screw-cap.com 2305-2800SS 2 mL Tube with 2. 2302-1700AW 2 mL Tube with 1. 2303-MM1 2 mL Tube with Mixed Matrix 1 Self-standing 2 mL microfuge tube with screw-cap.8 mm). prefilled with 1.0 mm Acid Washed Zirconium Beads.7 mm Acid Washed Zirconium Beads Self-standing 2 mL microfuge tube with screw-cap. fits 2190 Vial Rack. Holders 2196-16-PE Holder for 50 mL Centrifuge Tubes Thick. (9. Package of 50. 2304-400AW 2 mL Tube with 400 µm Acid Washed Silica Beads Self-standing 2 mL microfuge tube with screw-cap. 115 mm length. 2300 Holder for 2 mL microfuge Tubes Thick. Package of 100. prefilled with 3 mm Acid Washed Zirconium Beads.8 mm Stainless Steel Grinding Balls. prefilled with 100 µm Acid Washed Silica Beads.

2660. The 2650. Cryo-Blocks are chilled in 2600 Cryo-Station to preserve RNA and proteins during grinding. Sold as a pair.2. The insulated outer jacket of the Cryo-Station is chilled with liquid nitrogen and can be filled automatically or manually. to balance the load in the clamp. Cryo-blocks are chilled in 2600 Cryo-Station to preserve RNA and proteins during grinding.spexsampleprep. Sold as a pair. 2650 Cryo-Adapter keeps samples in titer plate cold during grinding. 2661 and 2664 Cryo-Blocks fit the 2199 Large Capacity Clamp. Two titer plates can be placed in the Cryo-Station well to be filled and kept cold. 2664 Cryo-Block for 50 mL Centrifuge Tubes Aluminum block holds six standard conical-bottom 50 mL centrifuge tubes for cryogenic milling. Use with 2195 Large Capacity Clamp Assembly. 2600 Cryo-Station A holding station for samples which must be kept chilled to preserve RNA for extraction.com Order Online 24/7: www. Cryo-Blocks are chilled in 2600 Cryo-Station to preserve RNA and proteins during grinding. can be found in the Freezer/Mill section. Sold as a pair. 2662. Sold as a pair.Section 1 Chapter 1 Section 1 Chapter 1 Kryo-Tech® These accessories are used to chill samples to cryogenic temperature and to maintain temperature during grinding. 2665 Cryo-Block for Micro-centrifuge or PCR Tubes Aluminum block holds 96 standard (0. as used in 2240-PC Vial Set. Cryo-Blocks are chilled in 2600 Cryo-Station to preserve RNA and proteins during grinding. Cryo-blocks can be quickly chilled in the 2600 CryoStation or directly in liquid nitrogen. Sold as a pair. 2662 Cryo-Block for 4 mL Polycarbonate Vials Aluminum block holds twenty-four 2241-PC vials. as used in 2250 Vial Set. The well can also hold a chilled cutting board to cut up sensitive samples for RNA analysis. set of 2 Aluminum block holds eight 2255 vials. Use with 2195 Large Capacity Clamp Assembly. 2260 Cryo-Block for 2255 Vial.6 mL) micro-centrifuge tubes. as used in 2240-PE Vial Set. CryoBlocks are chilled in 2600 Cryo-Station to preserve RNA and proteins during grinding. When inserted in titer plate and chilled in 2600 CryoStation.5 . Cryo-Blocks are chilled in 2600 Cryo-Station to preserve RNA and proteins during grinding. and will keep samples cold during grinding to preserve RNA and proteins from heat degradation. Sold as a pair. allowing 16 samples to be run simultaneously. Cryo-Blocks are chilled in 2600 CryoStation to preserve RNA and proteins during grinding. 2666 Cryo-Block for 48 Micro-centrifuge or PCR Tubes Aluminum block holds 48 standard (1. Cryo-Blocks Cryo-Blocks are made of aluminum. and fit the standard clamp. 2661 Cryo-Block for 15 mL Centrifuge Tubes Aluminum block holds fifteen 15 mL conical bottom centrifuge tubes. For use with 2199 Large Capacity Clamp Assembly. 2660 Cryo-Block for 15 mL Polycarbonate Vials Aluminum block holds six 2251PC vials.spexsampleprep. Cryo-Blocks are sold in pairs because they are used two at a time. 2650 Cryo-Adapter for Titer Plates Extruded aluminum insert for 2210 Titer Plate. Sold in pairs. and 2665 Cryo-Blocks have about the same footprint and height as deep-well titer plates.com 29 . 2663 Cryo-Block for 4 mL Polyethylene Vials Aluminum block holds twenty-four 2241-PE vials. 28 Order Online 24/7: www. Set includes two Cryo-Blocks. Additional products for liquid nitrogen handling. such as protective gloves and portable Dewars. They hold and chill titer plates and vials for grinding plant and animal tissue for nucleic acid and protein extractions.0 mL) microcentrifuge tubes. Sold as a pair. The 2260. preserving RNA and proteins.

• Coil holds one Large Vial. • Safety features include LN sensor and lid interlock. one Mid-Size Vial. or up to four Standard Small Vials.Section 1 Chapter 2 Section 1 Chapter 2 SPEX SamplePrep 6970EFM Enclosed Freezer/Mill® 6970M-115 Freezer/Mill – Single Grinding Coil for 115V/60Hz operation 6970M-230 Freezer/Mill – Single Grinding Coil for 230V/50Hz operation. (31. • Liquid nitrogen required for operation. CE Approved • Large cryogenic impact grinder with self-contained liquid nitrogen tub and insulated case. CE Approved • Totally enclosed cryogenic impact grinder with Auto-Fill System.spexsampleprep. • Touch-screen controls for programming grinding cycles. CE Approved 6970D-115 Freezer/Mill – Dual Grinding Coils for 115V/60Hz operation 6970D-230 Freezer/Mill – Dual Grinding Coils for 230V/50Hz operation.7 kg) net (6970D) 115V/60Hz or 230V/50Hz 3-prong standard North American plug for 115V/60Hz version 2-prong European CEE 7/7 plug for 230V/50Hz version 30 Order Online 24/7: www. Specifications: Dimensions: Weight: Voltage: Power Cord: 20 ½ in.com Order Online 24/7: www. and pre-cooling and cooling times • Grinding chambers in 6970D can be programmed and operated independently or simultaneously • Stores 10 grinding programs • Safety features include LN sensor and door interlock • Liquid nitrogen required for operation • 6970D and 6970M supplied with choice of 6870L Accessory Package for Large Vials or 6870S Accessory Package for Small Vials SPEX SamplePrep 6870 Freezer/Mill® 6870-115 Freezer/Mill – For 115V/60Hz operation 6870-230 Freezer/Mill – For 230V/50Hz operation. (55 cm) x 18 in.com 31 . one Mid-Size Vial. Eliminates liquid nitrogen (LN) exposure • Available with single (6970M) or dual (6970D) grinding chambers for increased sample throughput • Grind up to 8 samples using the standard Freezer/Mill Grinding Vials. (46 cm) x 17 in. (52 cm) x 21 ½ in.1 to 100 gram range • Each Coil holds one Large Vial. pre-cooling and cooling times. • Stores 10 grinding programs. (56 cm) x 18¼ in. (19 kg) net. impact rate. • Grinds samples in the 0. • 6870 Freezer/Mill supplied with choice of 6870L Accessory Package for Large Vials or 6870S Accessory Package for Small Vials. impact rate. • Accessory package for Mid-Sized Vials sold separately. 48 lbs. • Grinds samples in the 0. times. or up to four standard Small Vials • Color touch screen controls for programming grinding cycles and time. • 6820 Auto-Fill System available for automated filling with liquid nitrogen. (46 cm) 42 lbs. (43 cm) 70 lbs. (22 kg) gross 115V/60Hz or 230V/50Hz 3-prong standard North American plug for 115V/60Hz version 2-prong European CEE 7/7 plug for 230V/50Hz version Specifications: Dimensions: Weight: Voltage: Power Cord: 22 in.spexsampleprep.1 to 100 gram range.

5 mL (0. Polycarbonate is durable but should be cleaned with hot water and detergent.5. 6751C4 Small Polycarbonate Center Cylinder For 6751 vial set. Sample capacity 0. and four polycarbonate center cylinders (6751C4). The solid.5 . 25 lbs.1 .0. Made of nonmagnetic stainless steel. Sample capacity 0.1 .0 mL (0.5. 6751 Small Grinding Vial Set Set includes stainless steel impactor. 6752 Small Steel Center Cylinder For 6751 vial set. 32 Order Online 24/7: www. 6761 Small Poly-Vial Set For grinding soft tissues without metal contamination.Section 1 Chapter 2 Section 1 Chapter 2 SPEX SamplePrep 6770 Freezer/Mill® 6770-115 Freezer/Mill – For 115V/60Hz operation 6770-230 Freezer/Mill – For 230V/50Hz operation. Set includes one complete vial plus three spare center cylinders.com Order Online 24/7: www. not organic solvents. Each 6753V has stainless steel end plugs. (27 cm) x 13½in. impactor is polycarbonateencapsulated steel. (35 cm) 19 lbs.4. End plugs and center cylinder are polycarbonate. CE Approved • Cryogenic impact grinder with self-contained liquid nitrogen tub and insulated case. • Touch-screen controls for programming grinding cycles and time.1 . The center cylinder forms the grinding chamber.0 gram range. • Stores 10 grinding programs. 6751C20 Small Polycarbonate Center Cylinder Same as above.5 g) each.spexsampleprep.0 g).1 gram to 5. while the end plugs are removable for extraction of sample and cleaning.3 kg) gross 115V/60Hz or 230V/50Hz 3-prong standard North American plug for 115V/60Hz version 2-prong European CEE 7/7 plug for 230V/50Hz version 6753 Microvial Set Three 6753V Microvials with holder. impact rate. • Liquid nitrogen required for operation. • 6770 Freezer/Mill supplied with 6754 Extractor/Vial Opener and 6755 Small Vial Rack. • Grinds samples in the 0.5 . Replaces 6751C when sample contact with plastic is not advised.4. (11.0 mL (0. with grinding occurring as the sample is struck by the impactor against the end plug. Set includes one complete vial plus three spare center cylinders. but a package of 20. and an impactor.1 . Specifications: Dimensions: Weight: Voltage: Power Cord: 17 in. Sample capacity is approximate.com 33 . Transparent plastic allows visual check of grinding progress. • Coil holds one standard Small Grinding Vial or one 6753 Microvial Set • Pre-cooling chamber holds up to three additional vials. two end plugs. (43 cm) x 10½ in. Holder contains three 6753V Microvials for simultaneous operation. Sample capacity 0. It can be sterilized with a dilute bleach solution.0. • Safety features include LN sensor and lid interlock.spexsampleprep. Actual sample capacity range for a vial depends on the nature of the material.6 kg) net. Accessories Vials & Vial Sets Vials for the Freezer/Mill product line consist of a center cylinder. two end plugs. (8.0 g). cylindrical impactor is magnetically shuttled from end to end in the vial. center cylinder and impactor. pre-cooling and cooling times. sold in package of 4.

Will not add Cr to sample like stainless steel components of 6751 Vial. 6761.com 6881C20 Mid-Size Polycarbonate Center Cylinder Same as 6881C4. 6802 Large Steel Center Cylinder For 6801 Vial Set. 34 Order Online 24/7: www. Must be used with 6884 and 6886 Adapters. Cr-free ASTM 06 steel impactor and end plugs. plus four polycarbonate center cylinders (6801C4). Increases throughput. 6805 Vial Rack for Large Vials Epoxy-coated steel rack holds six 6801 or 6871 Vial Sets for storage and handling. It can be sterilized with a dilute bleach solution. polycarbonate center cylinder (6881C). The 6753C is inserted into an individual vial. 6871 Large Cr-Free Vial Set For grinding electronic components to test for chromium under RoHS/WEEE directives. 6801C4 Large Polycarbonate Center Cylinder For 6801 and 6871 Vial Sets. Used in place of 6801C when polycarbonate cylinder is not compatible with sample. then pushed through to clear sample from the tube. Sold in units of 4.com 35 . End plugs and center cylinder are polycarbonate. Polycarbonate is durable but should be cleaned with detergent and water.100 g). polycarbonate center cylinder (6881C). Made of nonmagnetic stainless steel. but a package of 20. 6753. Sample capacity up to 50 mL (1 . not organic solvents. but a package of 20. 6753.Section 1 Chapter 2 Section 1 Chapter 2 6771 Small Cr-Free Vial Set For RoHS/WEEE testing of electronic components for chromium. 6885 Mid-Size Poly-Vial For grinding soft tissues without metal contamination. Sample capacity up to 25 mL (1 . 6881 Mid-Size Vial Set Grinding vial intermediate in size between 6751 and 6801: sample capacity up to 25 mL (1 .spexsampleprep.4. Set includes one complete vial plus three extra cylinders. The 6814 AutoExtractor is an electrically powered version of our 6754 and 6804 Extractor/Vial Openers. The 6814 will open large Vial Sets (6801. Order Online 24/7: www. and 6771 Vial Sets. and pack of 100 O-rings. impactor is polycarbonate-encapsulated steel. 6814-230 AutoExtractor™ – For 230 V/50 Hz operation.5 g).40 g). 6883 Mid-Size Cr-Free Vial For grinding electronic components to test for chromium under RoHS/WEEE directives. Vial Racks 6755 Vial Rack for Small Vials For 6751. 6801 Large Grinding Vial Set Set includes stainless steel impactor and two end plugs.spexsampleprep. Sample capacity up to 25 mL (1 . Cr-free ASTM 06 steel impactor and end plugs. 6801C20 Large Polycarbonate Center Cylinder Same as 6801C4. Must be used with 6884 and 6886 Adapters. 6883.0 mL (0.1 . Sold in units of 4. Set includes one complete vial plus three extra cylinders. Polycarbonate is durable but should be cleaned with detergent and water. Cold vials can now be opened easily. 6871). Glass-reinforced acetal rack holds up to sixteen vials for storage and handling. O-rings are used on end plugs to prevent sample leakage during grinding. 6881C4 Mid-Size Polycarbonate Center Cylinder For 6881. two end plugs. not organic solvents. One 6805 is supplied with each 6870L Accessory Package. polycarbonate center cylinder (6801C).100 g). Must be used with 6884 and 6886 Adapters.5 . Will not add Cr like stainless steel components of 6801 vial. Transparent plastic allows visual check of grinding progress. Sample capacity up to 50 mL (1 . reduces operator effort.40 g).40 g). stainless steel center cylinder. 6753C Microvial Sample Extraction Tool For removing ground samples from Microvials. 6761. and 6885 Vial Sets. Vial set includes one complete vial and three spare cylinders. Set includes three extra 6751C cylinders. Shown with 6753V Microvial. and includes a special adapter for small Vial Sets (6751. Extractors 6814 AutoExtractor™ for Freezer/Mill® Vial Sets 6814-115 AutoExtractor™ – For 115 V/60 Hz operation. Stainless steel end plugs and impactor. End plugs and impactor are Cr-free ASTM 06 steel. One 6755 Vial Rack is supplied with each 6770 Freezer/Mill and 6870S Accessory Package.0. Not adaptable for Mid-Size Vial Sets. 6771). Vial set includes one complete vial plus three extra center cylinders. Set includes complete vial plus three spare center sections. 6781S Small Stainless Steel Grinding Vial Set Set includes stainless steel impactor. Sample capacity 0. Made of non-magnetic stainless steel. For use when contact with plastic is not recommended.

6870. is easily installed.com 37 . Add 6884 Adapter for use with Mid-Size Vials. or 6771 Vials in the 6870 or 6970EFM Freezer/Mills.spexsampleprep. and 6886 Mid-Size Vial Adapter for large Freezer/Mills. The Multi-Vial Adapter is an insert placed inside the coil to separate and align small vials during grinding. 6755 Vial Rack. Lever assists end-plug extraction. One 6804 is supplied with each 6870L Accessory Package. One 6754 is supplied with each 6770 Freezer/Mill and as part of the 6870S Accessory Package. Mid-size vials require the 6870M Mid-Size Vial Accessory Package.spexsampleprep. and 6771 Vial Sets. one 6755 Small Vial Rack. The 6870 Freezer/Mill can hold up to four small vials* (6751. and 6806 Multi-Vial Adapter. and one 6886 Mid-Size Vial Adapter for 6800-Series or 6970EFM Freezer/Mills. and one 6806 Multi-Vial Adapter. Insert attaches to bell of 6804. and 6885 Mid-Size Vial Sets. 6886 Mid-Size Vial Adapter for 6800-Series Freezer/Mills Positions and aligns Mid-Size vials in 6800. 6870M Mid-Size Vial Accessory Package For 6881. 6761. Small vials require the 6870S Small Vial Accessory Package. *Note: the 6753 Microvial Set can only be run one at a time in the 6870 Freezer/Mill. 6885). and is used to remove the vial end plugs from the center section. Includes 6884 Mid-Size Vial Adapter for 6804 Extractor/Vial Opener. One 6806 is supplied with each 6870S Accessory Package. and 6970EFM Freezer/Mills. 6753. 6761. 6804 Extractor/Vial Opener for Large and Mid-Sized Vials The Extractor/Vial Opener lifts vial sets in and out of the Freezer/Mill. and is used to remove the vial end plugs from the center section. 6850.com Order Online 24/7: www. Includes 6804 Extractor/Vial Opener and 6805 Vial Rack. consisting of one 6754 Extractor/Vial Opener. 36 Order Online 24/7: www.Section 1 Chapter 2 Section 1 Chapter 2 6754 Extractor/Vial Opener for Small Vials The Extractor/Vial Opener lifts 6700-series vials in and out of the Freezer/Mill. 6870L Large Vial Accessory Package For 6801 and 6871 Vial Sets. 6883. 6771) or one mid-size vial (6881. 6870S Small Vial Accessory Package For 6751. removed. The Accessory Package for mid-size vials must be purchased separately. 6883. Includes 6754 Extractor/Vial Opener. 6884 Mid-Size Vial Adapter for 6804 Extractor/Vial Opener Adapts 6804 Extractor/Vial Opener for use with Mid-Size Vials. Accessory Packages & Kits Each 6970EFM or 6870 Freezer/Mill is supplied with your choice of 6870L Large Vial Accessory Package or 6870S Small Vial Accessory Package. 6761. consisting of one 6884 Mid-Size Vial Adapter for 6804 Extractor/Vial Opener. Sample Adapters 6806 Multi-Vial Adapter Required when using one to four 6751.

50 L Capacity Cryogenic cylinder designed for storing and dispensing liquid nitrogen with pressure of up to 22 psi. Sturdy. Sturdy.spexsampleprep. We also offer transfer hoses as well as 25 L and 50 L Dewars for dispensing LN. Perfect for use with the 6970EFM or 6870 with autofill. The 6820 Auto-Fill System should be ordered at the same time as the 6870 Freezer/Mill so it can be installed and calibrated at our factory. These multi-layer-insulated gloves are lightweight and flexible.5 mm) NPT male fitting on one end and a CGA295 female fitting on the other end. which are sold separately. Compatible with 6806 and 6807 Cryogenic Transfer Hoses. Fitted with a 3/8 in. The boiling point of liquid nitrogen is -195. (1. such as the SPEX SamplePrep 6906 or 6907 Cryogenic Transfer Hoses. large (6900L) and X-large (6900XL).8 m) long flexible stainless steel hose suitable for transferring cryogenic fluids such as liquid nitrogen.spexsampleprep.7 mm) JIC female flare nut. 6906 Short Cryogenic Transfer Hose 4 ft. The transfer hose must be configured with a 1/2 inch (12.Section 1 Chapter 2 Section 1 Chapter 2 Liquid Nitrogen Handling Our products are designed to aid the user in the safe handling of liquid nitrogen. Fitted with a 3/8 in. The Auto-Fill System is a more efficient and safer way to handle the volume of liquid nitrogen required for processing samples in the 6870 Freezer/Mill. 38 Order Online 24/7: www. allow excellent dexterity. and vents nitrogen gas pressure that may build up in the hose when there is liquid nitrogen in the hose and the valves at both ends are closed. (1. five-wheel roller base makes moving Dewar from room to room safe and easy. Compatible with 6905 and 6910 Portable Cryogenic Dewar. 6820 Auto-Fill System for the 6870 Freezer/Mill The 6820 Auto-Fill System is designed to automatically maintain the required level of liquid nitrogen within the 6870 Freezer/Mill during operation. This automated system reduces the loss of liquid nitrogen and saves the time lost when manually filling the reservoir. Compatible with 6905 and 6910 Portable Cryogenic Dewar.com Order Online 24/7: www. Includes liquid withdrawal device for dispensing liquid nitrogen directly into the Freezer/Mill at rates up to 8 liters per minute. (9.80º C. stainless steel.7 mm) JIC female flare nut at each end for proper installation.com 39 . Transfer hoses are available in different lengths and can be constructed with different materials. 6970EFM and 6820 Auto-Fill system. and are comfortable to wear for extended periods of time. (9. 6905 Portable Cryogenic Dewar. 6970EFM and 6820 Auto-Fill system. The safety relief valve attaches at the high point of the transfer hose. Highly recommended for safe operation of SPEX SamplePrep Freezer/Mills. The Auto-Fill System requires a cryogenic transfer hose. Capacity 25 liters. 25 L Capacity Cryogenic Dewar designed for storing and dispensing small amounts of liquid nitrogen. The Auto-Fill System is also supplied with a safety relief valve that connects to the liquid nitrogen supply via a 1/2 inch (12. Our 6820 Auto-Fill System is an option for filling the 6870 Freezer/Mill without direct LN contact. safe and easy. Compatible with 6906 and 6907 transfer hoses. aluminum. The 6820 package does include an adapter to allow compatibility with the 6906 and 6907 Cryogenic Transfer Hoses. four-wheel design makes moving the cylinder from room to room. 6900 Cryogenic Gloves Designed to protect the hands and arms from the hazards associated with ultra-cold materials. 6910 Portable Pressurized Cryogenic Cylinder. When working with liquid nitrogen directly or indirectly. The gloves are sold as a pair and are available in small (6900S). medium (6900M).2 m) long flexible stainless steel hose suitable for transferring cryogenic fluids such as liquid nitrogen. Capacity 50 liters. 6907 Long Cryogenic Transfer Hose 6 ft.5 mm) NPT male fitting on one end and a CGA295 female fitting on the other end. cryogenic gloves must be worn to protect hands.

(37 kg) 98 lb. brittle samples • Also called a shaker mill or high-energy ball mill • Sample sizes in the 10 gram range for grinding. (61 cm) x 17 in. 1725 RPM @ 60 Hz or 1425 RPM @ 50 Hz Start and stop buttons.8 mm) vials SPEX SamplePrep 8000M Mixer/Mill® 8000M-115 Mixer/Mill . 1 in. clamps are run in balance with the same vial and load in each clamp • Accepts grinding/mixing vials from 2 3/8 in. CE Approved • Efficient two-clamp laboratory mill for pulverizing hard. x 2 in. (5. (44 kg) 115 V/60 Hz or 230 V/50 Hz 1⁄3 HP.9 cm) in length and up to 2 ¼ in. and up to 60 mL for blending powders or mixing emulsions • Reduces samples to analytical fineness • Can be utilized for mechanical alloying and nanomilling • Features include a variable-range electronic timer.For 115 V/60 Hz operation 8000D-230 Mixer/Mill .9 cm) back-and-forth. (5.com 41 .(19.9 cm) in length and up to 2 ¼ in.8 mm).1 mm x 50. dual clamps for multiple sample capacity.spexsampleprep.4 mm). 1/2 in.9 cm) back-and-forth. (2.spexsampleprep. and forced-air cooling • Timer is factory-set for 100-minute range. and 3/4 in.8 mm). (5. (46 cm) 76 lbs. 1/2 in. (12. 3-prong grounded plug for 115 V/60 Hz version 2-prong European plug for 230 V/50 Hz version Clamp Movement: 2 1⁄3 in. x 2 in. (43 cm) x 11 in.7 mm x 50.Section 1 Chapter 3 Section 1 Chapter 3 SPEX SamplePrep 8000D Dual Mixer/Mill® 8000D-115 Mixer/Mill . and up to 60 mL for blending powders or mixing emulsions • Reduces samples to analytical fineness • Can be utilized for mechanical alloying and nanomilling • Features include a variable-range electronic timer. safety interlock system.000 or 10. 1 in. and shock-mounted electric motor for tabletop operation • Timer is factory-set for 100-minute range.5 cm) side-to-side Clamp speed in complete back-and-forth cycles per minute: 1060 (115 V/60 Hz) or 875 (230 V/50 Hz) Clamp Movement: 2 1⁄3 in. (48 cm) x 14 in.7 cm) in diameter • The 8010 and 8011 adapters permit processing of multiple samples in 1/2 in. net (35 kg).8 mm) vials Specifications: Dimensions: Weight: Voltage: Motor: Controls: Power Cord: 19 in. (12. (28 cm) 82 lb. gross (41 kg) 115 V/60 Hz or 230 V/50 Hz 1⁄3 HP.000 minutes • Accepts grinding/mixing vials from 1 ¾ in. x 2 in. ( 2. CE Approved • Also called a shaker mill or high-energy ball mill • Sample sizes in the 10-gram range for grinding.1 mm x 50.For 230 V/50 Hz operation. 3-prong standard North American plug for 115 V/60 Hz version 2-prong European CEE 7/7 plug for 230 V/50 Hz version Specifications: Dimensions: Net Weight: Gross Weight: Voltage: Motor: Controls: Power Cord: 24 in.4 mm). x 1 in. programmable 100-minute timer with digital display.For 230 V/50 Hz operation. and 3/4 in.000 minutes • For efficiency. 1725 RPM @ 60 Hz or 1425 RPM @ 50 Hz Start and stop buttons. Optional chip is available to extend timer range to 1.7 mm x 25.7 mm x 25. x 1 in. Optional chip is available to extend timer range to 1.7 cm) in diameter • The 8010 and 8011 adapters permit processing of multiple samples in 1/2 in. (12. (12. (5.000 or 10.For 115 V/60 Hz operation 8000M-230 Mixer/Mill . (4. (6 cm) to 3 1/8 in. (7. safety interlock system. (36 cm) x 18 in.5 cm) to 3 1/8 in. programmable 100-minute timer with digital display. (7.7 mm x 50. 92 lbs. x 2 in.com Order Online 24/7: www. (19.5 cm) side-to-side Clamp speed in complete back-and-forth cycles per minute: 1060 (115 V/60 Hz) or 875 (230 V/50 Hz) 40 Order Online 24/7: www.

5 mL. (50. They are available in a wide variety of sizes and materials for maximum on-the-job flexibility over a wide range of applications.5 mL. (6. mixing load approximately 5 mL.7 mm) diameter x 1 in.4 mm) long. Volume 2. resettable 72-minute timer on the 5100-230 Mixer/Mill Mixer Mill Accessories Vials & Vial Sets Mixer/Mill vials are available individually or as part of a set which includes end caps and grinding media. (25. (19. (20 cm) 15. Volume 2. 3⁄8 in. Includes slip-on polyethylene cap. (12.7 mm) diameter x 1 in.5 gram to 1. (57. (12.7 mm) diameter x 2 in. 6133 Polystyrene Vial 3/4 in. 3119. (9.8 mm) long. mixing load approximately 1 mL. Accepts SPEX SamplePrep 3112. 3116 Polystyrene Vial 1/2 in. includes slip-on cap and 1/4 in. and 8006A methacrylate balls.7 mm) front-to-back. (12.5 mm) side-to-side Clamp speed in complete back-and-forth cycles per minute: 3000 (115 V/60 Hz or 2500 (230 V/50 Hz) 42 Order Online 24/7: www.6 mL.2 lbs.2–0.8 lbs. (12. mixing load approximately 2 mL. Specifications: Dimensions: Weight: Voltage: Motor: Controls: Power Cord: 12 in. Sold in units of 100. 3114 Stainless Steel Vial Set 1/2 in. 3119. Sold in units of 100.35 mm) stainless steel ball. 19. Made of 303 stainless steel. Volume 12 mL. (12. mixing load 1 mL. Includes slip-on polyethylene cap. Sold in units of 100. (33 cm) x 8 in. Sold in units of 100. or 8006A methacrylate balls. (50.com Order Online 24/7: www. resettable 72-minute timer on 230 V/50 Hz version 3-prong standard North American plug for 115 V/60 Hz version 2-prong European CEE 7/7 plug for 230 V/50 Hz version Clamp Movement: 1⁄2 in. Accepts SPEX SamplePrep 3112. 3000 RPM @ 60 Hz or 2500 RPM @ 50 Hz Push-button. Sold in units of 100.spexsampleprep. resettable 30-minute timer on the 5100-115 Mixer/Mill • Push-button.7 mm) diameter or two vials of 3/4 in. 6133PC Polycarbonate Vial 3/4 in.5 gram range • Holds three vials of 1/2 in. Accepts SPEX SamplePrep 3112 or 3119 methacrylate balls. (19. (20 cm) x 8 in. Accepts SPEX SamplePrep 3112 or 3119 methacrylate balls. Accepts SPEX SamplePrep 3112 or 3119 methacrylate balls. (12. resettable 30-minute timer on 115 V/60 Hz version Push-button. gross (9 kg) 115 V/60 Hz or 230 V/50 Hz 1/15 HP. Volume 5 mL.4 mm) long.1 mm) diameter (length of vials up to 21/4 in. • For grinding up to 3 mL or blending up to 10 mL of sample • Push-button.8 mm) long. (19. (25. Includes slip-on polyethylene cap. grinding load 0.8 mm) long. Small Vials and Vial Sets For use in all Mixer Mills (8000 Series requires adapter) 3111 Polystyrene Vial 1/2 in. mixing load approximately 2 mL.com 43 . (50. mixing load approximately 5 mL.Section 1 Chapter 3 Section 1 Chapter 3 SPEX SamplePrep 5100 Mixer/Mill® 5100-115 Mixer/Mill – For 115 V/60 Hz operation 5100-230 Mixer/Mill – For 230 V/50 Hz operation • High-energy “shaker mill” • Pulverizes and/or homogenizes samples of varying composition • Grinding containers constructed with a variety of materials • Typically grinds samples in the 0.1 mm) diameter x 2 in. Volume 12 mL. Volume 5 mL.7 mm) diameter x 2 in.spexsampleprep.1 mm) diameter x 2 in.2 mm). Includes slip-on polyethylene cap. net (7 kg).8 mm) long. (50. Includes slip-on polyethylene cap. 3116PC Polycarbonate Vial 1/2 in.

(7. two 1/2 in. 8003 Alumina Ceramic Vial Set For wet (use 8015 Clamp) or dry grinding/mixing. (15. Vial size 2 1/2 in. (5. (6.6 mL.2–0.5 mm) methacrylate balls. Vial body and cap liner made of hardened tool steel. lined with tungsten carbide. Large Vials and Vial Sets For use in 8000 Series Mixer/Mills 8001 Hardened Steel Vial Set For wet or dry grinding/mixing. mixing load approximately 50 mL. Volume 2.9 mm) tungsten carbide balls. Volume 1. (6. (19. includes stopper and 1/4 in. (6. (12. Volume 55 mL. (5. (33 mm) long. (9. Volume 55 mL. Heavy-gauge methacrylate body with methacrylate-lined aluminum screw-on cap. (12. Rugged construction allows grinding of soft materials without metallic contamination. Set includes solid zirconia ceramic vial and slip-on cap. mixing load approximately 25 mL. Includes center cylinder with two slip-on caps and 1/4 in. 8015 Clamp for 8003 Vial Set Clamps permit slurry grinding in SPEX SamplePrep 8003 Vial Set.spexsampleprep.spexsampleprep. and eight corprene gaskets. grinding load 2–8 mL. 3127 Hardened Tool Steel Vial Set 3/4 in. (6. Vial size 2 1/4 in.com 45 .5 mL. Set includes tungsten carbide-lined body. Volume 55 mL. grinding load 0. Volume 45 mL.35 cm) diameter x 2 11/16 in.com Order Online 24/7: www.7 cm) diameter x 2 1/2 in.7 mm) alumina ceramic ball.9 mm) diameter x 1 1/3 in.1 mm) diameter x 1 7/8 in. mixing load 3 mL. (11. (12. (11. (6. For use with SPEX SamplePrep 3112 or 8006A methacrylate balls.2 mm) tungsten carbide balls and six extra Viton gaskets. (5.7 cm) diameter x 2 3/4 in. Includes two slip-on Delrin® caps with tungsten carbide inserts. Made of hardened tool steel. Gaskets are Viton for enhanced resistance to heat and chemicals. Vial size 2 1/4 in. two 8006A 1/2 in. Vial size 2 1/4 in. grinding load 0. mixing load approximately 25 mL. grinding load 3–10 mL.35 mm) steel ball. mixing load approximately 25 mL. Volume 65 mL. Vial size 2 1/4 in.0 mL.2 – 0.35 cm) long. (6. (12. Set includes corprene gasket. two screw-on tungsten carbide-lined caps.2 mm) tungsten carbide balls. 8002 Polystyrene Vial For wet or dry mixing of liquids and powders.4 mm) long. grinding load 3–10 mL. One pair required for each 8003. 3118 Agate Vial Set 5/8 in. Made of hardened tool steel. (6. Sold in units of 20.1 mm) diameter x 2 1/8 in. (5. 5004 Tungsten Carbide-Lined Vial Set 3/4 in. (12.7 mm) diameter x 1 in. must be run inside cushioned SPEX SamplePrep 6133 vial (included). (6. grinding load 0. (7.4 cm) diameter x 2 1/2 in. grinding load 3-10 mL. The screw-on caps and body are 304 stainless steel.7 cm) diameter x 2 5/8 in. for SPEX SamplePrep 5004 Vial Set. Polystyrene body with plastic screw-on cap. Volume 5 mL. mixing load 1 mL. and seven corprene gaskets. sold in pairs. mixing load approximately 20 mL.5% alumina ceramic vial body and two slip-on caps. mixing load approximately 20 mL.7 cm) diameter x 3 in. 8005 Zirconia Ceramic Vial Set For wet or dry grinding/mixing. (25. (6. mixing load 1 mL.35 mm) steel ball. Set includes screw-on cap with O-ring.5–1.6 mm) long. (5. (7.8 cm) long. two 7/16 in.5 mL.7 cm) diameter x 2 1/2 in. mixing load approximately 25 mL. Handmade from flawless Brazilian agate. and eight corprene gaskets.6 mL. (54 mm) long. mixing load 2 mL.35 mm) steel balls. one 1/2 in. two 1/2 in.7 cm) long.7 mm) zirconia ceramic balls.35 cm) long. Sold in units of 100. Volume 135 mL. (19.35 mm) agate ball.7 cm) long. (47.0 cm) long. Set includes two 7/16 in.62 cm) long. six disposable methacrylate center cylinders.7 mm) and four 3112 3/8 in. (6. Volume 5 mL.Section 1 Chapter 3 Section 1 Chapter 3 3117 Hardened Tool Steel Vial Set 1/2 in.6 mL. 44 Order Online 24/7: www. 8004SS Steel-Jacketed Tungsten Carbide Vial Set For wet or dry grinding/mixing in extreme environments. Vial size 2 1/8 in.5–1. 8004 Tungsten Carbide Vial Set For wet or dry grinding/mixing.7 mm) and four 1/4 in. Vial size 2 1/4 in. 8006 Methacrylate Vial Set For wet or dry mixing of liquids and powders. and two 5/16 in. Includes slip-on cap and 1/4 in. 5004C Methacrylate Center Cylinder Disposable methacrylate center cylinder. Set includes high purity 99. grinding load 0. (5. grinding load 2–8 mL. Volume 45 mL.

(12. (7.6 mL 0. Includes screw-on cap. Vial size 1 1/2 in.5 g 1 g 10 g 10 g Blending Sample Volume 1 mL 2 mL 25 mL 25 mL 1 mL 25 mL 2.com Order Online 24/7: www. mixing load approximately 20 mL. 6135 Polyethylene Vial For wet or dry mixing.62 cm) long.5 mL 3-10 mL 3-10 mL 2-8 mL 0. O-ring. For use with SPEX SamplePrep 3112 or 8006A methacrylate balls. mixing load approximately 40 mL. Hardened steel vial body has grinding chamber with rounded ends for more efficient grinding/mixing. (6. For use with SPEX SamplePrep 3112 or 8006A methacrylate balls.2-0. (5. (7.7 mm) and four 1/4 in.spexsampleprep.5-1.62 cm) long. Volume 45 mL. grinding load 2–8 mL. (6.62 cm) long. grinding load 3–10 mL. (12. Set includes all-agate vial body.5 mL 25 mL 25 mL 20 mL Suitable for Slurry Grinding or Blending No No Yes Yes No Yes Yes Yes Yes Yes No No Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes 47 Hardened Steel Stainless Steel 0. Sold in units of 100. (6. (6.35 mm) stainless steel balls. (7. Volume 35 mL. and eight corprene gaskets. (12.35 mm) steel balls. Vial size 2 1/4 in.5 g 10 g Tungsten Carbide 1 g 10 g 10 g Alumina Ceramic 10 g Agate 0. mixing load approximately 25 mL. 6134 Polystyrene Vial For wet or dry mixing. Polyethylene vial with attached cap.7 mm) agate balls.5-1.7 cm) diameter x 3 in. 8014 Agate Vial Set For dry grinding/mixing. 8009 Round-Ended Hardened Steel Vial Set For wet or dry grinding/mixing. two 1/2 in. Vial size 1 in. (12. (6. (5. 8008 Silicon Nitride Vial Set For wet or dry grinding/mixing. Set includes screw-on cap with O-ring. Vial size 2 3/8 in. Set includes solid silicon nitride vial and slip-on cap. mixing load approximately 20 mL. Includes polyethylene slip-on cap.54 cm) diameter x 3 in.0 mL 3-10 mL 3-10 mL 0. Volume 75 mL.6 mL 5-10 mL 2-8 mL 2-8 mL - - - - - - - 20-50 mL 3 – 10 mL Typical Grinding Sample Weight 0. two 1/2 in. (7. Volume 45 mL. grinding load 3–10 mL.8 cm) long. two 1/2 in. Vial size 2 1/4 in. grinding load 3–8 mL. two 1/2 in.com .Section 1 Chapter 3 Section 1 Chapter 3 8007 Stainless Steel Vial Set For wet or dry grinding/mixing. Volume 65 mL. Vial body and cap liner made of hardened 440C stainless steel. two slip-on caps. Volume 35 mL. and seven corprene gaskets.7 cm) diameter x 2 3/4 in. (3.spexsampleprep.6 mL 3-10 mL 0.5 g 10 g 1 mL 25 mL 20 mL 20 mL Zirconia Ceramic 10 g Silicon Nitride 10 g Plastic - - - - - - - - - 1 mL 2 mL 2 mL 5 mL 5 mL 15 mL 40 mL 50 mL 20 mL 46 Order Online 24/7: www. Sold in units of 100 Comparison of Grinding Vials P/N 3117 3127 8001 8009 3114 8007 5004 8004 8004SS 8003 3118 8014 8005 8008 3111 3116 3116PC 6133 6133PC 6134 6135 8002 8006 Grinding Sample Volume 0.2-0.7 mm) silicon nitride balls.2-0.0 cm) long. (7.81 cm) diameter x 3 in. Vial size 2 1/2 in.62 cm) long.35 cm) diameter x 2 11/16 in.7 mm) and four 1/4 in. mixing load approximately 25 mL. (2.0 cm) diameter x 3 in. mixing load approximately 15 mL.

(7. for simultaneous running in 8000M Mixer/Mill. for SPEX SamplePrep 3118 Vial Set.35 mm) hardened steel balls for SPEX SamplePrep 8001 and 8009 Vial Sets. One-quart bottle. evaporates after grinding.com 49 .2 mm) diameter. 8008A Silicon Nitride Ball 1/2 in. Suitable vials include SPEX SamplePrep 3118.spexsampleprep. Four balls per set. 8003A Alumina Ceramic Ball 1/2 in. 48 Order Online 24/7: www. fit all SPEX SamplePrep plastic vials. Four balls per set. 8012 adapter is also necessary. 5004.7 mm) in diameter.1 mm) in diameter. (9. and 6133 vials. 3117B Hardened Tool Steel Ball Set 1/4 in.35 mm) hardened 440C stainless steel balls for SPEX SamplePrep 8007 Vial Set.7 mm) and four 1/4 in.1 mm) diameter vials. for SPEX SamplePrep 3117 and 3127 Vial Sets.4 mm) in length (3111. fit all SPEX SamplePrep plastic vials ¾ in. (12.35 mm) diameter stainless steel (440C) ball. (11. (12.9 mm) diameter tungsten carbide ball.7 mm) diameter agate ball for SPEX SamplePrep 8014 Vial Set. 8010 Multiple-Sample Adapter Holds seven vials. Sample Adapters For 8000 Series Mixer/Mills Special adapters enable simultaneous running of multiple samples in the 8000 Series Mixer/Mills. 3127. each 1/2 in. (12. 3114. 8006A Methacrylate Balls Methacrylate balls 1/2 in. Instructions included. (6. 3114. 8005A Zirconia Ceramic Ball 1⁄2 in. fit all SPEX SamplePrep plastic vials. Can be used in 8000D Mixer/ Mill with 3118. for SPEX SamplePrep 3114 Vial Set. respectively. 25 grams (approximately 24 mL) in dropper bottle. (6.7 mm) diameter. 3116 and 3117. 5004 and 6133. (6. Four balls per set.2 mm) diameter tungsten carbide ball for SPEX SamplePrep 8004 and 8004SS Vial Sets. (6.spexsampleprep. or with 3111. Vials run at one time should be same length. 8001B Steel Ball Set Two 1/2 in. (19. SPEX SamplePrep PrepAid® Grinding Aids 3640 PrepAid Propylene Glycol – (C3H8O2) Liquid grinding aid. Suitable vials include SPEX SamplePrep 3111. Can be used in 8000D Mixer/ Mill with 3116 vials. 8011 Multiple-Sample Adapter Holds four vials.1 mm) diameter and larger. each 3/4 in. (12. 3119 Methacrylate Balls Methacrylate Balls 1/8 in. 5004A Tungsten Carbide Ball Set 5/16 in. 3117) or when running 3127 vials with 8011 adapter in the 8000D. 3114. Prevents caking. To use 3127 vials in 8000D.7 mm) diameter alumina ceramic ball for SPEX SamplePrep 8003 Vial Set. 8012 Vial Clamp Adapter for the 8000D Mixer/Mill Required when running 8010 adapter with vials 1 in. 3114SB Stainless Steel Ball Set 1/4 in.com Order Online 24/7: www.7 mm) and 3/4 in. (25. (12. reduces contamination. 8004A Tungsten Carbide Ball 7/16 in. (12. and 3117 vials if 8012 adapter is also used.7 mm) diameter silicon nitride ball for SPEX SamplePrep 8008 Vial Set.7 mm) and four 1/4 in.Section 1 Chapter 3 Section 1 Chapter 3 Grinding Media 3112 Methacrylate Balls Methacrylate Balls 3/8 in. Instructions included.5 mm) diameter. for SPEX SamplePrep 5004 Vial Set. Sold in units of 100. 8007B Stainless Steel Ball Set Two 1/2 in. (12. 3650 PrepAid Vertrel® XF Liquid fluorocarbon grinding aid. (12. The 8010 and 8011 multiple-sample adapters accommodate 1/2 in. (19. 8014A Agate Ball 1/2 in. 3118A Agate Ball 1/4 in.35 mm) diameter agate ball. (6. for simultaneous running in 8000M Mixer/Mill.35 mm) inch diameter steel ball.7 mm) diameter zirconia ceramic ball for SPEX SamplePrep 8005 Vial Set. Vials run at one time should be same length. Sold in units of 100. Sold in units of 100. (12. (19. (3.

spexsampleprep.For 230 V/50 Hz operation. Timer is not supplied Specifications: Dimensions: Weight Voltage: Power Cord: 19 in (48 cm) x 19 in (48 cm) x 40 in (102 cm) 225 lbs. gross (102 kg) 115 V/60 Hz or 230 V/50 Hz 3-prong standard North American plug for 115 V/60 Hz version 2-prong European CEE 7/7 plug for 230 V/50 Hz version Specifications: Dimensions: Weight Voltage: Power Cord: 13 in.Section 1 Chapter 4 Section 1 Chapter 4 SPEX SamplePrep 8530 Enclosed Shatterbox® 8530-115 Enclosed Shatterbox® .For 115 V/60 Hz operation 8530-230 Enclosed Shatterbox® . (60 cm) 135 lbs.com 51 . sold separately SPEX SamplePrep 8500 Shatterbox® 8500-115 Shatterbox® – For 115 V/60 Hz operation 8500-230 Shatterbox® – For 230 V/50 Hz operation • Features a cam-activated clamp that requires only moderate hand pressure to secure the grinding dish in the Shatterbox and is adjustable for containers of different heights • Perforated metal skirt provides ventilation for continuous operation.com Order Online 24/7: www. CE Approved • Features a cam-activated clamp that requires only moderate hand pressure to secure the grinding dish in the Shatterbox and is adjustable to secure containers of different heights • LCD display with environmentally safe. gross (61 kg) 115 V/60 Hz or 230 V/50 Hz 3-prong standard North American plug for 115 V/60 Hz version 2-prong European CEE 7/7 plug for 230 V/50 Hz version Motor: 1⁄2 horsepower @ 835 RPM Motor: 1⁄2 horsepower @ 835 RPM 50 Order Online 24/7: www.(33 cm) x 23 1⁄2 in. and a rubber cover protects against dust • Includes an anti-skid wood/rubber floor mount and an extra set of drive belts • Grinding containers are sold separately.spexsampleprep. push-button membrane switch • Soundproof enclosure reduces noise levels • Equipped with a safety interlock system and lockable casters • Wide choice of grinding containers. (33 cm) x 13 in.

(17.com Order Online 24/7: www. recommended load 30-100 mL.9 in. 3. (20. ring. (9 cm x 5. dish and lid all made of solid tungsten carbide.9 in. Includes puck. Nominal volume 650 mL. and lid. 8 kg). 17.spexsampleprep. (9. high. recommended grinding load 2-20 mL. puck and ring are solid tungsten carbide.spexsampleprep. dish with O-ring gasket and lid. Nominal volume 90 mL. 5 kg).2 cm x 8 cm. dish with O-ring gasket. high.5 kg). and lid. 3. puck. dish with gasket. Dish and lid are steel shells with tungsten carbide inserts.2 cm x 5. high. and lid. (15. Includes puck. Must be used either one or three at a time with 8507R Rack. Includes puck. all made of 52-100 hardened tool steel.7 lbs.4 cm. (17. 29 lbs. (15. and lid made of 52-100 hardened tool steel. and lid. 4 lbs. diameter x 3. 8506 Zirconia Ceramic Grinding Container Grinding container lined with Mg-stabilized zirconia ceramic. puck is solid zirconia ceramic.5 cm. Sample P/N Material Volume 8501 8507 8521 8504 8508 8505 8506 Hardened Steel Hardened Steel Hardened Steel Tungsten Carbide Tungsten Carbide Alumina Ceramic Zirconia Ceramic 20-50 mL 5-20 mL 30-100 mL 20-60 mL 5-20 mL 15-40 mL 15-40 mL Typical Sample Suitable for Weight Blending 50 g 15 g 90 g 50 g 15 g 40 g 40 g Y Y Y Y Y Y Y Suitable for Slurry Grinding Yes Yes Yes Yes Yes Yes Yes 52 Order Online 24/7: www.3 in. Nominal volume 340 mL. recommended grinding load 20-50 mL.6 in. 6. Includes puck. 29 lbs. 3. high.3 cm x 8. dish.5% alumina ceramic. Must be used either one or three at a time with 8507R Rack. recommended grinding load 15-40 mL. ring. dish with O-ring gasket.com 53 . 8521 Large Hardened Steel Grinding Container Large grinding container with dish. diameter x 2. 13 lbs. Nominal volume 240 mL. high.2 in. recommended grinding load 20-50 mL. 8505 Alumina Ceramic Grinding Container Grinding container lined with 99. Dish has reinforcing aluminum band. 12. 8 in. Includes puck.3 in. diameter x 3. 8508 Small Tungsten Carbide Grinding Container Small grinding container with puck. and lid. Nominal volume 170 mL. puck is solid alumina ceramic. high.5 kg). diameter x 3. Steel lid and aluminum dish are lined with alumina ceramic plates. 6. and lid.9 kg). 6 in. Steel lid and aluminum dish are lined with zirconia ceramic. ring.Section 1 Chapter 4 Section 1 Chapter 4 Accessories Grinding Dishes 8501 Hardened Steel Grinding Container Grinding container with puck. 1. Includes puck. dish and lid made of 52-100 hardened steel. 11 lbs. Includes puck. 7.2 in. dish with O-ring gasket.9 in. diameter x 2. diameter x 3.5 lbs. dish with O-ring gasket.5 cm x 8 cm. 8504 Tungsten Carbide Grinding Container Grinding container lined with tungsten carbide. recommended grinding load 2-20 mL. diameter x 2.6 in.5 cm x 7. and lid. Nominal volume 80 mL. dish.2 cm x 8 cm.3 in high. recommended grinding load 15-40 mL. 6 kg).3 in.9 cm. 8507 Small Hardened Steel Grinding Container Small grinding container with puck. 13 kg).2 in.2 cm. Nominal volume 170 mL. ring. 6.

Rack lid is matched to Shatterbox clamp. Instructions included. either 8507 or 8508. 8521).000 – 70. net (55 kg). consistency and throughput • Program allows the technician to enter final pressure desired. and other analytical methods • Automation improves sample uniformity. SPEX SamplePrep 3635 Automated X-Press® 3635-115 Automated X-Press – For 115 V/60 Hz operation 3635-230 Automated X-Press – For 230 V/50 Hz operation CE Approved • Unique programmable laboratory press • 35-ton (31. Instructions included.com Order Online 24/7: www. time to hold at the final pressure. and holds grinding containers down during operation.1-31. 8504.25 inches diameter (8 cm) Adjustable 2. (58 cm) x 11 in. 3650 PrepAid Vertrel® XF Liquid fluorocarbon grinding aid. One-quart bottle. gross (87 kg) 115 V/60 Hz or 230 V/50 Hz 1⁄3 horsepower 3-prong standard North American plug for 115 V/60 Hz version 2-prong European CEE 7/7 plug for 230 V/50 Hz version 10–35 tons ram pressure (9. Specifications: Dimensions: Weight: Voltage: Motor: Power Cord: Force: Platen Size: Daylight: Upper Screw Adjustment: 23 in. 25 grams (approximately 24 mL) in dropper bottle.8 metric tons or 20.com 55 . evaporates after grinding. all three should be the same kind.) 3. and four locating pins for positioning one or three grinding containers.Section 1 Chapter 4 Section 1 Chapter 5 Racks and Holders 8507R Rack Holds one or three 8507 or 8508 grinding containers in Shatterbox.000 Ibs.0 inches (5 to 15 cm) 3.5 cm) 54 Order Online 24/7: www. (82 cm) 121 Ibs. and interval to return back to zero pressure • Typical pressing cycle is less than two minutes • Accepts all SPEX SamplePrep die sets • A safety interlock and automatic pump shut-off safety valve ensure safe operation PrepAid® Grinding Aids & Sample Binders 3640 PrepAid Propylene Glycol – (C3H8O2) Liquid grinding aid. 190 lbs.0 to 6.spexsampleprep.spexsampleprep. When 8507R Rack is used with three grinding containers. Prevents caking. IR.0 inch (2. 8525 Transporter For lifting and moving heavier Shatterbox grinding containers (8501. twin handles make for easy twohanded lifting. Rack base plate has handles to lift Rack into or out of Shatterbox. (28 cm) x 32 1⁄2 in. Spring-loaded clamp grips lip of dish.8 metric ton) hydraulic press ideal for repetitive pressing of sample pellets for XRF.5 inches (9 cm) Platen Movement: 1. reduces contamination.

000 lbs.4 cm) 56 Order Online 24/7: www. (76 cm) 120 lbs.com Order Online 24/7: www.9 metric tons or 0–24.spexsampleprep. (0 to 23 cm) Specifications: Dimensions: Weight: Force: Platen Size: Daylight: 12 1⁄2 in.6 cm) Platen Movement: 1 3⁄4 in. (47 cm) x 30 in.2 cubic meters per minute or 198 liters per minute) of air 3621 SPEX SamplePrep-Carver Model C Full-size 12-ton (10. net (90 kg) 0–12 tons (0-10. (41 cm) 200 Ibs.) Platen Movement: 5 in.7 metric ton) maximum pressure is ideal for pressing sample pellets for XRF. net (55 kg) 205 lbs. (15 x 15 cm) Adjustable.9 metric ton) manual hydraulic press with buffer plate accepts all SPEX SamplePrep pellet dies. Specifications Dimensions: Weight: Force: Platen Size: Daylight: 36 in. or 6.7 cm) 6 x 6 in. (38 cm) x 16 in.000 Ibs. diameter (14 cm) Adjustable 1 1⁄4 to 5 3⁄4 inches (3. gross (93 kg) 0-25 tons (0-22.) 5 1⁄2 in. • Patented air-actuation system combines ease of use of a motorized press with the simplicity of a manual press • Single push-button operation • Pressure is measured with a dial and the pressure control valve can be set to produce repetitive. (12. manually controlled laboratory press • 25-ton (22.1 atm.Section 1 Chapter 5 Section 1 Chapter 5 SPEX SamplePrep 3628 Air-Actuated Bench-Press® 3628 Bench-Press. CE Approved • Air-actuated. IR.com 57 . (32 cm) x 16 in. and other analytical methods • Compact design ideally suited for laboratory benchtop applications.spexsampleprep. reproducible pressures • Neither hand-pumping nor electrical hook-up is required • Can be operated off an air compressor or a tank of compressed air • Requires 90 psi (6.7 metric tons or 0-50. (91 cm) x 15 in. 0 to 9 in. (4.2 to 14.2 bars) and 7 cubic feet per minute (0.

round (10 cm) 5 3⁄4 inches (14. and knock-out ring for sample disk extraction.1 metric tons). Load limit 50 tons (45. 35 mm Tungsten Carbide Pellets available (3616C). net (52 kg) 0–12 tons (0-10. Load limit 50 tons (45. (48 cm) x 24 in. 31 mm Tungsten Carbide Pellets available (3623C). (51 cm) x 10 1⁄4 in.7 metric ton) manual hydraulic press with buffer plate accepts all SPEX SamplePrep pellet dies. Order Online 24/7: www. base.2 lbs (1 kg).4 metric tons). weight 2.com 59 . plunger.13 mm Die Set. net (158 kg) 0–25 tons (0-22. base.8 lbs (4 kg). Specifications Dimensions: Weight: Force: Platen Size: Daylight: 42 in.7 metric tons or 0–50. weight 6. Accessories Pellet Die Sets SPEX SamplePrep dies are designed to fit all SPEX SamplePrep presses. base. Set includes evacuable die body. Ideally suited for IR work with SPEX SamplePrep 3616 . plunger. and they are equally compatible with other standard laboratory presses using stand-alone dies. weight 2. and knock-out ring for sample disk extraction.000 Ibs. O-ring vacuum seals.com 3622 SPEX SamplePrep-Carver Model M 25-ton (22. 3610 Die Set – 10 mm Used to form KBr disks for IR analysis.4 metric tons). two 13 mm polished steel pellets. Compatible with SPEX SamplePrep 3617 (38 mm) Spec-Caps.) 4 in. (23 x 23 cm) Adjustable.9 metric tons or 0–24. plunger.5 kg).6 lbs (3 kg). 3623 Die Set – 31 mm To form 31 mm standard sample disks for XRF. plunger. (26 cm) x 8 in.4 metric tons). weight 10 lbs (4. 3614 Die Set – 40 mm To form 40 mm sample disks. Set includes evacuable die body. O-ring vacuum seals. O-ring vacuum seals.2 lbs (1 kg).6 cm) Platen Movement: 5 1⁄8 in. Specifications Dimensions: Weight: Force: Platen Size Daylight: 20 1⁄4 in.000 Ibs. base. (16. plunger. Set in­cludes evacuable die body. two 35 mm polished steel pellets.Section 1 Chapter 5 Section 1 Chapter 5 3626 SPEX SamplePrep-Carver 12-ton Press Benchtop 12-ton (10. and knock-out ring for sample disk extraction. (20 cm) 115 Ibs. Set includes evacuable die body. Load limit 50 tons (45.spexsampleprep.9 metric ton) manual hydraulic press. 40 mm Tungsten Carbide Pellets available (3614C). Compatible with SPEX SamplePrep 3619 and 3619A Spec-Caps. O-ring vacuum seals. and knock-out ring for sample disk extraction.5 cm) 58 Order Online 24/7: www. Load limit 10 tons (9. Compatible with SPEX SamplePrep 3615 (33 mm) Spec-Caps. (107 cm) x 19 in. base. 0 to 9 in. O-ring vacuum seals.1 metric tons).spexsampleprep. two 10 mm polished steel pellets. Load limit 10 tons (9. and knock-out ring for sample disk extraction. two polished steel pellets. two 40 mm polished steel pellets.) 9 x 9 in. (0 to 23 cm) Platen Movement: 6 1⁄2 in. weight 8. (61 cm) 350 Ibs. 3616 Die Set – 35 mm To form 35 mm sample disks. (13 cm) 3613 Die Set – 13 mm Used to form KBr disks for IR analysis. Set includes evacuable die body.

It may be substituted for the 3619 30 mm Spec-Cap in all applications where flaring is recommended. Produces pellets 35 mm x 5 mm. and other analytical techniques. or together with SPEX SamplePrep dies at a discount.spexsampleprep. Please contact SPEX SamplePrep for further information. 3623W Die Sleeve-and-Plunger Set – 31 mm Used with 3623. sold in pairs. marked.30 mm 30 mm wide x 8 mm deep. Sold in units of 1000.spexsampleprep. Sleeve-and-Plunger Sets Sleeve-and-Plunger Sets allow easy preparation of XRF disks with binder matrix supporting a layer of sample. 3615M Spec-Cap – 33 mm Same as 3615. ideal for smaller amounts (<1 g) of analyte. prevents damage to die. Sold in units of 1000. 31 mm Evacuable Pellet die and PrepAid Sample Binder. Tungsten carbide pellets are much harder than steel. Instructions included. 35 mm and 40 mm tungsten carbide pellets which can be substituted for polished steel pellets. Thus reinforced. and has an unpainted surface. For routine pressing of abrasive materials. 3619 Spec-Cap® . sold in pairs. 3623C Tungsten Carbide Pellets . 3616ST Steel Pellets – 35 mm For 3616 die. Sold in units of 100. for 3623 die. but more brittle. Sold in units of 100. Spec-Caps® for Reinforcing XRF Sample Disks SPEX SamplePrep Spec-Caps are shallow. sold in pairs. sample disks are resistant to chipping and breaking. 40 mm Evacuable Pellet Die and PrepAid Sample Binder. 3613ST Steel Pellets – 13 mm For 3613 die. Produces pellets 31 mm x 5 mm. Instructions included. 35 mm Evacuable Pellet Die and PrepAid Sample Binder.31 mm For 3623 die. Forms stable XRF sample disks with binder matrix supporting small quantity of sample.com Order Online 24/7: www. 3614C Tungsten Carbide Pellets – 40 mm For 3614 die. The 3619A has been preflared for a snug fit in the 3623 31 mm Evacuable Pellet Die. Produces pellets 31 mm x 5 mm. Sold in units of 100. 3615 Spec-Cap – 33 mm 33 mm wide x 8 mm deep. sold in pairs. sold in pairs. Forms stable XRF sample disks with binder matrix supporting small quantity of sample. 3614ST Steel Pellets – 40 mm For 3614 die. and stored than unclad disks.Section 1 Chapter 5 Section 1 Chapter 5 Replacement Pellets Replacement or spare steel pellets for die operation can be purchased separately. Sold in units of 1000. Makes sturdy disks. 3619A Pre-Flared Spec-Cap – 31 mm 31 mm wide x 8 mm deep. Eliminates need for 3618 Edge-Flaring Tool. Outside painted to prevent seizure in die and to facilitate labeling. 3623ST Steel Pellets – 31 mm For 3623 die. 3616W Die Sleeve-and-Plunger Set – 35 mm Used with 3616. Outside painted to prevent seizure in die and to facilitate labeling. for 3616 die. 3614W Die Sleeve-and-Plunger Set – 40 mm Used with 3614. and are not guaranteed against breakage. sold in pairs. SPEX SamplePrep offers 31 mm. All replacement pellets are sold in pairs. Instructions included. 3619M Spec-Cap – 30 mm Same as 3619. for 3623 die. These sets can be purchased separately.com 61 . and are more easily handled. sold in pairs. XRF. 3619AM Pre-Flared Spec-Cap – 31 mm Same as 3619A. The Spec-Cap forms the bottom and sides of the finished pellet. thin-walled aluminum cups which are routinely used in the production of pressed-powder sample disks for OES. Forms stable XRF sample disks with binder matrix supporting small quantity of sample. 60 Order Online 24/7: www. 3616C Tungsten Carbide Pellets – 35 mm For 3616 die.

but a 450g bottle. Will bond 600-750 disks or provide matrix for 75-105 supported sample disks. 3644-450 PrepAid UltraBind® Same as 3644-150. 150g bottle. thus preventing sample loss and pellet jamming. Produces pellets 40 mm x 5 mm. Instructions included. UltraBind may include low levels of NaCl. Instructions included. 3646-450 PrepAid Paraffin Binder – (CnH2n+2) Same as 3646-150. or used undiluted as sample matrix with Sleeve-and-Plunger Set. Can be blended with sample at 10% by weight to form XRF sample disks. Instructions included. Instructions included. Sold in units of 1000. 3642-450 PrepAid Cellulose Binder – (C6H10O5)n Same as 3642-150. Instructions included. Will bond 200-250 disks. 3646-150 PrepAid Paraffin Binder – (CnH2n+2) ≤ 30 µm powder. 3625 Edge-Flaring Tool For 3615 Spec-Caps.spexsampleprep. Combines the moisture resistance of Paraffin Binder along with the ease of removing a prepared disk from the die set associated with the Cellulose Binder. 3644-150 PrepAid UltraBind® < 20 µm powder. Will bond 200–250 disks or provide matrix for 25–35 supported-sample disks. but a 450g bottle. Will bond 200250 disks or provide matrix for 25-35 supported sample disks. Outside is painted to prevent seizure in die and to facilitate labeling. 150g bottle. Will bond 600-750 disks or provide matrix for 72-105 supported sample disks. Can be blended with sample at 10% by weight to form XRF sample disk.spexsampleprep. 3618 Edge-Flaring Tool For 3617 and 3619 Spec-Caps. 150g bottle. but a 450 g bottle. for 3614 die. Will bond 600-750 disks. SPEX SamplePrep PrepAid® Binders 3642-150 PrepAid Cellulose Binder – (C6H10O5)n ≤ 20 µm powder.com Order Online 24/7: www. 62 Order Online 24/7: www. or used undiluted as sample matrix with Sleeve-and-Plunger Set.com 63 . Sold in units of 100.Section 1 Chapter 5 Section 1 Chapter 5 3617 Spec-Cap – 38 mm 38 mm wide x 9 mm deep. Can be blended with sample at 10–20% by weight to form moisture-resistant XRF sample disk. 3617M Spec-Cap – 38 mm Same as 3617. This tool widens the Spec-Cap rim to ensure a snug fit against the walls of the die. Instructions included.

com 65 .Section 1 Chapter 6 Section 1 Chapter 6 Katanax® K1 Prime Automated Electric Fluxer Available in 115 V/60 Hz and 230 V/50 Hz. and wet chemistry analysis. CE Approved • Six-position automated electric fusion machine • Prepare glass disks for XRF or solutions for AA. ICP. • Multi-lingual. and wet chemistry analysis • Throughput of 20-30 samples/hour • Includes built-in and customizable fusion methods • Multi-lingual.9” (27. • User-adjustable holding temperature to minimize ramping time.1” (58. 240V standard North American plug Specifications Voltages Power (max) Dimensions Mass: Power Cord 64 110-127VAC. spare fuses) • Instruction Manual Specification: Voltages Power (max) Dimensions Mass 220-240 VAC (50-60Hz) 3000 W 19” (48 cm) x 36” (91 cm) x 19” (48 cm) 95 lbs (43 kg) 3-prong.spexsampleprep. ICP. foolproof fusion method development wizard • Closed electric oven ensures all crucibles and molds are at the same temperature • Real-time temperature display • User-adjustable holding temperature to minimize ramping time • Both disk and solution units are included • Please specify mold size when ordering • Solution kit available. spare fuses) • K2 Prime Fluxer • Special outlet for installation hook-up • Tool Kit (hex keys. foolproof fusion method development wizard. • Independent heaters for the crucible and mold enable optimal temperature control and homogenization. Patent Pending Katanax® K2 Prime Automated Electric Fluxer For 230 V/ 50/60 Hz operation.6” (39. • Throughput of 5-7 samples/hour. • Please specify mold size when ordering.com Power Cord Order Online 24/7: www.spexsampleprep. • Prepare glass disks for XRF or solutions for AA. • Real-time temperature display.5cm) x 10.5cm) 66 lbs (30kg) 3-prong standard North American plug for 115V / 60 Hz Model 2-prong European CEE 7/7 plug for 230V / 50Hz Model Order Online 24/7: www. accommodates 5 Teflon® beakers. Complete K2 Prime Kit includes: Patent Pending Complete K1 Prime Kit includes: • K1 Prime Fluxer • Mold Heating/Cooling Unit • Unbreakable Teflon Beaker • Mold Holder • Power Cord • Instruction Manual • Tool Kit (hex keys. • Solution Agitation Unit available. • Includes built-in and customizable fusion methods. CE Approved models • Single-position automated electric fusion machine. 220-240VAC (50-60Hz) 1300W 15. • Both disk and solution units included.5cm) x 23.

26 g. Crucibles KP1001A Regular Crucible 95% Pt/5% Au. Platinumware. Price quotations are available upon request by contacting SPEX SamplePrep Customer Service at (732) 623-0465. KP1006A Heavy-Duty Mold – 32 mm 95% Pt/5% Au.30 mL • Straight-walled • Height – 32 mm • Outer Diameter – 41 mm • Made of 95% platinum. 66 Order Online 24/7: www. 30 g.spexsampleprep.30 to 40 mm • Outer Rim Diameter . KP1002A Heavy-Duty Crucible 95% Pt/5% Au. 30 g.com Order Online 24/7: www. Capacity 30 mL. 18 g.6 mm • Inner Base Diameter . 7154 Short Tongs For handling crucibles. the standard non-wetting alloy for borate fusions. 21 g. Straight-walled crucible designed specifically for the Katanax K1 and K2 Automated Electric Fluxers. Labware & Handling Tools 7151T Long Tongs For handling crucibles. Accessories SPEX SamplePrep offers crucibles made of 95% platinum and 5% gold. 5% gold (borate fusions) or 100% zirconium (peroxide fusions) • Standard or reinforced The Katanax K1 and K2 accept common round molds with the following characteristics: • Depth . Pt/Au crucibles and molds are offered in regular and heavy-duty versions. Please note that prices are quoted daily and may change due to market fluctuations. Straight-walled crucible designed specifically for the Katanax K1 and K2 Automate Electric Fluxers. Straight-walled crucible designed specifically for the Katanax K1 and K2 Automated Electric Fluxers with a thicker rim and bottom for greater durability. 55 g.39 to 49 mm KP0049A Zirconium Crucible 100% Zirconium. All platinumware is sold separately from the instrument. While the Katanax K1 and K2 Automated Electric Fluxers accept most common molds. 20 in.com 67 . Capacity 30 mL. heavy-duty platinumware lasts longer. has better temperature control. they require crucibles with very particular specifications. Capacity 30 mL. 25 g. KP1007A Mold – 35 mm 95% Pt/5% Au. Molds & Mold Holders KP1003A Mold – 30 mm 95% Pt/5% Au. 9 in. Zirconium crucibles are available for peroxide fusions. KP1005A Mold – 32 mm 95% Pt/5% Au. KP1004A Heavy-Duty Mold – 30 mm 95% Pt/5% Au. Racks & Holders 7151R Rack For holding six 7152 or 7152HP graphite crucibles.spexsampleprep. and is less likely to warp.Section 1 Chapter 6 Section 1 Chapter 6 Crucibles and Molds for Katanax K1 and K2 Automated Electric Fluxers The Katanax K1 and K2 accept crucibles with the following characteristics: • Capacity . Ni-Cr (nichrome) alloys used for rack withstand temperatures as high as 1200° C. Accessory Packages & Kits 7151 Rack and Tongs For holding six 7152 or 7152HP graphite crucibles. 36 g.

x 28.spexsampleprep.Section 1 Chapter 6 Section 1 Chapter 6 KP1008A Heavy-Duty Mold – 35 mm 95% Pt/5% Au.4 mL capacity. KP1009A Mold – 40 mm 95% Pt/5% Au. for 32 mm molds KP0039A Mold Holder. sold in units of 100. 0. 6-position 68 Order Online 24/7: www. Platinum crucible heater lid used in place of the zirconium crucible heater lid that is supplied with the K1. Custom sizes are available. Recommended for users concerned with possible contamination due to the zirconium lid. 6-position KP5604A – Mold holder. 8. x 19 mm.D. 40mm.6 mm. KP1011A Platinum Crucible Heater Lid 95% Pt/5% Au.com Order Online 24/7: www. 32mm. 48 g. Graphite Crucibles for Muffle Furnaces 7152 Graphite Crucibles 31. Mold Holders for the K1 Prime Automated Electric Fluxer KP0037A Mold Holder. 7153 Graphite Crucibles Micro.4 mL capacity. 30mm. High-purity graphite. KP0235A Mold Plate. 34 g. KP1015A Zirconium Crucible Heater Lid 100% Zirconium crucible heater lid as supplied with the K1.8 mm O.8 mm O. 8.D. KP0010A Teflon® Beaker Unbreakable Teflon beaker used for preparing solutions. sold in units of 10. Protects the crucible. 6-position KP5605A – Mold holder. 6-position KP5606A – Mold holder. KP1010A Heavy-Duty Mold – 40 mm 95% Pt/5% Au. 35mm. 16 g. for 30 mm molds KP0038A Mold Holder. 48 g. for 40 mm molds Mold Holders and Plates for the K2 Prime Automated Electric Fluxer All Mold Plates are designed to hold six molds. for 35 mm molds KP5603A – Mold holder. for 35 mm molds KP0040A Mold Holder. x 28. 7152HP Graphite Crucibles 31. 9.6 mm.6 mL capacity. High purity graphite. and aids in pouring.com 69 .D. conserves heat during fusion.spexsampleprep.5 mm O. Regular purity graphite. sold in units of 100.

x 38. flat bottom.D. Highpurity graphite. flat bottom. x 38. 32 mL capacity.5 mL capacity.7 mm I. sold in units of 10. flat bottom. 32 mL capacity. 33. High-purity graphite.D. 27 mL capacity.spexsampleprep.7 mm glass disks.com Order Online 24/7: www. 27 ml capacity. x 38. x 38. 50.spexsampleprep.0 mm.8 mm O. 31 mm I. 7158 Graphite Crucibles For casting 31 mm glass disks. Regular-purity graphite. High-purity graphite. x 38. 7157 Graphite Crucibles For casting 31 mm glass disks. flat bottom.4 mm O.0 mm. 50. sold in units of 10. 44.Section 1 Chapter 6 Section 1 Chapter 6 7155 Graphite Crucibles 38.D.D.D.1 mm O. Highpurity graphite. flat bottom.1 mm.1 mm O. 7156 Graphite Crucibles 38. 44. flat bottom. flat bottom.4 mm I.D. 7161 Graphite Crucibles For casting 40 mm glass disks.D.7 mm I.D.7 mm glass disks. sold in units of 10. 25.1 mm O.com 71 . 20 ml capacity. 7160 Graphite Crucibles For casting 33. 33.D. 20 ml capacity.D. x 46. sold in units of 10. 57. x 46. 7159 Graphite Crucibles For casting 33. 31 mm I. sold in units of 10.1 mm. 70 Order Online 24/7: www. Regular-purity graphite. sold in units of 10. 44.D. 25.4 mm O.D. sold in units of 10.4 mm I.D. 40 mm I.1 mm.1 mm.D.1 mm. Regular-purity graphite.8 mm O.

D.50 67.67/32. SPEX Fusion Flux Mixture LiT LiT/LiBr LiT/LiI LiT/LiM LiT/LiM/LiBr LiT/LiM/LiI LiT/LiM LiT/LiM/LiBr LiT/LiM/LiI LiT/LiM LiT/LiM/LiBr LiM LiM/LiBr LiM/LiBr 72 Composition (%) 100. A small amount of LiBr or LiI is added to the flux when making a “glass bead” (lithium borate sample disk).75/0.D. 57.89/0. at 6-7 mg per drop.83/0. to keep the melt from sticking to the crucible or mold.00 99.50 99.com Order Online 24/7: www.00 (12/22) 34.00/65.50/1.75/49.50/0.50 Pure FFB-1000-02 FFB-1005-02 FFB-1007-02 FFB-6700-02 FFB-6705-02 FFB-6707-02 FFB-5000-02 FFB-5005-02 FFB-5007-02 FFB-3500-02 FFB-3505-02 FFB-0000-02 FFB-0005-02 FFB-0007-02 Ultra-Pure FFB-1000-03 FFB-1005-03 FFB-1007-03 FFB-6700-03 FFB-6705-03 FFB-6707-03 FFB-5000-03 FFB-5005-03 FFB-5007-03 FFB-3500-03 FFB-3505-03 FFB-0000-03 FFB-0005-03 FFB-0007-03 Order Online 24/7: www.83/0. 44.67/0. Additional LiBr or LiI is added to the flux before making a solution for ICP/AA analysis.94/21.50/0.50 49.spexsampleprep. Please call SPEX SamplePrep for a free sample of flux.50 50.75/0.75/49.1 mm O.67/32.17) 100. NOTE: Glass disks cast in graphite crucibles will have rough faces which should be polished flat for analytical accuracy.00 49.50 66.50/0.00 99. Additives Additive Description LiBr crystal (125g) LiBr – 15mL solution LiBr – 15mL solution (10pk) LiI crystal (125g) – trihydrate salt LiI – 15mL solution LiI – 15mL solution (10pk) LiF crystals (125g) LiNO3 (250g) LiNO3 (500g) Part Number FFB-100-03 FFB-103-03 FFB-105-03 FFB-110-03 FFB-113-03 FFB-115-03 FFB-200-03 FFB-300-03 FFB-301-03 Fusion Flux SPEX SamplePrep is proud to offer the full line of SPEX Fusion Fluxes and additives.00/33.00 66.Section 1 Chapter 6 Section 1 Chapter 6 7162 Graphite Crucibles For casting 40 mm glass disks. so the entire melt is transferred to the beaker.50 35. x 38.5 mL capacity. These fluxes have exceptional qualities due to their purity and coarse glass-bead texture. sold in units of 10.00/50. or information on a custom flux. flat bottom.1 mm.50 (11. Regular-purity graphite.83/64.com 73 .spexsampleprep.50 98. LiBr solution in a dropper bottle is a convenient way to add non-wetting agent to a fusion. Some of these fluxes include lithium bromide or lithium iodide as a non-wetting agent. 40 mm I.

Many solid samples. XRF. Sold in units of 100. or used undiluted as sample matrix with Sleeve-and-Plunger Set. The Spec-Cap forms the bottom and sides of the finished pellet.spexsampleprep. require virtually no preparation. 3615 33 mm Spec-Cap 33 mm wide x 8 mm deep. Sold in units of 1000. and assure you of reproducible. This tool widens the Spec-Cap rim to ensure a snug fit against the walls of the die. and biological materials. marked. for 3623 die. Sold in units of 1000. Produces pellets 40 mm x 5 mm. The 3619A has been preflared for a snug fit in the 3623 31 mm Evacuable Pellet Die. 3619M 30 mm Spec-Cap Same as 3619. Sold in units of 1000. and stored than unclad disks. if homogeneous. and other analytical techniques. such as refractories. Then the homogenized material can be dissolved for analysis as a liquid sample. SPEX SamplePrep manufactures disposable sample-handling accessories for powder and liquid XRF samples. It may be substituted for the 3619 30 mm Spec-Cap in all applications where flaring is recommended. 3619AM 31 mm Pre-Flared Spec-Cap Same as 3619A. sample disks are resistant to chipping and breaking. Produces pellets 31 mm x 5 mm. 74 Order Online 24/7: www. These and the related products listed here will save you time and money. Sold in units of 100. Eliminates need for 3618 Edge-Flaring Tool. Outside painted to prevent seizure in die and to facilitate labeling. Others. Sold in units of 100. but a 450 g bottle. Will bond 600-750 disks or provide matrix for 72-105 supported sample disks. Outside painted to prevent seizure in die and to facilitate labeling. 3625 Edge-Flaring Tool For 3615 Spec-Caps.spexsampleprep. 3617M 38 mm Spec-Cap Same as 3617.com Order Online 24/7: www. 3618 Edge-Flaring Tool For 3617 and 3619 Spec-Caps. Outside is painted to prevent seizure in die and to facilitate labeling. Will bond 200-250 disks or provide matrix for 25-35 supported sample disks. or cast as a glasslike solid. thus preventing sample loss and pellet jamming. pressed into pellet form. and are more easily handled. thus preventing sample loss and pellet jamming.Section 1 Chapter 7 Section 1 Chapter 7 XRF Accessories Introduction The XRF spectroscopist is confronted with an almost infinite variety of samples. for 3623 die.com 75 . Instructions included. Over the last twenty years. 3642-450 PrepAid Cellulose Binder – (C6H10O5)n Same as 3642-150. and must be pulverized or fused. can be machined to the proper shape and run directly. Millions more liquid XRF samples have been run in SPEX SamplePrep X-Cells. Sold in units of 1000. 3617 38 mm Spec-Cap 38 mm wide x 9 mm deep. Instructions included. ores. thin-walled aluminum cups which are routinely used in the production of pressedpowder sample disks for OES. Produces pellets 31 mm x 5 mm. PrepAid Binders 3642-150 PrepAid Cellulose Binder – (C6H10O5)n ≤ 20 µm powder. contamination-free results. Produces pellets 35 mm x 5 mm. millions of powder samples for XRF have been pressed and protected in the SPEX SamplePrep Spec-Cap. from water to oil. an aluminum cap for reinforcing pellets. 150 g bottle. for 3616 die. and has an unpainted surface. 3619A 31 mm Pre-Flared Spec-Cap 31 mm wide x 8 mm deep. are too inhomogeneous. 3615M 33 mm Spec-Cap Same as 3615. Sold in units of 100. Liquid samples. This tool widens the Spec-Cap rim to ensure a snug fit against the walls of the die. for 3614 die. Can be blended with sample at 10% by weight to form XRF sample disk. Thus reinforced. Spec-Caps® SPEX SamplePrep® Spec-Caps are shallow. 3619 30 mm Spec-Cap® 30 mm wide x 8 mm deep.

0 22 19 22 Overall O. Sold in units of 100.0 31.6 Window Capacity Plane O. Can be run with open back.D.0 8. Squared snap-ring insures proper positioning in standard 31 mm sample hold­ers.6 31.6 24. Sold in units of 100. 3571 X-Cell. and open body. Prevents trapped air from forming a bubble under the window film when the X-cell is used in the upright position. sealed window back. Can be blended with sample at 10–20% by weight to form moisture-resis­­tant XRF sample disk. 150 g bottle. Polyethylene snap-on collar and cup with vent and reservoir. Combines the moisture resistance of Paraffin Binder along with the ease of removing a prepared disk from the die set associated with the Cellulose Binder.5* 0. 3644-450 PrepAid UltraBind® Same as 3644-150. Note: All measurements in mm unless otherwise noted X-Cell Number Description 3529 3561 3571 3527 3565 3577 *To fill line Overall Height 22. Requires window film.Section 1 Chapter 7 Section 1 Chapter 7 3644-150 PrepAid UltraBind® < 20 µm powder. or sample isolation.6 38. 43 mm Closed X-Ray Cell For Horiba Sulfur Analyzers. Aperture (mL) 30. Squared snap-ring design insures proper positioning in standard 31 mm sample holders.3 8.spexsampleprep. 3646-450 PrepAid Paraffin Binder – (CnH2n+2) Same as 3646-150.6 39.5 31. Will bond 600-750 disks or provide matrix for 75-105 supported sample disks. Can be blended with sample at 10% by weight to form XRF sample disks. SPEX SamplePrep X-Cells 3527I Bubble-Free Cell Insert Patented insert for the 3527 40 mm X-cell. Requires window film.6 31. Requires window film. 3565 X-Cell. Sold in units of 100. 3561 X-Cell. X-Cells 3527 X-Cell. Requires window film. or micro-porous film.spexsampleprep. or used undiluted as sample matrix with Sleeve-and-Plunger Set. Features recessed window. Chapter 3). Requires window film. For normal optics XRF spectrometers made by most major manufacturers. Bonds 600-750 disks. 6. collar. powders and other solids. 31 mm Micro X-ray Cell with Collar Two polyethylene snap-rings. Instructions included.5 24.3 mm window is centered in standard 31 mm sample holder. Will bond 200-250 disks. air-sensitive or hazardous samples. 31 mm Closed X-Ray Cell Polyethylene snap-ring and cup with snap-post vent and reservoir.0 22. Sold separately from 3527 X-Cell in units of 100. or micro-porous film. Versatile design accepts liquids.5 48.0 31. and cup with snap-post vent and reservoir. Will bond 200–250 disks or provide matrix for 25–35 supported-sample disks. 40 mm Closed X-Ray Cell Polyethylene snap-ring and cup with snap-post vent and reservoir. 150 g bottle. Sold in units of 100. 3646-150 PrepAid Paraffin Binder – (CnH2n+2) ≤ 30 µm powder. pastes. 3529 X-Cell. Requires window film.5 31 mm X-Cell 31 mm Universal X-Cell 31 mm Open End X-Cell 40 mm X-Cell 43 mm X-Cell Micro X-Cell 76 Order Online 24/7: www. 31 mm Double Open End X-Ray Cell with Collar Two polyethylene snap-rings. Instructions included. and open body. Can be run with open back. purging. Unique cell for small. collar.5 38.0 31. UltraBind may include low levels of NaCl (See Section 2. Instructions included.0 13 11.5 24. Sold in units of 100.0 10.com 77 . Instructions included. 32.5 31. but a 450 g bottle. Sold in units of 100.com Order Online 24/7: www.0 43. For hazardous or sensitive samples. but a 450 g bottle. 31 mm Universal Closed X-Ray Cell with Collar Polyethylene snap-ring.0 22. and fill mark on inside of cup. top can be fitted with a standard 7 x 13 mm serum bottle closure for injection. 3577 X-Cell.D. Instructions included.8 6. collar. sealed window back.

(73 mm) wide.2 mil (5 µm) thick. 500 per box with paper interleaving. Supplied as continuous roll 2 7/8 in. and Thermo Instruments.25 mil (6 µm) thick. 17 ft. Supplied as pre-cut circles 2 1/2 in. Supplied as pre-cut circles 3 1/4 in. 300 ft. (82. (73 mm) wide. 3520 Polypropylene Window Film (Roll) 0. (15 m) long. Supplied as pre-cut circles 2 1/2 in.5 mm) diameter.2 µm pores. (73 mm) wide.6 mm) diameter. Supplied as continuous roll 2 7/8 in. 3517 Mylar Window Film (Roll) 0.spexsampleprep. Supplied as continuous roll 2 7/8 in. in box with serrated edge for tearing film to desired length. 78 Order Online 24/7: www. (63. 3521 Polypropylene Pre-Cut Circles 0.3 mil (8 µm) thick. (92 m) long.12 mil (3 µm) thick. 300 ft. (92 m) long. (92 m) long. 3525 Ultralene® Window Film (Roll) 0. 3512 Kapton Pre-Cut Circles 0. 500 sheets per box.5 mm) diameter. 500 sheets per box.2 mil (5 µm) thick. 50 ft. Supplied as pre-cut circles 2 1/2 in. The requirements of the application will dictate the type and size of X-Cell and which window material to use. 3518 Mylar Pre-Cut Circles 0. 3526 Ultralene® Pre-Cut Circles 0.5 mm) diameter. (63. 300 ft. in box with serrated edge for tearing film to desired length. (73 mm) wide. (92 m) long.com 79 . 3524 Micro-porous Teflon® Film (Roll) Film has 0. 300 ft. in box with serrated edge for cutting film to desired length. 3515 Mylar® Pre-Cut Circles (Large) 0. 500 sheets per box. Not a window film.3 mil (8 µm) thick. in box with serrated edge for tearing film to desired length.16 mil (4 µm) thick. Thin Film 3511 Kapton® Window Film (Roll) 0. Equalizes pressure when installed on back of 3571 and 3577 X-Cells. (5 m) long in box with serrated edge for cutting film to length. (73 mm) wide.16 mil (4 µm) thick. (63.Section 1 Chapter 7 Section 1 Chapter 7 SPEX SamplePrep X-Cells are designed to fit the major brands of XRF spectrometers such as PANalytical. (63. Supplied as pre-cut circles 2 1/2 in. in box with serrated edge for tearing to desired length. (51 mm) wide. Supplied as continuous roll 2 7/8 in. Rigaku.5 mm) diameter. Supplied as continuous roll 2 7/8 in. Supplied as continuous roll 2 in. 3516 Mylar Window Film (Roll) 0.spexsampleprep. 500 sheets per box.com Order Online 24/7: www. Bruker.25 mil (6 µm) thick.25 mil (6 µm) thick.

Section 1
Chapter 7

Section 1
Chapter 7

Film P/N Description 3511 3512 3515 3516 3517 3518 3520 3521 3524 3525 3526 Kapton Kapton Mylar Mylar Mylar Mylar Polypropylene Polypropylene Micro-Porous Teflon Ultralene Ultralene

Thickness Thickness (mil) (micron) Type Qty .3 .3 .25 .12 .25 .25 .20 .20 .20 .16 .16 8 8 6 3 6 6 5 5 Micro-Porous 4 4 Roll Precut Precut Roll Roll Precut Roll Precut Roll Roll Precut 50 ft (15m) 500 Circles 500 Circles 300 ft (92m) 300 ft (92m) 500 Circles 300 ft (92m) 500 Circles 17 ft (5m) 300ft (92m) 500 Circles

Diameter 2 ½ in.(63.5mm) 3 ¼ in (82.6mm) 2 ½ in (63.5mm) 2 ½ in (63.5mm) 2 ½ in (63.5mm)

Certified Reference Materials for Organic and Inorganic Spectroscopy and Chromatography
SPEX CertiPrep® has been providing Certified Reference Materials (CRMs) for spectroscopy and chromatography for over fifty-five years. Our products are manufactured in Metuchen, NJ, and used by laboratories around the world. As new technologies have developed, we made it our business to produce superior Certified Reference Materials for those instruments and technologies. We have a full line of inorganic and organic standards for AA, ICP, ICP-MS, IC, GC, GC/MS, HPLC and LC/MS. We built our reputation on providing chemists and environmental scientists with products that exhibit Quality, Reliability and Convenience. Our Web site offers online ordering capabilities, product searches, and a technical knowledgebase. Our SPoints program rewards our valued customers with SPoints that are redeemable for great gifts. To request the latest SPEX CertiPrep CRM literature, visit our Web site at www.spexcertiprep.com, or contact CRM customer service via email at crmsales@spexcsp.com or via phone at either 732-549-7144 or 1-800-LAB-SPEX, x444.

Services available from SPEX CertiPrep
Extended Customer Service Technical Customer Service is available 8:00 am - 5:30 p.m. (EST) Monday - Friday. Total Customer Satisfaction SPEX CertiPrep has always been committed to providing every customer with “Total Customer Satisfaction.” We take pride in ensuring every customer is satisfied with our products and services. Our support does not end when the product reaches the customer’s facility; we have technical support available to answer any question. New SPEX CertiPrep website SPEX CertiPrep’s easy-to-navigate Web site was designed to give our customers easier access to our large product offering and technical knowledgebase. Customers can view catalog products and pricing, place orders, and submit requests for custom standards. Registered users can also check order status, download Certificates of Analysis, and view their current SPoints balance. Our Web site also offers technical whitepapers, posters, and presentations. Visitors can contact us through the Web site’s “Live Chat” control for instant order and technical assistance. Visit us at www.spexcertiprep.com today!

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Order Online 24/7: www.spexsampleprep.com

Order Online 24/7: www.spexsampleprep.com

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Section 1
Chapter 7

Section 1
Chapter 7

Accreditations SPEX CertiPrep is certified by UL DQS for ISO 9001 and accredited by A2LA as complying with the requirements of ISO/IEC 17025 and ISO/IEC Guide 34. These certifications and accreditations cover both our organic and inorganic Certified Reference Materials, giving us the most comprehensive scope in the industry. SPEXertificate® SPEX CertiPrep’s SPEXertificate® is the most comprehensive Certificate of Analysis in the industry! The SPEXertificate® includes actual reported values for the final solution – not reported values of the starting materials or by a calculation. The certificate also includes trace impurity measurements for up to 68 elements, measurement uncertainty, and NIST traceability when available.

everything needed for instrument calibrations, calibration verifications, interference checks, calibration blanks, and sample spikes. The standards are to be used in conjunction with the US EPA’s Statement of Work for Inorganic Analysis; Multi-Media/ Multi-Concentration Document Number ILM06.0/ILM05.2. Claritas PPT® Grade Standards for ICP-AES and ICP-MS. SPEX CertiPrep Claritas PPT standards are a class of certified inorganic reference standards designed specifically for today’s new generation of trace ICP-AES and ICP-MS instrumentation. Our chemists have formulated this line of high-purity standards for user convenience and stability, while providing documentation tailored to extremely low levels of detection. Every Claritas PPT Standard is supplied with a comprehensive SPEXertificate® of Analysis that reports actual measured values in the solution of both the major analytes and up to 68 trace element impurities at PPT levels. Ion Chromatography The Certificate of Analysis for every Ion Chromatography Standard reports ICP trace metal analysis of the starting materials, classical wet assay values for the major constituents, and an ion chromatography check for the major ion(s). SPEX CertiPrep Eluents are made from high purity salts and filtered ASTM Type I water. Ion Selective Electrode Standards Ion Standards are compatible with all of the leading Ion Selective Electrodes and ionic strength adjustment buffers and are made from high purity salts and filtered ASTM Type I water. Organometallic Oil Standards SPEX CertiPrep presents a comprehensive offering of 37 single-element standards at 1000 µg/g and 5000 µg/g in base oil; popular 23-, 21-, 12- and 5-element blends in base oil; sulfur in #2 diesel fuel; sulfur oil standards for diesel fuel analysis in base oil; and base oil and kerosene blanks. These standards are commonly used for the determination of wear metals in engine oils and other lubricants in machines such as automobiles, aircraft, heavy equipment, trucks, locomotives, and military vehicles. Consumer Safety Standards SPEX CertiPrep offers a line of Certified Reference Materials for a range of Consumer Safety Products analysis. We offer standards designed for the analysis of metals in plastic toys, Phthalates in polyethylene, and RoHS/WEEE analysis. Organic Reference Materials for GC, GC/MS, HPLC & LC/MS Each standard is sold in 1 mL ampules and comes with a pre-labeled “transfer/storage” vial for extending shelf life. The concentration of each analyte in the standard is optimized, taking into account the vapor pressure, evaporation rates, breakdown rates and dilution schemes. SPEX CertiPrep offers stock standards used with environmental testing methods for 500 Series Drinking Water Methods, 600 Series Wastewater Methods, and 8000 Series Solid and Hazardous Waste Methods.

Products available from SPEX CertiPrep
Custom Standards SPEX CertiPrep offers a comprehensive custom Certified Reference Materials program to fit the needs of each customer. Custom standards are designed around the requirements of our customer’s individual methods or procedures. Our chemists evaluate the custom standards request and determine elements/ analytes compatibility and standard matrix needed to keep the product stable. We have an established database of chemical interactions from our years of standard manufacturing experience to help ensure every custom standard we product is of the highest quality. We offer custom standards for most of our inorganic product lines in volumes of 100 mL, 250 mL, 500 mL and 1L. Organic customs are available in ampules from 1 to 20 mL. We can recommend standards that will work with specific methods and prevent interferences. Contact us 1-800-LAB-SPEX or www. spexcertiprep.com for further information. Assurance® Grade Standards for ICP and AA SPEX CertiPrep’s Assurance® Grade Single Element Standards are high quality calibration standards for both AA and ICP instrumentation. Each Assurance® Grade Single Element standard comes with a Certificate of Analysis that lists the values of the main element measured by two independent methods, and reports actual measured impurities of up to 30 elements. Assurance® Multi-Element Solution Standards SPEX CertiPrep offers a large catalog of multi-element standards formulated for the most common environmental analyses. Stock standards include a number of blends containing metals of concern in groundwater, drinking water and solid waste. Assurance® Contract Laboratory Program (CLP) Standards CLP standards are a complete series of multi-element standards and blanks designed for use in the U.S. Environmental Protection Agency’s Contract Laboratory Program, or CLP. These solutions provide
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Section 1
Chapter 7

Contamination Control Products Made for Chemists by Chemists®. Our line of contamination control products are designed by SPEX CertiPrep’s chemists in response to the need for cost-effective, easy-to-use equipment and high-purity matrix/wash blanks for the clean laboratory environment. Our Pipette Washer/Dryer is lightweight, compact, convenient to use, and made of durable polyethylene. Independent valves control flow of water to the back and front rows of washer. The unit contains 23 cone-shaped plastic pipette holders which are designed to accommodate pipettes from 0.5-250 mL in size. An optional pump and basin are also available. Sub-boiling Acid Stills are available in PTFE or Quartz; these Acid Stills allow the preparation of ultrapure acids right in the laboratory at a fraction of the cost of purchasing them ready-made. Solids and Matrix Based Reference Materials SPEX CertiPrep offers a wide range of Solid and Matrix based Certified Reference Materials to customers worldwide. We provide over 8000 RMs and CRMs sourced from over 100 producers across the globe. CRMS and RMs for: • Metal – Disks • Metal – Chips • Ferro-Alloys • Geological Samples • Refractory Samples • Industrial By-Products/Process • Oil & Coal • Food & Agriculture • Environment & Health • Biological Fluids • Pure Chemicals • Physical Testing

Section 2

Technical Information

Please visit our website for more details: www.spexcertiprep.com.

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SPEX SamplePrep offers a full range of cryogenic. After homogenization. Freezer/Mill technology.6mL up to 50mL. Thus there is no cross-sample contamination. A detailed explanation of the various cryogenic techniques can be found in Section 2. Chapter 2. and electronic controls which allow an entire grinding sequence to be programmed. The loading of the beads should always allow adequate movement inside the sample vials but can be up to 80% of the total sample volume.spexsampleprep. The method is one of the few that totally avoids possible cross-contamination between samples because both vials and grinding media are disposable. Details of different extraction techniques and appropriate grinding media for different sample types can be found in the application notes section of this handbook. Cryogenic Grinding Cryogenic grinding of plant and animal tissue is a very effective technique for the Microbiologist. SPEX SamplePrep Freezer/Mills are cryogenic laboratory mills which chill samples in liquid nitrogen and pulverize them with a magnetically driven impactor. Tough tissues may require precooling to embrittle the sample and this also serves to preserve any temperature sensitive components such as RNA or Proteins. Speed and effectiveness of disruption can be increased dramatically by increasing the density. Samples that require extraction of nucleic acids must be kept at -80º C or lower during the entire extraction process. The higher the ratio of grinding media to sample volume.spexsampleprep. grinding media such as steel or ceramic balls or glass beads are vigorously agitated inside a sealed vial or titer plate with the sample. Utilizing SPEX SamplePrep Freezer/Mills will maintain the sample temperatures well below these critical temperatures during the automated grinding sequence. The size and amount of the grinding media used is important.Tissue Homogenization / Cell Lysis Chapter 1 Section 2 Tissue Homogenization / Cell Lysis Section 2 Chapter 1 Bead Milling Bead milling is the preferred method to disrupt a variety of microorganisms and plant or animal tissues. These features have made the SPEX Freezer/Mill the most effective in the world. For samples that are soft or flexible at room temperature. The Geno/Grinder® has also been successfully used for pesticide residue extraction from fruit and vegetable samples using the QuEChERS technique. SPEX SamplePrep offers a comprehensive range of grinding media. Kryo-Tech® accessories for this purpose. It is considered the method of choice for disruption for yeast and fungi and tough-to-disrupt cells like bacteria and microalgaew.com Order Online 24/7: www. 86 Order Online 24/7: www. The powerful and compact design enables complete disruption with or without buffer in about 1-3 minutes with high yields. Low shearing of nucleic acids can be achieved by varying the agitation speed of the mill. the “mill of last resort” for many normally ungrindable samples. cryogenic grinding may be the only viable technique for processing your samples. The patented design with a true linear grinding motion provides the most efficient mechanism for tissue homogenization and cell lysis. the beads settle and the cell extract can be removed. vials and titer plates for samples ranging from 0. Each sample is placed in a separate grinding vial which is immersed in a liquid nitrogen bath inside the mill.com 87 . The Geno/Grinder® offers analysts a versatile high-throughput bead mill for plant or animal tissue homogenization. has been built into three models. Disruption or cell lysis occurs as a result of the crushing action of the grinding media as they collide with the sample. The most commonly used grinding balls are steel ball bearings of 4mm in diameter. In bead milling. All models include significant safety features. the faster the rate of cell disruption. form and amount of grinding media in the sample vial or titer plate. and the low temperature of the sample is maintained during grinding. field-proven since the 1960s. provided there is still adequate agitation of the bead slurry.

The hallmark SPEX SamplePrep Freezer/Mills.spexsampleprep. The following charts are available to assist you in your selection of a SPEX SamplePrep mill and grinding container. SPEX SamplePrep has laboratory mills and grinding containers capable of pulverizing and blending all kinds of samples. so after use the container is cleaned and not the mill. Chart B – Compostition of Standard Steels Used in SPEX SamplePrep Equipment and Accessories This chart is essentially an extension of Chart C that lists all the steel alloys used in SPEX SamplePrep grinding containers and accessories. feel free to contact our product specialists. etc. All these mills have multiple-sample capacity with smaller samples. SPEX SamplePrep mills were designed for spectroscopists who were concerned not only about reducing samples to uniform homogeneous powders. dissolved. The 8000M and 8000D Mixer/ Mills are high-energy ball mills that not only pulverize samples in the 10 gram range but are suitable for blending powders and making emulsions up to approximately 60 mL. most polymers. Then the sample can be adapted to a particular analytical technique. and a wide choice of grinding container sizes and materials. and maintaining cryogenic temperatures in the vial during grinding. with a density of approximately 1. with the theoretical composition of each given in percentages. The 6770. 88 Order Online 24/7: www. but also about what was added to the samples during processing. 6870 and 6970 EFM Freezer Mills are unique cryogenic mills that can grind almost any “ungrindable” sample. pressed into a sample disk.3g/mL. from metals to plastics. Clearly the analyst must choose the proper weight for his sample. They are not for batch or production milling.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending Section 2 Chapter 2 When to Pulverize The nonhomogeneity of materials in the real world presents a serious sampling dilemma: how to represent a large. durability. (If your lab deals with a variety of samples. Forty years after its introduction the Freezer/Mill remains the most widely used and most effective cryogenic mill in the world. resistance to abrasion. including all plant and animal tissue. more than one type of container may be necessary). for maximum on-the-job flexibility over a wide range of applications. fused. The recommended maximum sample volume for grinding is approximately 20% of a container’s volume.com 89 . you have a choice of several proven SPEX SamplePrep mills. or containers. hardness. The information that follows addresses these concerns and can help you to select the proper SPEX SamplePrep mill and grinding container for your application. The “typical grinding sample” is quartz sand. often nonuniform whole with a small analytical sample. The 8500 and 8530 Shatterboxes are ring-and-puck mills that are ideal for rapid grinding of samples up to approximately 100 grams. but for rapid.com Order Online 24/7: www. and their suitability for your applications. Freezer/Mills require liquid nitrogen for chilling the sample. If your samples can be pulverized by impact at room temperature. Often the best approach is first to take a quantity of the material large enough to be compositionally representative and reduce it to a fine homogeneous powder. The 5100 Mixer/Mill is a smaller high-energy ball mill. for blending 40–50%. These are usually the basis for selecting the proper container for a particular application. and used as is. or we can loan you a mill for short-term trials in your own lab.spexsampleprep. and countless other samples that are resistant to room-temperature milling. efficient grinding of analytical samples ranging in amounts from less than one gram up to approximately 100 grams. with about 10% the sample capacity of the 8000-series Mixer/Mills. in a volume conducive to efficient grinding. based on its density and other characteristics. in 5 minutes or less. Chart A – SPEX SamplePrep Sample Container Materials Selection Chart This chart reviews the key properties of each grinding container material. the more confident you can be that they will do the job you need to get done. The more you know about SPEX SamplePrep mills. Mixer/Mills and Shatterbox all have separate grinding containers for individual samples. and pesticides to pharmaceuticals. rocks to living tissue. How to Select a Laboratory Mill and Grinding Container SPEX SamplePrep mills are intended for the analytical laboratory. including major and minor elements. To discuss any SPEX SamplePrep mills and containers. We also offer test-grinding of your samples in our applications lab. and efficiency. Optimum grinding efficiency is achieved with samples toward the middle of the volume range.

3127 3613.50 - - - 3117 Order Online 24/7: www.com Order Online 24/7: www. Mn.com 91 .03 - 1. Mn. 6871. Ca. 3616.30 0.6 Moderate High Rockwell:C 60-65 Mohs: 5 – 5 ½ Rockwell: C 55-60 Mohs:5 – 5 ½ Rockwell: C 55-60 Moderate Moderate High High 0. 6753.45 ASTM 06 - 6752. 8501.25 Agate Si Al. 3614. C Stainless Steel Fe.25 - 0.6 - - - 6771.60 max - - Mohs: 8 ½ + Knoop: High Long-wearing Very High 1400-1800 Subject to breakage Mohs: 9 Very High Rockwell: R45N 83 Knoop: 2100 Extremely High Long-wearing Moderate Brittle Very long- wearing Moderate Moderate 8-10 8-12 - - 17-19 18-20 12-14 14.60 max Compositions are theoretical.00 max 16-18 - 0. Mg Mohs: 5 ½ .045 max 0. Hf Silicon Nitride Si Y.00 max 1. Al.20-0. K. 8007.20 max Plastic C - Mohs 1 ½ Low Low Disposable 1 All reported less than 0.00 max 1.060 max 0.35 0. Na. 8004SS 5200.40 Type Carbon Number % 0.10 - - 0.00 max 1.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending 2150. Mn. Si1 Cr-Free Steel Fe C.00 1. 6883 - 0. and determining which element(s) were added during the sample grinding.42 90 Tool Steel 303 304 410 416 0.03 0. Ti. 3127 Where Used 3114 Chart A: SPEX SamplePrep Container Materials Selection Chart Material Major Minor Hardness Element(s) Element(s) Resistance Durability Comparitive to Abrasion Efficiency High High High Chromium Nickel Molybdenum Zirconium % % % % 0. 8507. 8009.90 1.08 max 0. 0. 3114SB. The major element is iron. C. Actual composition of individual grinding vials should be determined by analyzing known samples ground in those containers. S.15 max 0. 8521 52-100 0. 8007B Section 2 Chapter 2 3117B.60 max 0. Mg1 Mohs: 6 – 7 Knoop: 550 – 800 Zirconia Zr Mg. Mo Tungsten Carbide W.00 max 2. Ca Mohs 8 ½ Extremely Very long- Rockwell: R45N 74-79 High wearing Knoop 1160 Mohs 8 ½ + Knoop 1600 Extremely High Very long- wearing Chart B: Composition of Standard Steels Used in SPEX SamplePrep Equipment & Accessories Silicon % 1. Cr Ni. minor elements listed below will vary. actual lot analyses are not available. Fe.10 0.02% 2.1 0. Fe.60 max - - 6753 440C 1.90 - - 1.60 0.spexsampleprep. Additional trace elements may be present and will change from lot to lot.00 max 0. Co Te.95-1.040 max 0.3-1.25 max 0.030 max 1. 8001.60 Moderate Low for grinding. Si.040 max 0.50 - Hardened Steel Fe Cr.15 min 0. Ca.6801.spexsampleprep. Nb Alumina Ceramic Al Si. High for blending 0. Si. 3623 6751.030 max Sulfur % 0.030 max 0.15 min Manganese Phosphorus % % 0.15 max 0.

In addition. some of which are easy to grind while others are very difficult. The new series of Mid-Size Vials has about half the capacity of the 6801 vial. The behavior of metals and metal alloys during cryogenic milling is highly variable. equivalent to weights of 10 to 20 grams for polymers and 20 to 40 grams for bone. and the 6771 Cr-Free Vial for grinding electronic components without adding chromium. temperature also affects the outcome: the colder a sample. As with samples ground at room temperature. grinding time. but can be made into thin films or fibers. Many flexible plastics which can routinely be milled in pellet form are difficult to grind as thin fibers and films. hair. but their physical form is important. corresponding to weights of 1 to 2 grams for polymers and 2 to 4 grams for bone. usually to a fine particle size: hair. The 6753 Microvial set includes three 6753V Microvials.” Many such samples respond to the strategies of reducing the sample volume. and clay minerals may be pulverized for XRD study without distorting their crystal structure. Successes have also been scored by using “filler” grinding agents such as detergent and quartz sand. as they become rigid when chilled. cereal grains. and even lengthening the pre-cooling period to 30 minutes or so. the pellets grind fairly easily.com Order Online 24/7: www. typical sample volume is 1 to 2 mL. Chilling times vary with the mill and the insulating ability of the sample but can range from 10 minutes to 30 minutes or more. weight. and the requirements of the analyst.spexsampleprep. while pure copper remains malleable. Polymers in general can be ground. These include polymers. or grinding time. The SPEX SamplePrep Freezer/Mills impels a steel impactor magnetically while the sample vial is immersed in liquid nitrogen. impure copper as well as many copper alloys can be ground without much trouble. typically between 30 mg and 200 mg. fingernails. Many analytical samples which are too flexible or sensitive to be impact-ground at room temperature can be embrittled by chilling. wood. bone. In cryogenic grinding. DNA was successfully extracted from the Romanov bone fragments after they had been ground in a SPEX SamplePrep Freezer/Mill. 10 times that of the 6770 Freezer/Mill. For this reason we at SPEX SamplePrep recommend that you discuss your samples and grinding requirements with one of our specialists before selecting a mill. If there is any question about whether a sample can be ground in a Freezer/Mill we will request that a portion be submitted for test-grinding. The 6801 Vial has at least 50 mL maximum sample capacity. For example. it rarely receives publicity. etc. muscle tissue. For efficient grinding. When a sample initially resists grinding. the finer the particle size will be. There are also many samples which degrade in various ways during normal grinding. The 6751 Vial has a sample volume limit of about 5 mL. but the films and fibers may remain flexible and become difficult to grind cryogenically. those processed cryo­genically vary enormously in their “grindability. fingernails. As the particles become smaller they become more flexible. The recent identification of the remains of Czar Nicholas II of Russia not only solved a mystery nearly eighty years old but also emphasized the importance of cryogenic techniques in both forensic and archaeological research. but whose critical properties are preserved by chilling. Cryogenic grinding presents unique challenges for designers of laboratory mills. chilling time. cotton fiber. grinding times rarely exceed a few minutes with either mill. rubber. plant stems and roots. Bone. a given sample material may exist in several forms. For example. and impact frequency for any sample ground in a SPEX SamplePrep Freezer/Mill are determined by experimentation. as the low temperatures required are very hard on mechanical equip­ment. Coal. As a rule of thumb. seeds. and 92 Order Online 24/7: www. the smaller the sample and the longer it is ground. bone. bulkier samples may restrict movement of the impactor. and other biological materials can be cryogenically ground in preparation for nucleic acid extraction without damaging DNA and even RNA through heating. Typical sample volumes are 10 to 20 mL. for example.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending Section 2 Chapter 2 Key Points About Cryogenic Grinding While cryogenic grinding has long been a vital sample preparation tool for the analytical chemist. skin. Nearly every naturally occurring material of biological origin can be cryogenically ground. it may not be because it is “ungrindable. can be cryogenically ground to retain its more volatile components. polypropylene is supplied to molders as small pellets.” and it is difficult to predict the optimum sample size. samples can be pulverized quickly. the experience of the operator. and progressively more difficult to grind. Each Microvial can hold a small amount of sample. We strongly suggest submitting samples for test grinding if there is any question about the suitability of our mills and techniques for your application. Once chilled. and muscle tissue. and then pulverized. Many silicone compounds remain elastic and hard-to-grind in any form. Limits of Cryogenic Grinding Not every substance which is difficult to grind at room temperature can be pulverized by cryogenic milling. Specialized grinding vials with similar capacity are the 6761 Poly-Vial for metal-free grinding of delicate samples. Metal samples as a rule should be test-ground. polymers in general cannot be ground to as fine a particle size as biological samples. increasing grinding time. textiles.com 93 . For the same reason. which remain flexible even at -200°C. the more finely it can be ground.spexsampleprep. Guide to Freezer/Mill Sample Capacity The optimum volume.

These samples (Fig. USB flash drives that act as portable hard disk drives. some of the components may be more fragile than others. However.spexsampleprep. and then break them up through impact.com 95 . 6871. but as much as 20-30 minutes for complicated components such as the USB flash drive and RAM module. each suited for their own special type of mill. The vial is then loaded into the Freezer/Mill and immersed in liquid nitrogen until the contents are thoroughly chilled. RoHS/WEEE states that if the component can be mechanically separated. Solder and Glass standards to come designed for RoHS WEEE compliance limits. uniform powder (Fig. mercury. Cryogenic grinding in the SPEX SamplePrep Freezer/Mill® is the easiest way to homogenize these materials. assures that the sample used for analysis is representative of the batch. chromium VI. Furthermore. or shearing. In the case of the Freezer/Mill. However. The definition of exactly what this means is an ongoing process. Metals. solder. crushing. much less an entire batch of boards. The concentrations of hazardous substances such as lead. would be first cut into manageable pieces. A small piece taken from a board here or there at random would not be representative of the whole board. it is impractical to break down the board into its several components. Some components may grind at room temperature. Grinding time can vary greatly depending on the type of sample and its pliability but a grinding time of 8-10 minutes can be expected in the case of the USB flash drive and RAM module. cross-sample contamination is easily controlled and sample integrity is maintained. wire. 6761. 1) are composites of many materials: metals. etc. This vial also contains a magnetically driven Cr-free impactor. Many components such as circuit boards. The sample inside the vial is pulverized. cadmium. the sample. for additional information. usually a matter of 10-15 minutes. or 6883).spexsampleprep. SPEX CertiPrep Ltd. and because the sample is isolated in a closed grinding vial. Cryogenic Grinding for RoHS/WEEE The Restriction of Hazardous Substances (RoHS) and Waste Electrical and Electronic Equipment (WEEE) Directives of the European Union were introduced to minimize the accumulation of hazardous waste in landfills from the disposal of electrical and electronic equipment. and in effect homogenizing them. The general principle behind cryogenic grinding is to chill samples until they are brittle. polymers and resins are difficult if not impossible to grind using traditional methods. These are then placed in the appropriately sized SPEX SamplePrep Chromium94 Order Online 24/7: www. sampling many boards. cryogenic grinding in the SPEX SamplePrep Freezer/Mill is the answer. in order to get an accurate analytical result. such as the USB flash drive or RAM module. and the larger RAM modules that are installed on computer motherboards. Order Online 24/7: www. and are very difficult to grind into powder. polybrominated diphenylethers (PBDEs). Please contact our European Division. then each component is subject to the RoHS limits. and some may not. 2) can then be used for XRF. or other types of analyses. The 6870 Freezer/Mill can also hold up four 6751. For such situations. We now offer a range of powder Polymers. these products and components must be reduced to homogeneous.com Free Grinding Vial (6771. substrates. Hence. one thing is certain. When all of these components are part of the same integral memory board. fusion. and polybrominated biphenyls (PBBs) are restricted in electrical and electronic products and/or components. and 6771 vials for simultaneous grinding of multiple smaller samples. The resultant fine. memory boards are made to be rugged and durable over a wide range of conditions. representative samples. Some may require a shearing action and other abrasion. resins. resins and other materials all have distinct and different properties when put through conventional laboratory mills.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending Section 2 Chapter 2 includes a Poly-Vial and Cr-Free Vial as well as the standard 6881 Mid-Size Vial. Consider analyzing circuit boards: for example.

Halide-releasing compounds corrode steel and should be ground in tungsten carbide. 2 2 1 1. 3) Three different nylons yielded similar results 4) 2x – two-minute grinds with one-minute cooling period between 5) Equal amount of sand added. Necessary for an important minority of samples. adding little contamination. it’s the workhorse of the lab. suitable for general-purpose grinding. but contributes Ni as well.com Order Online 24/7: www.spexsampleprep. alumina. Agate is harder than steel. It is about one and one-half times as dense as alumina. purpose: ethanol-toluene extraction 96 Order Online 24/7: www.9% silica and is extremely wear-resistant. Other than tungsten. brittle materials and for mixing and storing powders. and hardness superior to agate and zirconia. the contamination SPEX SamplePrep zirconia ceramic does contribute is often not important to the analyst.5 2 3 0. Tungsten carbide is substantially harder and heavier than steel. cobalt (a binder) is the major contaminant.5 2 2 2 2 Form 2 mil Piece Pellets Chunk Corrugated 10mm Flakes Dog Hair Clipping Chunk Whole Tooth 7mm Pieces Raw.spexsampleprep. And because it is mostly zirconium oxide with low percentages of magnesium oxide and hafnium oxide.5g of Tide detergent was added 2) Equal weight of sodium sulfate was added as dehydrating agent. With these vials only traces of organic impurities are added to your sample. grinding almost as fast as steel.5 0.5 1. SPEX SamplePrep’s containers have been selected with care to offer optimum capability in the lab. consider SPEX SamplePrep silicon nitride. It is extremely durable compared to agate. and magnesium present. with some silicon. Stainless steel is less subject to chemical attack. Silicon nitride is a tough space-age material with remarkable wear characteristics. Alumina ceramic is ideal for extremely hard samples or in cases where steel and tungsten carbide contaminants are objectionable. It’s also brittle and must be handled with care. zirconia. very low.5% pure aluminum oxide. Zirconia is a ceramic which in many ways approaches the ideal grinding medium. It is lightweight and brittle but very abrasion-resistant.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending Section 2 Chapter 2 Grinding Tests with the Freezer/Mill Material Aluminum Foil Black loaded thermoplastic Candle Wax Cardboard Fish Scales Hair Hot Melt Adhesive Human Tooth Human Vertebrae Mouse Skin Nylon 3 Key Points About Grinding Weight (g) 11 3 1. ½ Animal 3mm Beads 2mm Shot 10mil Sheet Fibers ½ in. If it is important to have a container whose only major contaminant is silicon. grinding is faster and contamination is minimal.55 0.5 0. The proper grinding vial or dish will greatly enhance analytical accuracy. They’re recommended as a long-term “best buy” for grinding almost anything. The grinding container is generally harder than the material to be ground and should be of a substance whose presence in the sample will not interfere with analysis. calcium. Since it is both hard and tough it wears very slowly. alumina ceramic vials are a helpful addition to any lab’s grinding armory. Hardened steel is durable and tough. Methacrylate and polystyrene vials and balls are ideal for pulverizing soft. Thick Sheet 5mm Shearings Wad Stick 2mil Tape Tape Pellets Chips Time* 3 x 2 3 x 1 2 2 x 2 2 x 2 2 2 x 2 1 x 2 2 x 2 3 2 x 24 3 2 3 x 2 2 x 2 2 2 2 2 x 2 2 x 2 3 x 1 2 x 2 Final Size Mesh 100-200 100-200 100-200 200 200 200 50 200 200 200 100-200 30 200 100-200 50-100 25-50 200 100 100 100 100-200 100 Grinding Container Materials Your selection of appropriate grinding and mixing containers is as important as your choice of a mill. Tungsten carbide vials and dishes are the most effective and versatile of all. Oil-Extended Sheep Wool Space Food Teflon Duct Tape Urethane Elastomer Wood *3 x 2 denotes grinding periods of 2 minutes each with re-cooling of approximately 4 minutes between grinds 1) 0.3 Permalloy 5 Polyethylene Polypropylene Rubber Rubber.5 1.5 0. and while it contains some yttria and alumina. overall contamination levels will be very. If cared for.5 0.5 1 1.com 97 . All SPEX SamplePrep alumina components are 99. some Fe and Cr contamination can be expected. or silicon nitride containers. When hard substances are ground in steel containers. and chemically inert to almost anything except HF. agate. tungsten carbide containers will last indefinitely. Agate vials are for the grinding and mixing of samples when organic and metallic contamination is equally undesirable. Agate is 99. Cr-free steel rusts easily but can be used to grind samples for RoHS/WEEE testing.

the fusing of particles under pressure. There are many different steels. rock. its selection is critical. they are unlikely to cake. Howard Kanare of Construction Technology Laboratories. then briefly grind an expendable portion of the next sample and discard it. as in many soils and cements. John. requires a leak-proof grinding container. Prepare a 3614 40mm Pellet Die with a flared 3617 Spec-Cap. analytical results can be refined accordingly. Once the contributed impurities and their proportions are known for a grinding container. and 7 mL of Vertrel XF. and the procedure can be as simple or as complex as your analytical objectives warrant. Major. almost no two grinding containers will have exactly the same elemental profile. preferably with your own analytical equipment and techniques. a lubricant and a binding agent. Dry soaps/detergents are lubricants. graphite is an anti-static agent as well as a lubricant. Caking can result from moisture. which may contain an abrasive. and grinding time). Lacking known samples. and transfer the ground sample/binder powder to the die. Advances in X-ray Analysis. SPEX SamplePrep’s selection of grinding container materials gives you maximum flexibility in choosing the best approach for your samples and analytical aims. one may grind portions of a single sample for increasing lengths of time. The simplest approach is to grind samples of known composition and see what is added by grinding. and removed afterwards. JCPDS – International Centre for Diffraction Data. Although slurry grinding is a reasonably reliable way of grinding a sample to micron-sized particles. Cleaning Containers Grinding containers should be cleaned between sample runs to avoid cross contamination. As the grinding container is the major source of contamination. Other grinding aids include polyvinyl alcohol. heat. Typical XRF samples such as cement. Seyfarth. In some applications a simple wipedown with ethanol may suffice. and we can only hint at the possibilities. and cobalt are not generally looked for in these slags. and check to see which elements increase in proportion to grinding time. it clearly will vary with the composition and condition of the grinding container. If the caking is due to moisture. In addition. both in the exact proportions of the major elements and in trace element composition. and the expected low-level contaminants of tungsten. Many of the techniques which make sample preparation an “art” are devoted to getting around caking. Larry (2001). Water. it is sloppy and time-consuming.com 99 . the size. after consulting the material safety data sheet. another practical approach is to brush out a container.com Order Online 24/7: www. A fluorocarbon fluid. if particles remain in suspension during grinding. 2. Often the formulas are proprietary.3 wt. 98 Order Online 24/7: www. and trace elements predictably found in SPEX SamplePrep grinding containers are listed in Chart A. and Arias. open the grinding container in a hood until the Vertrel XF has evaporated. Approaching a Universal Sample Preparation Method for XRF Analysis of Powder Materials. the sample can be dried before grinding. and toughness of the sample. and adds extra steps to one’s sample preparation procedure. or other liquids are added to the sample before grinding. and similar material can be routinely ground below 10 microns. we strongly recommend determining the exact elemental profile of your individual grinding containers. alcohol. and some also include an abrasive. regardless of the actual contamination level.0 minutes. carbon. and is available as a PrepAid product. clinker. In general. Propylene glycol must be used safely. hardness.spexsampleprep. the resulting profile can be fitted to the analytical results. When the contaminants are known and can be quantified. there are many proprietary grinding aids as well. Newtown Square PA. An example is the grinding of steel slags in a tungsten carbide container: tungsten carbide grinds rapidly. and the grinding container is easier to clean. The technique that follows was pioneered by John Anzelmo and colleagues at Bruker AXS and is here adapted for SPEX SamplePrep equipment: in an 8501 Hardened Steel Grinding Container load together 10 grams of sample. a DuPont product sold as a cleaning fluid. and quickly evaporates from an open grinding container without leaving any residue. Alexander.5 grams of 3642 Cellulose or 3644 Ultrabind binder. (While this level is important. is finding increased acceptance as a grinding aid. However. one’s objective should be to minimize contamination levels while avoiding elements which will interfere with analysis. each with specific compositions. Vertrel XF also lowers contamination levels from the grinding container. Grind in an 8530 Shatterbox for 2. static charge accumulation. and ceramics.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending Section 2 Chapter 2 Contamination Processing a sample always contaminates it. phenyl acetate and aspirin. Vertrel® XF. contamination is lowered. roughly 0. Our experience is that the “grindability” of almost any sample is enhanced by the use of Vertrel XF. and other causes. carbides. Successful analysis depends on recognizing the sources of contamination and controlling them. Other samples can be successfully ground with a variety of additives.spexsampleprep. In a swing mill such as the SPEX SamplePrep Shatterbox. Inc. Chapter 2. 44.%) for laboratory fine grinding of Portland cement and many minerals. Dry grinding is simpler and quicker. Because of these variations in grinding container composition. Section 2. there are inevitable variations from batch to batch of the same material. strictly speaking. Reference Anzelmo. has publicized the use of propylene glycol (one drop for up to ten grams of sample. so that a type of tungsten carbide engineered to have specific properties will have a different makeup from two different manufacturers. further particle size reduction is clearly inhibited. Grinding Aids When samples agglomerate or “cake” during grinding. it is available as a PrepAid product. Press at 20 tons for 0. it prevents sample caking during grinding. oven-dried samples can be ground quickly to less than ten microns without agglomeration or sticking to the mill walls. minor. Vol. Slurry grinding is an obvious approach. but requires much more careful matching of the technique to the sample.3 minutes in a 3635 X-Press.

. Zuniga. and then wash the container thoroughly. some of this powder is released into the environment. 7. M. pp. Vol. pp. pp.J.L. Materials Science and Engineering: A.. Infrared Mulls KBr pellets and Nujol mulls are quickly prepared with SPEX SamplePrep Mixer/Mills using small plastic (3111).. Serafini. we strongly encourage you to do your own search for applicable publications and references. L. Mixer/Mill. Vol. to convert an inhomogeneous solid to a fine. A. the 25-ton air-actuated 3628 Bench-Press. Acta Materialia. Steel and agate produce no IR background. Munir.. then rinse and dry the container. Nanostructured Materials. Drying is speeded by the use of a blow-dryer or similar appliance. Concas. and the 35-ton 3635 Automated X-Press. This includes mechanical alloying techniques. McCormick. 5246 – 5249. 1996. 416. chemical cleaning or multiple grinds with quartz may be necessary. 2006. Issue: 1-2. 110-119. Over the years nearly one hundred articles have been published in refereed scientific journals regarding the SPEX SamplePrep Mixer/Mill and its use for mechanical alloying. November. E. or even by checking the impurities appearing in successive batches of ground quartz sand. Dreizin. Respiratory Protection The general objective of sample grinding is. C. Hardened steel and even stainless steel containers can rust. N. Lai. Perez. pp. Effect of mechanical alloying conditions on the microstructure evolution and electrode characteristics of Mg63Ni30Y7. 2006. Ward. Huang... Mickel. A high-energy ball mill can be used to accomplish this. It should be noted that grinding containers become more difficult to clean with age because of progressive pitting and scratching of the grinding surfaces.J. August 2006. Inevitably. pp. 2266-2273..S. Effect of ball milling on simultaneous spark plasma synthesis and densification of TiC-TiB2 composites. Mechanical milling of magnesium powder.. S. T.. Pisu. Issue: 10.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending Section 2 Chapter 2 For more thorough cleaning one may grind one or more batches of pure quartz sand. Vol. widely known as the “SPEX Mill”. 47-56. 31.. agate (3118) and steel vials (3114).. pp. We offer 12-ton and 25-ton manual presses. such as the plating of container walls with a malleable metal. The following publication list is intended to highlight the more recent publications that we are aware of and is not intended to be comprehensive.A. Khorkounov. Journal of Materials Science. Vol. the SPEX SamplePrep 100 Order Online 24/7: www. R. Microstructural evolution during mechanical alloying of Mg and Ni. pp. kept in a plastic bag with a desiccating agent.. Issue: 16. Issue: 1-2. J. Nishimura.com Order Online 24/7: www. Gebert. Even harmless rock and cement samples can become potentially harmful to the respiratory system when finely pulverized.. Dave. Takacs.-L. Cao. A. Modeling of comminution processes in Spex Mixer/Mill. R.. Sharif.J. Luton. evaluations of grinding vial materials. Vol. Journal of Alloys and Compounds. Crawford. Issue: 11. Huang.. Vol. 434. January 2.. A study of mechanical alloying processes using reactive milling and discrete element modeling. Rojas. Vol. we recommend that steel containers be thoroughly dried after cleaning and. Lavernia. Issue: 1-2. Aybar. 67-79. Materials Science and Engineering A. if stored. R. We strongly recommend the wearing of an approved dust-mask during this procedure.. Cao. Ch. Vol..A. Issue: 1-2. January 2. pp. S. 2001. Pelletizing Samples Powder can be turned into pellets for X-ray and IR analysis with SPEX SamplePrep presses and dies. Lavernia.. Chen. B.J. International Journal of Hydrogen Energy. 267-276.-L. 2005. While iron oxide coatings can be removed by warm dilute oxalic acid solution or abrasive cleaning.spexsampleprep. M.N. 61. Synthesis of nanocrystalline Fe-B-Si powders. 2909-2918. Effect of the heating rate on crystallization behavior of mechanically alloyed Mg50Ni50 amorphous alloy.com 101 .J. allow running for extended periods.J. Over the past few decades. Locci.. June. homogeneous powder. 2006. Orru. In extreme cases. G. L. P..G. D.M. G. S. A. O. Formation of supersaturated solid solutions by mechanical alloying. June. Chemical Engineering Science. and numerous other topics. 3746-3760. A cleaning procedure is easily evaluated by grinding and analyzing a known sample. W. Nuri Celik. Aydinbeyli. The high energy of the milling action. usually during the emptying or cleaning of the grinding container. Gasan.. pp. is a process originally developed for the production of oxide dispersion strengthened super alloys.. December. 23-29. Issue: 1-2. also referred to as reactive milling.. October 25. H. An effective single-step grinding procedure for most grinding containers is to grind pure quartz sand together with hot water and detergent. Schoenitz.. E. P. The polystyrene spectrum appears as a constant background and can easily be subtracted. 2005. A. Hwang. 2006. Issue: 15. Issue: 1-2.. McHenry. Z... A safety advantage of this cleaning method is that it controls respirable airborne dust. R. mechanical alloying is often used as a solid-state powder processing technique that generates powders with unique microstructures. 53. and suggest the use of a laboratory fume hood. Perez. If you are considering the Mixer/Mill for your own mechanical alloying application. Schultz. A. Nanostructured Materials. Vol. and the durability of the motor.. 22–33. has become the industry standard for mechanical alloying applications. 391. E. P. Mechanical Alloying Mechanical alloying. Ordonez. 7. 1996. K. Journal of Alloys and Compounds. B. B.spexsampleprep. N. pp. Vol. April 5. E. Lavernia. June 8. M. of course. 318. Today. 41. Temperature of the milling balls in shaker and planetary mills..

They have an internal volume of 50-60 mL with a grinding capacity of about 10 mL and a blending capacity of 25 mL. Grinding Action The SPEX SamplePrep 8000 Series Mixer/Mills are functionally described as shaker mills or high-energy ball mills. It has even been used for grinding gallstones. Controls The 115 V/60 Hz version of the 5100 Mixer/Mill has a push-button. They are available in hardened and stainless steel. (5. the Mixer/Mill was used to grind samples.com 103 . the vial.spexsampleprep. resettable 30-minute timer. each end of the vials describing a “figure-eight”. and tungsten carbide. (19 mm) in diameter without adapters. inks. We recommend that vials for the 8000D Mixer/Mill be purchased and used in pairs to maintain the balanced motion of the clamps. tungsten carbide. Many of the earliest 8000 Mixer/Mills are still in service. catalyst supports. and hundreds of other brittle. The steel housing protects the entire clamp mechanism and vials and the lid is equipped with a locking latch. (6. It holds three 1⁄2 in. resettable 72-minute timer.4 mm) to 21⁄2 in. simply because it has proven extremely durable. The single clamp 8000M (previously the 8000) is known simply as “the SPEX Mill” to thousands of users and has been in service for over forty years. and methacrylate. zirconia ceramic. 8000 Series Mixer/Mills The SPEX SamplePrep 8000 Series Mixer/Mills are efficient compact laboratory mills capable of pulverizing one or two samples in the 10-gram range. minerals.com 102 Order Online 24/7: www. about two inches Order Online 24/7: www. The length of that swing is the same as the internal length of the vial.7 mm) diameter or two 3⁄4 in. rocks. and then blend them with graphite for arc/spark spectroscopy. If only one sample needs to be ground. the second similar vial should be clamped in place without the sample or grinding ball. vibration is reduced and component life extended. and pharmaceuticals. ceramics. often hard samples. All of the vials except for the agate are able to accommodate slurry grinding. The dual-clamp 8000D Mixer/Mill combines two clamps on one shaft with an electronic 100-minute timer (extended timer available). The 5100 Mixer/Mill can also be used for mixing powders and slurry grinding and is commonly used to blend samples with KBr for IR analysis. Applications 8000 Series Mixer/Mills have been used for pulverizing rocks. Early on. which contains a sample and one or more balls.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending Section 2 Chapter 2 SPEX SamplePrep Mixer/Mills 5100 Mixer/Mill The SPEX SamplePrep 5100 is a highly effective impact grinder and blender for samples weighing 1 gram or less and offers many advantages over other small mixers. The 8000M Mixer/Mills have also achieved notoriety for their ability to mechanically alloy small quantities of materials. agate. silicon nitride.spexsampleprep. hardened and stainless steel. (19 mm) diameter vials.35 mm) vertical oscillation. Now similar samples are ground and then blended with binder before being pressed into samples disks for XRF. Safety Features The rugged construction of the 5100 Mixer/Mill ensures a long life of heavy work. In each clamp.5 mm) long and up to 3⁄4 in. cement.8 mm) horizontal movement and a 1⁄4 in. Vials are available in plastic (polystyrene and polycarbonate). As the two clamps move in balance. (7. (12. alumina ceramic. (63. sand. (4. at every stroke there is an impact at the end of the vial – over 100 per second – to crush the material rapidly and reproducibly. Applications The 5100 Mixer/Mill is ideal for grinding small amounts of brittle samples such as minerals. A fan keeps the clamps and motor cool during operation. The clamp mechanism has changed little since the earliest versions.7 cm) wide and up to 3 in. or glass. slag. A one-inch (25. (25. Grinding Vials 8000 Series grinding vials are 2 1⁄4 in. The vigorous motion of the clamp is also excellent for making emulsions such as paints. and the 8000D Mixer/Mill with two clamps.4 mm) component of motion along the axis of the vial is complemented by two motions at right angles to the vial axis: a 3⁄16 in.1 cm) long. Now the wind-up timer has been replaced by an electronic 100-minute timer (extended timer available) and the mill’s safety features have been improved. agate. Grinding Action The high grinding and mixing efficiency of the 5100 Mixer/Mill is a result of its three-dimensional action. They shake one or two containers back and forth several thousand times a minute. is shaken in a complex motion which combines back-and-forth swings with short lateral movements. There are two versions: the classic 8000M Mixer/ Mill with one clamp. That is. Grinding Vials The continuously adjustable jaws accept vials from 1 in. The resulting action is consistent with the general shape and size of the vials. The 230 V/50 Hz version has a push-button.

The motors are also equipped with a thermal overload protector and the 230-volt 8000M and 8000D Mixer/Mills are CE Approved. The timer is factory-set for a maximum of 100 minutes but this may be extended to 1. Due to the amplitude and velocity of the clamp’s swing. enough to pulverize the toughest rocks. Prolonged continuous operation of Mixer/Mills requires special maintenance and warranty restriction may apply. Controls The electronic timer of the 8000 Series Mixer/Mills displays the programmed running time in minutes and seconds. A steel cabinet protects the entire clamp mechanism and vials.spexsampleprep. While the mill is operating. With each swing the balls impact against one end of the vial.000 or 10. Each clamp has a lock nut to prevent it from loosening while the mill is running. Push-button controls include start. Pulverizing and Blending Grinding Tests with 8000 Series Mixer/Mills Material Form Antimony Asbestos Bauxite Bismuth Bone Boron Carbide Brake Linings Carbon (activated) Carbnauba Wax Cement (Portland) Chrome Ore Chromium Cobalot Copper Ferro Cr Ferro Nb Floor Tile Germanium Ilmenite Limonite Ore Porcelain Potassium Pyrosulfate Reforming Catalyst Sand Silica Silica Silicon Silicon Pieces Fluff 60 mesh Chunks Chunks Chunks Chunks Pieces Piece Powder Chunk Chunk Pieces Shot 100 mesh - Chunk Pieces Grains Grains Chunk Fused Button 3mm Beads Grains Chips Chips Chunks 6mm Lumps Vial – Time (min) Amount (g) % Passing Method 325 mesh L-D WC-D HS-W PJ-D AC-D WC-D WC-D HS-D PJ-D AC-W WC-D WC-W WC-W WC-D WC-W WC-W WC-D L-D WC-D HS-W WC-D PV-D AC-D WC-D L-D AC-D WC-D L-D 5 10 30 20 10 15 * 10 2 30 10 20 10 15 20 60 ** 5 10 30 15 10 5 2 30 20 15 10 26 * 3 5 * 7 * 10 5 20 15 10 10 2 5 5 ** 5 5 3 6 5 5 12 15 5 10 5 97 * * 75 35 100 * 90 20 100 39 50 91 95 94 10 ** 38 98 100 83 100 * 86 * 97 92 30 104 Order Online 24/7: www.000 minutes for special applications such as mechanical alloying with the installation of a special chip.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending Section 2 Chapter 2 (5. Both of the 8000 Series Mixer/Mills are equipped with safety interlocks so that they cannot be operated with the lid open.08 cm). simultaneously milling the sample to a powder and blending it. slags. the timer also counts down the amount of time left in the run. Safety Features The 8000 Series Mixer/Mill’s rugged and durable construction is the reason why many of the original mills are still in use. Contact SPEX SamplePrep for details.spexsampleprep. stop and pause functions as well as timed programming. and ceramics.com 105 .com Order Online 24/7: www. each ball develops fairly high G-forces.

dried marsh-grass. noisy lab conditions and is still used in many locations where the working environment requires a rugged. The 8525 Transporter can be used to move the heavier grinding containers (8501. the full-sized. which can be run either one or three at a time with the 8507R Rack. with resultant particle size well below 200 mesh (approximately 50 microns). a puck. is available in hardened steel (8501).Satisfactory for extractions SPEX SamplePrep Shatterbox Since its introduction over thirty years ago. Vial – Time (min) Amount (g) % Passing Method 325 mesh HS-W WC-W HS-W HS-D HS-D WC-D WC-W WC-D WC-W AC-D AC-W 20 10 20 10 10 * 15 10 30 10 30 3 5 3 5 5 * 10 25 5 1 15 100 84 100 ** ** * 100 50 82 50 100 - 100 mesh - - - Chunks - Lumps - Pieces - 106 Order Online 24/7: www. grinding efficiency decreases as the container becomes more tightly packed. slags. with a nominal volume of about 100 mL.Suitable for X-ray or optical emission spectroscopy L – 8006 Acrylic Vial W – Wet ground (water or trichloroethylene slurry) D – Dry ground PV – 6133 Polystyrene Vial **. ceramics. and further reduced by the millstone-like action of the puck and ring against the container floor. The original SPEX SamplePrep swing mill. 8521) in and out of the Shatterbox.com Order Online 24/7: www. the 8500 Shatterbox. Grinding times are usually between two and five minutes. but have been used for hundreds of other materials including sulfur pellets. The 8530 Shatterbox is ideal for labs concerned with minimizing noise and maximizing safety. soils. and ring. Grinding Action The Shatterbox swings a dish-shaped grinding container in a tight. Note that the actual capacity of the containers is much higher. which offers the same grinding performance as the 8530 but without the timer and cabinet. 8504. and zirconia ceramic (8506). Now as then. simple mill. There are also small grinding containers made of hardened steel (8507) and tungsten carbide (8508). rocks. was developed for cement plants and steel mills with open. However. it is the most efficient way to pulverize up to 100 grams of brittle material to analytical fineness. and (in most containers) a ring. With grinding aids.spexsampleprep.com 107 . Applications Shatterboxes typically grind cement mix. the SPEX SamplePrep Shatterbox has become the most popular “swing mill” in the United States. As these grinding elements swing free inside the container.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending Section 2 Chapter 2 (con’t) Pulverizing and Blending Grinding Tests with 8000 Series Mixer/Mills Material Form Slag (blast furnance) Slag (copper) Slag (open hearth) Straw Tomato Stems Transite Tungsten Carbide Tungsten Welding Flux Wood Zirconium Carbide Table Reference HS – 8001 Hardened Steel Vial WC – 8004 Tungsten Carbide Vial PJ – 8002 Polystyrene Vial AC – 8003 Ceramic Vial *. tungsten carbide (8504). This corresponds to a typical sample size of 75-100 grams. Inside the container are the sample. Grinding Containers The standard grinding containers. puck. These grinding containers have about a fifth the capacity of the standard grinding containers and a typical sample size of 10 grams. high-speed horizontal circle. and (for example) the steel container has been used for as little as 4 grams and as much as 100 grams. 8530 Enclosed Shatterbox. and the original 8500. Typical grinding loads for samples such as cement. There are two Shatterbox models. rock. or slag are 50 grams for the steel and tungsten carbide containers and 30 grams for the ceramic containers. the sample is rapidly crushed between the walls of the container. and pharmaceuticals. alumina ceramic (8505). and ores. An oversize steel grinding container (8521) is also available and has approximately a 150 mL capacity. smaller samples can be reduced below 10 microns.spexsampleprep.

spexsampleprep.Grinding & Pulverizing / Mixing & Blending Chapter 2 Section 2 Grinding & Pulverizing / Mixing & Blending Section 2 Chapter 2 Controls The 8500 Shatterbox can be plugged into a standard lab timer that is not included with the mill. with which the mill can be moved about the lab and then fixed in place.5 5 3 4 3 4 6 2 3 2 6 2 4 3 15 2. It is shipped with a rubber-matted plywood base to prevent it from walking during operation. raw mix Iron Powder Sand Slag. The 8530 Shatterbox features a LCD display with an environmentally safe. The old screw-down clamp has been replaced with the cam-activated clamp to accommodate all SPEX SamplePrep grinding containers.com 109 . and the cylinders control movement of the lid when it is closed or opened. Grinding Tests with the 8501 and 8504 Grinding Containers 8501 8504 % % Form as Time Amount Passing Time Amount Passing Material Received (min) (g) 325 mesh (min) (g) 325 mesh Asbestos Cement (Portland raw mix) Ferro-chromium Ferro-maganese Ferro-molybdenum Ferro-niobium Ferro-silicon Fero-titanium Fiberglass Flourite Garnet (synthetic) Glass Graphite Mineral Fiber Insulation Oil Shale Pesticide Phosphate. push-button membrane switch. The interlock holds the lid closed whenever the mill is running. The 8530 Shatterbox includes a sound-insulated steel cabinet with lockable casters. Safety Features The 8500 Shatterbox contains a motor protected by a perforated shield to allow ample air-cooling for continuous running. 10% 108 Order Online 24/7: www.com Order Online 24/7: www. 5% **Household detergent (Tide) added. Safety features of the 8530 Shatterbox include a safety interlock and gas cylinders for the lid.4mm <100 mesh <60 mesh <80 mesh <10 mesh Chunks 12 2.spexsampleprep. blast furnace Fibrous >60 mesh >100 mesh >200 mesh <80 mesh <80 mesh <80 mesh <80 mesh Thin sheets >100 mesh Chunks Chunks Fiber Fiber 6.5 6 10 1 20 40* 25 25 25 25 25 25 10 50 200 35 15 15 60 50 40 5 100 10** 100 100 100 100 100 100 100 100 100 100 15 100 100 100 100 100 100 68 100 100 - - - - - - - - 2 - 10 2 - - - - - - 4 - - - - - - - - - 15 - 200 35 - - - - - - 100 - 100 96 100 100 - *Sodium alkylarylsulfonate added. and a rubber “skirt” shields the drive mechanism but is easy to move aside when the drive belts need to be replaced.

Although this can be accomplished by spreading the powder on the window film of a cell designed for liquid samples (such as a SPEX SamplePrep X-Cell). SPEX SamplePrep presses. IR disks are 13 mm across and consist largely of pure potassium bromide (KBr) with the pulverized sample blended in. by the matrix. and analytical requirements. incorporates a thin layer of sample on a disk of binder. which may be 31 mm. orthoboric acid. Running a series of standards or known samples will help to confirm that your chosen procedure results in accurate. and IR often require samples in the form of round. changing the particle size should have little or no effect. Although sample disks can be cast from a fusion melt. what size of die and what pressure to use. cellulose and paraffin Prep-Aid binders. While methods and mills for pulverizing are as varied as the samples themselves. Further. Preparing Powder Samples for XRF X-ray fluorescence spectrometry often requires the sample to be in a homogeneous powdered form with a planar surface. whatever the sample or analytical technique. makes this procedure easy. and 40 mm. flat-surfaced disks. 110 Order Online 24/7: www. 35 mm. most samples are blended with 50% pelletizing-grade graphite. the 25-ton 3628 Air-Actuated Bench-Press. Hence there is a limit to the depth to which the existing radiation can penetrate and result in fluorescence emitted from the sample. 40 mm. and Sleeve-and-Plunger sets to form sample pellets with a thin layer of sample on a binder matrix. used with the appropriate pellet die. IR.Pressing & Pelletizing Chapter 3 Section 2 Pressing & Pelletizing Section 2 Chapter 3 Introduction Analytical spectroscopic methods such as XRF. SPEX SamplePrep dies and presses ensure production of uniform sample disks. In the end.g. e. equipment. flatter surface that provides greater analytical accuracy and sensitivity. pellet die sets. XRF binders include cellulose. 35 mm. Typically. dies. Fortunately. The prime requirement for an XRF binder is that it does not contribute impurities. especially for wavelength XRF. graphite. or even larger. it will yield a higher intensity relative to the component of fixed particle size. The sampling method and the amount of sample to be ground. Pellet dies are available in the standard sizes of 13 mm. as the sample disk must be able to transmit infrared light. Accessories include: aluminum Spec-Caps to form and protect 31 mm. Chapter 4). As particle size becomes small relative to the critical thickness. paraffin. and the 35-ton 3635 Automated X-Press. when the particle size becomes small enough. This is due to the reduction in the size and extent of the voids in the sample. etc. spark ablation. and placed in a pellet die (with or without a Spec-Cap) to be pressed into a sample disk which will hold together and has a flat.spexsampleprep. as well as SPEX SamplePrep’s own UltraBind. the average penetration of the X-ray is of the same order of magnitude as the large particles. compression of the powder in a pellet die yields a denser. 35 mm. then split to obtain enough powder for an XRF sample disk. the resulting fluorescence is also absorbed. if the particle size of both components is decreased. Ultrabind. As the disk must be electrically conductive for these techniques. and the nature of the binders or additives. This results from the filling of the voids by components with smaller particle sizes. This disk is then placed in the sample holder of the XRF spectrometer. they often begin as a powder and are pressed to shape in a pellet die. OES. Reproducibility is a cardinal virtue in sample preparation. no Spec-Cap-type jacket is used. In case A. particularly useful when only a small amount of sample is available. pellet pressing requires simpler tools. XRF disks do not require a binder or Spec-Cap if the sample coheres under pressure.com Order Online 24/7: www. an exact procedure must be developed for each type of sample. however. the type of mill and the grinding time. since the average penetration depth covers many particles of many components. The following how-to suggestions apply chiefly to XRF sample preparation. in whole or in part. 40 mm pellets. There are many different procedures for preparing powdered samples for XRF analysis. polyvinyl alcohol. and proprietary products with special properties. compositionally uniform surface. a representative quantity of the sample is first pulverized. OES and spark ablation systems generally use 31 mm disks. Particle Size Effects It is impossible to say a priori how fine to pulverize a given sample.spexsampleprep. In case B. usually 6 to 10 grams. but the basic principles of forming sample disks are the same for OES. For preparation of pellet samples. as the particle size of one of two sample components is decreased. It has been known for many years that the X-ray fluorescence intensity from a sample will increase as the particle size of the sample is decreased. The major differences are the diameters of the disks. the intensities stabilize. and a change in the size of these particles would have a substantial effect on the fluorescent intensity. The diameter of XRF sample disks is dependent on the size of the spectrometer sample holder. and die accessories. Presses include a 12-ton and 25-ton SPEX SamplePrep-Carver manual presses. By the same reasoning. and pelletizing accessories are sophisticated in design. whether to include a binder or press the disk in a Spec-Cap. and often pressed in an aluminum Spec-Cap. (refer to section on Fusion Products beginning in Section 2. 31 mm. An alternate technique. but most analysts use a binder or a Spec-Cap or both. fluorescence intensities emitted from different sample components approach stable values. their respective intensities may increase or decrease depending on their relative absorption coefficients. As an X-ray enters a pelletized sample disk the exciting radiation is absorbed by the matrix.com 111 . but functionally simple and very effective. This depth is usually called the critical or infinite thickness. all these details may vary and must be worked out by the analyst to suit his or her samples. reproducible data. The SPEX SamplePrep Sleeve-and-Plunger set. When a particle within the matrix absorbs radiation. SPEX SamplePrep offers a full range of laboratory presses. That powder is blended with a binder if necessary. This is shown graphically on the next page.

112 Order Online 24/7: www. Pressing Sample Disks To make a sample disk. blended with a binder before pressing.). An optional aluminum cup such as the Spec-Cap contains the powder. The powder to be pressed must be fine-grained and homogeneous. flat. etc.com Order Online 24/7: www. stable. a pellet die set. Binders when properly used enhance analytical accuracy by stabilizing the sample disk and keeping it from distorting or crumbling during analysis and/ or storage. it may be necessary to add a binding/ briquetting agent such as cellulose. the analytical surface of the disk is not only flat but also uniform. measuring the particle size. which yields a durable disk of solid binder with a thin layer of sample on one side. and a machine for exerting the necessary pressure on the powder. in all its details. or UltraBind. it can be routinized to yield consistent. or pressed in a thin layer on a binder matrix.spexsampleprep. the limiting par­ticle size is often determined empirically by grinding the sample for a given length of time.com 113 . smooth material for sand­wiching the sample powder. protects the die bore against abrasive samples during pressing. in any case. binders. Compact. In an ideal sample disk pressed for XRF. If the pulverized sample material is not readily compressed into a stable. cohesive disk. reliable analytical results.Pressing & Pelletizing Chapter 3 Section 2 Pressing & Pelletizing Section 2 Chapter 3 In practice. and subsequently protects the pellet against chipping or breaking. and truly representative of the original sample. analyzing the sample. paraffin. involves the use of a sleeve-and-plunger set with a pellet die. A review follows of the processes and tools involved in the actual pressing (pellet dies. and anti-sticking agents. While the pressing of powders into disks for XRF analysis is. This is true whether the sample was pressed without binder in a Spec-Cap. often a mixture of thoroughly pulverized sample material and an appropriate binder. and PrepAid binders. then repeating at longer grind­ing times until the intensities reach a plateau. SPEX SamplePrep offers laboratory mills and grinding vials that are ideal for this pro­cedure. accessories. a fairly intricate exercise.spexsampleprep. The discussion assumes that the analyte has been properly sampled (so that it is representative) and adequately pulverized (to minimize particle size effects). presses. you need a sufficient quantity of homogeneous powder. A binder can be uniformly blended with the sample or used as a backing for a thin layer of sample. and uniform sample disks can be ensured by the use of reliable SPEX SamplePrep dies. including two pellets of polished steel or other hard. An alternate technique.

into the bore.spexsampleprep. which are primarily used to produce KBr disks for infrared spectrometry. delays. the pellet should drop smoothly to the bottom of the bore. several minutes may be appropriate. or sticks to the die or scratches it. and add the upper polished pellet. These include Spec-Caps. A good test is to assemble the die bore and base. due to compression of the air inside the die. holding it there for a certain length of time. careful bleed period can be difficult to accomplish with manual presses. it should be fairly easy to remove it from the die. When evacuating a die. the sample disk may have a raised. 35 mm or 40 mm dies during pressing. and chipped or broken sample disks. Care and Maintenance of the SPEX SamplePrep Evacuable Pellet Die The SPEX SamplePrep evacuable pellet die is a precision tool which must be handled carefully and diligently maintained for proper operation. and pore space.com The Use of the Vacuum in Pellet Pressing All SPEX SamplePrep evacuable pellet dies have a vacuum hose attachment. When the evacuation port is unsealed. the use of a vacuum is necessary to draw moisture out of the KBr.Pressing & Pelletizing Chapter 3 Section 2 Pressing & Pelletizing Section 2 Chapter 3 Technique for Pressing a Sample Disk In pressing samples for XRF. a matter of microns. Troublesome samples will often benefit from this technique. by pressing the analytical sample between two polished pellets of steel or tungsten carbide. Any SPEX SamplePrep pellet die will fit these presses. PrepAid binders. Some samples cohere adequately at low pressures. A holding time at maximum pressure of at least 30 seconds is recommended. Sleeve-and-Plunger sets. A basic pressing sequence consists of raising the pressure to a specific level. precise fit of the working parts is absolutely necessary. This may be due to elastic rebound of gases trapped in the sample. During holding time the pressure should be maintained as well as possible. For samples that do not bind well. Once the sample disk is pressed. depending on the size of the die and the nature of the sample. A slow. (When this happens. Polished pellets are made with close tolerances and sharp edges so that a sample powder will not “feather” into the gap between the pellet and the bore. In the case of 13 mm dies. Although in design and function such dies are very simple. In a pellet die in proper condition. If the polished pellet sinks immediately with the evacuation port sealed. but 31 mm and larger dies usually have load limits higher than either the capacity of the press or the pressure required to form a sample disk. but in fact the withdrawal of air and moisture from the sample can improve disk compaction and quality. The overall uniformity of the sample disks (and hence of the analytical results) will inevitably be greater. for a 35 mm disk. polished side down. compaction of the sample decreases pore space and increases analytical accuracy. and various anti-sticking agents. because a binder may take time to completely penetrate the sample. the loaded pellet die is placed in a hydraulic press. A pellet die in good condition will produce thousands of sample disks without difficulty. A gradual release of pressure after the hold period is perhaps even more important than prolonged holding time. analysts do not bother to evacuate their 31 mm. or the seal between the die body and base is damaged. It should remain at or near the top of the bore. crumbly lip and the disk and upper polished pellet may be difficult to remove from the die). so some care must be exercised. seal the evacuation port with a fingertip. either by hand or with the use of the knock-out ring supplied with each SPEX SamplePrep die. moisture. level it. When the sample does not hold together well after pressing. but their fit should be so precise that the pulverized sample will not “leak” around the pellet edges. insert the lower polished pellet. and then releasing it. pour the sample into the bore. and the 35-ton 3635 Automated X-Press. but uniform high pressure is recommended. sample after sample. The maximum pressure for a given task varies considerably. as they can be dented or chipped by dropping them even a short distance onto a hard surface. Typical pressures for a 31 mm disk are from 20 to 25 tons. Such dents are extremely dangerous to Order Online 24/7: www. Some analysts hold pressure for 5 minutes or more. but it is still never a good idea to dump pressure abruptly in any pelletizing procedure. as the pressure release control is often not sensitive. A minimum bleed time of 15 seconds is recommended. or for other reasons. Each has its proper application and technique. detailed later in this Chapter. If a sample is simply brought to maximum pressure. Obviously maximum pressures should not exceed the load limits of the die. and place a polished pellet (polished side up) in the bore. and for a 40 mm disk. Another significant advantage of the 3635 X-Press is that lengthy hold times and precisely controlled pressure release can be programmed in. the polished pellets should pass smoothly through the die bore without binding. it is either a loose fit. Most samples contain gases. and the pressure is raised to a level that will cause the sample or sample/binder mixture to cohere into a stable sample disk. and will remain the same. preferably slowly. An advantage of the 3635 Automated X-Press is that it turns on the pump if the pressure drops more than 1 ton during the holding period. Holding time and bleed time are both important.com 115 . and the pressure is abruptly released. there are various pelletizing aids available. polished side up.spexsampleprep. the sample disk often does not hold together. from 22 to 30 tons. Most XRF 114 Order Online 24/7: www. The simplest way of loading the die is to assemble the die barrel and die base. The edges of these pellets are by far the most vulnerable part of a die. and spring back when pushed down lightly. then insert the plunger. and removal or reduction of these can in fact affect the stability and uniformity of the sample disk. a damaged or heavily worn die is likely to produce frustration. from 25 to 35 tons. The 13 mm die has a 10-ton limit. Any damage to the polished pellets or the bore of a pellet die should be corrected immediately. which enables a vacuum pump to be hooked up to the die before and during a pressing operation. the 25-ton 3628 Air-Actuated Bench-Press. it is advisable to make sure both the upper and lower O-rings are in place and in good condition. and place the assembled die in the press. As “infinite depth” is very shallow for XRF analysis of most elements. Set-Up and Loading of the SPEX SamplePrep Evacuable Pellet Die Most evacuable pellet dies operate in the same way. This approach works well if the sample coheres well under pressure and is neither abrasive nor adhesive. Manual and motorized hydraulic presses are available for this task: SPEX SamplePrep offers 12-ton and 25-ton SPEX SamplePrep-Carver manual presses. and easily jeopardized.

spexsampleprep. perhaps the greatest is that unless the sample material is unusually dense or incompressible. A lightly scarred die bore. and 3617. The Spec-Cap also protects the bore of the die from abrasive samples. be kept in a desiccator if they are to be retained. properly smoothed. the top of the sample disk and the edge of the Spec-Cap will coincide. allowing the disk to be written on and handled without crumbling or contamination. Steel has a hardness similar to glass. Damage to the polished face of the pellet should also be avoided. It will neither stick to a die nor contaminate a sample. prone to cracking and possibly (in the case of low-Z elements) less than “infinitely thick. 3615. 30 mm. and the technique of assembling the die around a loaded Spec-Cap requires some finesse. but can also serve as a pellet matrix. for a 35 mm sample disk. The simpler is to fill the Spec-Cap with sample. use the same cleaning technique you would for a glass lens or mirror. paraffin. and always treat it as the precision tool it is. Generic binders include cellulose. can continue in use. supporting a thin layer of sample. and rotate it gently in the mouth of the bore to make sure it is properly lined up. and graphite. and the paint on the 116 Order Online 24/7: www. and when successful is quite efficient. makes 40 mm disks). scarring it deeply. If it does not. boric acid. and detector. as sample can wedge into the space left by the chip. 600 grit) emery paper. (A badly chipped pellet should be retired. PrepAid® Cellulose (3642) has a particle size of less than 20 microns. level it off. one with a pristine polished pellet and the other with the worn pellet. Not only can they cause the pellets to bind in the die. Of these. There are two types of Spec-Caps. the lower polished pellet inserted. and its leading edge is not significantly chipped. but also. in other words. and the most easily damaged. and blends quickly and completely with samples at 10% by weight. Here the Spec-Cap is flared before being placed in the die. Binders can be liquids or powders. A sample disk properly prepared with a Spec-Cap will be encased by the Spec-Cap on one side and around its edge. Binders Many analytical samples cohere well under pressure. Scratches on the order of 20–30 microns can cause shielding effects in the sample disk. but will probably not affect the functioning of the die. which with time can enlarge or damage the die. Minor damage to the polished pellets and die bore should be immediately corrected with a fine-grained (e. Binders are usually blended with the sample after pulverizing and before pressing. When a polished pellet is placed in the diebore. as with time they can absorb moisture and slowly swell and crack. the fit is so precise that a very slight tilt will cause them to stick. 38 mm. crumble-proof sample disk achieved with a minimum of dilution. A simple technique for inserting the polished pellet into the die bore is to hold the trailing edge of the pellet lightly with the finger-tips. treat them like glass. In addition. further chipping is likely to occur under pressure). When this happens. This approach allows many samples to be set up and marked in advance. Obviously if analytical results are being distorted because of the condition of the polished pellets. straight-walled Spec-Caps can be used in two ways. and overall abrasion of the polished pellet face can very slightly change the geometry and distance in the critical relationship between X-ray tube. During pressing. 5 to 8 grams. Alternatively. ideal for blending and pelletizing. as this can cause the pellet to chip. unpainted with flared walls (3619A. Obviously the sample weight will vary with the density of the sample and the size of the disk. Above all. take extra care that they do not jam. to avoid both sample cross-contamination and the possibility of disk jamming or sticking from sample build-up. and quite possibly ruin the die. those samples which crumble or ablate after pressing require a binder. but the general range of sample weight is.com Proper Use of the SPEX SamplePrep Spec-Cap Spec-Caps are shallow aluminum cups in which a sample is pressed. 3615. Disks stabilized with cellulose should. making it difficult to extract the pellet from the die. When the proper amount of sample is added. 3617. In cleaning the polished pellets. With this technique the die bore and base are assembled. makes 31 mm disks. Pellet dies should be cleaned after every use. UltraBind. Analytical accuracy is what suffers. cellulose and paraffin are available through SPEX SamplePrep in extra-pure. and compare the analytical data. contamination. A simple way to check polished pellets is to press two sample disks of identical material. the sample disk will be very thin. 8 to 12 grams. careful corrective action should be taken immediately. and assemble the die around the filled Spec-Cap. for a 40 mm disk.com 117 . 7 to 10 grams. satisfies our notions of the perfect all-around binder: Order Online 24/7: www.spexsampleprep. sample disk. and range from commonly available reagents to brand name products with secret formulas. but the degree to which such distortion is tolerable will vary considerably from user to user. it should move freely. The painted. makes 31 mm disks) and painted with straight walls (3619. the flared Spec-Cap technique may be used with either the painted Spec-Caps or the 3619A Pre-Flared Spec-Caps. but there are handicaps. with the upper polished pellet and the plunger following. and 3619 Spec-Caps acts as a lubricant. some simple rules should be kept in mind: keep the die clean. It can also be used undiluted as a sample matrix with the sleeve-and-plunger technique. making it easier to remove the sample disk from the die. and. and the flared Spec-Cap pushed down against that lower pellet. the stressed edge of the pellet can spall off. for a 31 mm disk. The resulting chip can be dragged through the bore. In handling the pellet die.” There is also a chance of the Spec-Cap wall crumpling inward. When inserting the polished pellets into the bore of the die. and does not cake in the bottle during storage. free the pellet gently. finely powdered form. do not push it down further and make the situation worse. makes 35 mm disks. and effort. 3619 and 3617 Spec-Caps are flared by the user with the 3618 Edge-Flaring Tool. it is time to replace them. 33 mm. and it is important to avoid scratching the polished surface. the pellet and die can continue in service. 3615 Spec-Caps are flared by the user with the 3625 Edge-Flaring Tool. and potentially jamming the plunger and ruining the die. Their use should lead to a stable. and the 3619A Spec-Cap is flared at the factory. an exclusive SPEX SamplePrep product. If after this the pellet will still pass smoothly through the die bore.Pressing & Pelletizing Chapter 3 Section 2 Pressing & Pelletizing Section 2 Chapter 3 the integrity of the die. Remember that the polished pellets are the most critical parts of the die. the sample powder is forced inside the Spec-Cap. however. Then the sample is poured into the die.g. under the high pressures of pelletizing.

The 31 mm sample disk accepted as the standard size by most XRF manufacturers and users was originated for the point-to-plane technique in arc/spark optical emission spectroscopy. As the die barrel moves down. and 40 mm dies. The classic example of this genre is aspirin. and the lower polished pellet placed in the bore of the die.com 119 . Order Online 24/7: www. binders can also be used in unblended form as a sample support. Ultrabind blends easily with samples to yield a disk which is easy to remove from the die. described in this chapter.com to attain very fine particle size. (Binders have a much lower specific gravity than most sample materials. Even though samples are typically blended with 10% binder by weight. In some cases this can be done by inverting the die and standing it on the plunger. Its disadvantage for XRF is that it must be used in a proportion of at least 50% of the sample disk by weight. and blends rapidly with any sample. Graphite powder makes sample disks unaffected by moisture. As with cellulose. Now the plunger is carefully withdrawn followed by the sleeve. The finished disk consists of solid binder with a uniform sample layer “bull’s-eye” in the target area of the disk. and is an excellent disk matrix when used with the Sleeve-and-Plunger technique. it is much more hygroscopic than cellulose and hence it typically supplied in granular form. it should be remarked that their most conspicuous property is that of caking under pressure. Sleeve-and-Plunger Technique: Binder as Sample Disk Matrix Besides being blended with a powdered sample. and moisture-resistant. and durable enough to withstand rough handling. Liquid binders are also used. Other advantages are that the disk is quite strong and stable without a Spec-Cap.spexsampleprep. easing the polished pellets and the sample disk out of the die without damaging them. or at least of flowing under pressure and then caking when the pressure is relieved. Sample disks pressed with graphite are also used for spark ablation techniques. This leaves a thin layer of formed sample in the die. all the sample particles receive a light coating of the polymer. and the plunger inserted in the sleeve to even out the sample powder and tamp it down. but that was because of its high conductivity. Generally these are in tablet form. the technique is successful with small quantities of sample. requiring grinding in a mill or mortar-and pestle to become a fine enough powder to blend evenly with a sample. and others. as the binder penetrates the pore space between particles rather than separating them. mechanical force can be applied to the die. The sample is also presented to the spectrometer in nearly undiluted form. Hence there is a good chance that adding a binder to the sample before grinding will lead to caking in the grinding container. Then the sleeve is inserted in the bore. so that a uniform amount can be easily added to the sample just before grinding. If hand pressure will not budge the plunger. The sample is poured onto that part of the polished pellet left exposed. Some analysts add boric acid to the sample during the final stage of grinding to achieve this. Boric acid is commonly available in pure form. beginning in Section 1. It also resists cracking and swelling in storage. When a grinding aid such as Vertrel® XF (3650) is used. the plunger pushes the polished pellets and sample disk up. A fine (20 µm) powder. so that subsequent pelletizing is more direct and efficient. diluting the sample and diminishing its XRF emissions). and the die taken out of the press.spexsampleprep. Of the use of binders in general. Solid binders also include powdered wax. the knock-out ring (supplied with each SPEX SamplePrep pellet die) should be used. Most batches. and can be used diluted or undiluted to make a stable sample disk. 35 mm. Most appear to be a solution of polymer(s) in solvent(s). and is self-lubricating. The knock-out ring is a tube which fits into the recess in the lower end of the die barrel. making it easy to free disks from the pellet die. and that grinding aids are often needed 118 Order Online 24/7: www. the disk may have a much higher proportion of binder by volume. but there are more sophisticated. proprietary grinding/binding tablets available. With the die base removed and the knock-out ring in place. this is the technique. UltraBind® (3644) is described on page 200 along with other PrepAid binders. they are blended with a sample prior to pressing. the binder can usually be added to the sample before grinding. Sample Disk Removal When the sample disk has been formed.g. However. Sample disks bonded with boric acid must be kept in a desiccator if they are to be preserved. Sample disks formed with 10% to 20% paraffin are air-stable. and are described. onto and around which the binder is poured. A typical XRF disk made with a SPEX SamplePrep Sleeve-and-Plunger Set consists of a thin layer of powder supported by a binder matrix. the fine (30 µm) powder blends evenly with samples and does not contaminate them. It also serves a its own lubricant. Graphite was used extensively in the development of sample-disk pressing techniques. However. pulverized acrylic plastic. however. as in this concentration it will stick to the die. followed by the die plunger. cement-mix ground to below 10 microns) is more likely to bind well under pressure than the same sample ground to moderate fineness. First the barrel and base are assembled. have low amounts of NaCl as a relic of the manufacturing process. Since most of the X-ray fluorescence emission measured by an XRF spectrometer comes from within a few microns of the surface. paraffin should not be used undiluted with the sleeve-and-plunger technique. Powdered Paraffin (3646) is also offered by SPEX SamplePrep.Pressing & Pelletizing Chapter 3 Section 2 Pressing & Pelletizing Section 2 Chapter 3 it blends well with samples. and will not scratch the bore of the die. Finally the upper polished pellet is inserted in the bore. as the waxy binder seals the surface against moisture. and the assembled die is transferred to the press and put through a pressing cycle. their reputed advantage is that during blending. and pressing down on the edge of the die barrel with the heels of the hands. is easy to remove from the die. When a SPEX SamplePrep Sleeve-and-Plunger Set is used to make XRF sample disks. removing the base. Sleeve-and-Plunger Sets are available for SPEX SamplePrep 31 mm. strong when palletized. often a gram or less. Chapter 5 of this Handbook. the disk must then be removed from the die. There are also materials which are touted as aids for both grinding and binding. In this connection it should be noted that a very finely ground sample (e. where a high-voltage current is passed through the sample.

the surface of the sample disk should be very flat and very clean. will still degrade in the spectrometer. Sample disks can also be degraded by X-rays. sweat.spexsampleprep. but releasing agents are not widely used because of concerns about sample contamination.com 121 . leaving a thin coating of fluoropolymer on the die bore. If it must be kept as a reference sample or standard. it will also contaminate the face of the sample disk with lubricant. (Flatness can be checked by holding a sample disk against a polished pellet). leaving the disk with an irregular and possibly non-representative sample surface. When the pressed sample disk has been removed from the die. (A more elegant approach is to cut circles of film the size of the die bore. After application. chips. it is advisable to have that standard made in duplicate. and should be easy to remove from the die. and swell. after the use of binders and the most careful pressing procedures. Physical damage to the disk surface also affects accuracy: scratches.Pressing & Pelletizing Chapter 3 Section 2 Pressing & Pelletizing Section 2 Chapter 3 Whether the sample disk is extracted by hand. Most pressed powders will absorb moisture with time. This may be due to the pellet being damaged or poorly cleaned. If a pressed sample disk is to be used as a standard. Anti-Sticking Agents In commercial molding operations. and the sample disk is carefully handled during and after removal from the die. 120 Order Online 24/7: www. The most common remedy is to place a piece of XRF window film (e. When the die is then loaded and the sample pressed. detailed below. Even the heat produced by the X-ray beam can cause small flakes or particles to break loose from the face of the disk. and incidental contaminants are easily transferred to the analytical surface of the sample disk. The use of the press together with the die’s knock-out ring is common practice. and contaminating the spectrometer. pits. it should be preserved in a desiccator. it is best to analyze a sample disk as soon as possible after it is pressed. This is the case with XRF sample disk preparation. Often the first symptom of sample disk degradation is a decline in analytical accuracy. with the spare disk carefully preserved. skin oils. However. the sample disk and the polished pellets should have lubricant only along their edges. one ingenious solution has been to place a pressed 31 mm sample disk inside a SPEX SamplePrep 3527 40 mm X-Cell. releasing agents are often necessary to effect the easy removal of the product from the mold. for additional information. and the upper polished pellet pushed down on top of it. Every XRF analyst knows the anguish of having a sample disk emerge from the die firmly attached to the polished pellet.com Order Online 24/7: www. metals. SPEX SamplePrep 3516 Mylar window film is recommended because of its 0. the use of a lubricant in the bore of the die does not have to contaminate the face of the sample if that lubricant is carefully applied. at best the disk is ruined. SPEX SamplePrep 4 micron Ultralene) where it will protect the spectrometer. or with the press and knockout ring. there is a fluoropolymer spray which can be squirted into the bore of a die before the die is loaded. There can be sample disks which.12 mil thinness. It follows that these disks should be handled carefully. Consult the Anti-Sticking Agents section. As a general rule. and as long as the disk does not bind to the die bore or the polished pellets. the knock-out ring approach works well enough. the die barrel and plunger should be kept in an inverted position to minimize the risk of damaging the sample disk during extraction. a piece of film can be placed over the bore. While spraying the polished pellet with lubricant will prevent sample adhesion. The standard in daily use should be periodically compared with the standard kept in reserve. Sample Disk Handling and Care For maximum precision in XRF analysis. whether of plastics. any such lubricant should be thoroughly tested before it is incorporated in a pressing pro­cedure. but it is more likely that the sample is at fault. the volatile carrier evaporates. For example. and preferably not with bare skin. After the sample powder is added to the die and leveled. to avoid both surface contamination and damage. and in general it is difficult to remove a pressed sample disk from a die by hand pressure alone. the film is peeled off and discarded). or other materials. and swelling or curving should all be watched for and guarded against.g. Sample disks should be handled only by their edges.spexsampleprep. Even samples which are not inherently sticky can become somewhat adhesive when forced against a steel plate by 25 tons of ram pressure. Even so. Some samples exhibit a kind of elastic rebound shortly after pressing. The use of lubricants in the die usually makes it possible to extract the sample disk by hand. The simplest non contaminating approach is to place a piece of thin plastic film between the polished pellet and the sample before pressing. as well as minimizing the chances of the sample disk jamming or sticking in the die bore.

maintain or repair as necessary. If the sample disk sticks to the polished pellet. before pressing. • use polished tungsten carbide pellets. .com 123 . . or allow the edges to become dented. Each SPEX SamplePrep die set is a complete unit. . and/or bleed time . . If the polished pellets become chipped or jammed. A convenient “knock-out ring” allows easy extraction of the steel pellets and sample disk from the die. • STOP IMMEDIATELY. Never tilt the pellets so that they become jammed when being placed in the die. . If the sample disk is hard to remove from the die. use a binder. (If they become jammed. . The following pointers are essentially an index to this section of the Handbook. grind the sample finer. . However.com Order Online 24/7: www. it is flying in the face of experience to assume that nothing can go wrong.g.spexsampleprep. protect the spectrometer with SPEX SamplePrep XRF Window Film. • grind the sample finer. check that the bore of the die and the polished pellets are clean and undamaged. free them as gently as possible). and two polished steel pellets. . volatiles. Each precision-machined SPEX SamplePrep die set also incorporates a vacuum hose attachment. To prevent further damage. 31 mm for most OES and XRF instruments. etc. e. Always put the squared-off end of the plunger into the die. . and take corrective action to avoid making matters worse. 122 Order Online 24/7: www. Selecting a Pellet Die The choice of die is generally determined by the requirements of the analytical instrument. a plunger. This allows evacuation of gases. if the stepped/beveled end of the plunger contacts a polished pellet under pressure. evacuate the die during pressing. between the sample and the polished pellet. store the sample disk in a desiccator if it is to be retained. If the polished steel pellets become scratched in normal usage. and moisture during pressing. polypropylene. . prepare disks with a binder matrix. Never drop the pellets. indexed by problem: If the sample disk comes out of the die smoothly.spexsampleprep. . SPEX SamplePrep offers dies to make four standard sizes of sample disks: 13 mm for IR spectrometers. use a lubricant. • • • • use Spec-Caps. always remember. the pellet can chip. If sample disks degrade rapidly in use. assisting compaction and preventing possible sample disk rupture under vacuum-path conditions. Made of hardened stainless steel for durability and extra wear. . but breaks. the SPEX SamplePrep die includes a body with detachable base. evacuate the die during pressing. • put a thin sheet of SPEX SamplePrep Mylar. hold time. use Spec-Caps. SPEX SamplePrep 3623C. Sample material is pressed in the die bore between the polished pellets. • • • • • increase pressure. . • • • • use a binder. Dies are clearly labeled with bore size and maximum safe load. yielding a compact sample disk ready for the spectrometer’s sample holder. . and 35 mm and 40 mm for newer XRF spectrometers.Pressing & Pelletizing Chapter 3 Section 2 Pressing & Pelletizing Section 2 Chapter 3 Trouble Shooting A carefully conceived and implemented disk pressing procedure should give the analyst few difficulties.

sand and ore but such samples are subject to segregation during grinding and pressing. the sample when fused must be in the form of an oxidized. it has proven to be the best method for materials that have these characteristics when X-ray fluorescence analysis is the method of choice. The coal sample must be ashed and the ash is then fused. cement). and ICP. and other liquid-analyzing techniques. However. Reduced metals must also be oxidized. Recent advances also allow borate fusion of samples containing sulfides. Extra steps necessary to prepare organic materials and reduced inorganics for fusion can extend turnaround time but still may be the most accurate method to choose.g. so structural and molecular information should be measured before the fusion is made. There have been recent advances in improving the performance of fusions for trace analysis. The samples are mixed in powdered form with a flux. SPEX SamplePrep has a full range of equipment for either approach. Because fusion eliminates particle size and mineralogical effects and produces a homogeneous sample. quickest. zirconia and alumina). building materials and mining concentrates. SPEX SamplePrep also provides the full line of SPEX Fusion Flux. or both (e. carbides. 124 Order Online 24/7: www. inorganic compound. since the sample is diluted during fusion. etc. hybrid oxidation/fusion techniques have been developed for reliable borate fusions of sulfides. and graphite crucibles for smaller-scale operations with muffle furnaces. either lithium tetraborate or a mixture of lithium tetraborate and lithium metaborate. and the use of dilute HCl or HNO3 to dissolve the melt. and slags from smelters. The sulfur in the coal will volatilize in the process and therefore sulfur cannot be measured). sand. Borate fusion has become increasingly popular as a preparation technique for XRF sample disks. The pressed powder method can be highly accurate when carefully done with multi-phase samples such as cements. each with their own advantages. and the use of hazardous acids (e. and to matrix effects (e. While borate fusions do require some caution in evacuating heat and fumes.g. the more consistent the particle size. Most of these samples are naturally oxygen–rich and do not require chemical transformation prior to borate fusions. Borate glass disks are easier to preserve than pressed powder disks because they are stable if carefully stored in desiccators. Compounds without oxygen such as sulfides. typically ten to fifteen minutes to make glass disks or solutions with automated fluxers. ICP. the major advantage of borate fusion is that it is often simpler and quicker than dissolution with acid in a microwave pressure vessel. etc. or quickly dissolved in dilute nitric acid or hydrochloric acid for analysis in solution by AA or ICP. the melt can be cast as a glass disk or poured into a dilute acid solution and dissolved. reproducible fusions. rock. Cement is usually a blend of carbonates and silicates. as borate glass is essentially a solid solution with few matrix-matching problems. chlorides.spexsampleprep. Synthetic standards for XRF can also be made from pure oxides with the borate fusion method.g. Please consult our applications specialists to help determine which method is more suitable for your laboratory. refractories. glass.g. The fusion method will reduce matrix effects but not eliminate them. metal ores and silicate rocks). carbides and some ferro-alloy materials formerly considered out-of-bounds for the technique. can take fifteen minutes or less in an automated fluxer. Organic compounds must be ashed. and so forth. When to Employ Borate Fusion Borate fusions are widely used for samples which are either difficult to prepare as homogenous pressed powder (e. hard to dissolve in acid (e. but also their industrial products and by-products such as cement. The Katanax K1 and K2 Prime Series Automated Electric Fluxers for rapid. The sample forms borate salts and this eliminates particle size and mineralogical effects. Once fusion is complete. from ignition of the heating elements to decanting of a clear solution. One of the advantages of borate fusion is the short preparation time. Fusion destroys the original form of the sample. The sample mixture is heated until the flux melts and the sample dissolves in it. mining and minerals. yielding a homogenous melt.spexsampleprep. Additional industrial samples include pigments such as TiO2. The melt can be cast as a glass disk for XRF. ceramics. ferroalloys. AA. A complete fusion/solution procedure.com Order Online 24/7: www. while other compounds form during fusion. the more reproducible and accurate the fusion will be. The high temperature of borate fusion (1000˚ to 1150˚ C) drives off compounds of volatile metals such as Hg. refineries and glass plants. Sn. Platinum-group metals cannot be fused with borates because these compounds reduce during fusion and the metals will not only remain insoluble in the flux but can also alloy with the 95% platinum/5% gold crucibles and damage or destroy them. HF) is avoided. Samples analyzed include not only raw materials like dolomite. For samples prepared as liquids.com 125 .g. borate fusion can be quicker overall than microwave dissolution in pressure vessels. Borate fusion methods offer a wide range of applications but may not be suitable for all materials. SPEX SamplePrep offers two approaches to borate fusion. For borate fusions to be successful. and Sb. The sample must be ground to a fine powder before the fusion. rock. (An example of this is the analysis of metallurgical coal. The use of borate fusions will also minimize matrix effects which are seen in XRF analysis. zirconia and alumina are oxides. Many users of the K1 and K2 Prime Series Automated Electric Fluxers are in the following industries: cement. and similar materials for elemental analysis by XRF. and most accurate analytical approach. must be oxidized before being fused. For many samples borate fusion is the simplest.Fusion Chapter 4 Section 2 Fusion Section 2 Chapter 4 Introduction Borate fusion is an extremely effective method of preparing cement. In preparing samples for AA. ceramics. Both fusion and pulverizing/pressing are important and widely used sample preparation methods. basalt and iron ore. blast furnaces. particle size and mineralogical effects). Borate fusion may not be the method of choice if the analyst is interested in trace analysis. hazardous reagents such as HF and other concentrated mineral acids are not necessary.

when programmed for similar samples can produce up to 25 fused disks per hour. First the sample is mixed with a flux in an appropriate ratio (usually between 1:2 and 1:10). e. and potassium pyrosulfate (K2S2O7).6 grams of cement mixed with 6 grams of flux and about half a percent of LiBr. carbonates.P. whereas a molten flux bead with excessive NWA will ball up when poured and not form a complete disk. 10% HNO3) and stirred until the glass flux dissolves. using 0. but is available for those who find its physical characteristics superior for their application. etc. lithium metaborate. Lithium metaborate or “met/tet” mixtures are more suitable for acidic oxides such as silicate rocks and silica-alumina refractories. The same borate fusion procedures can be carried out manually in a muffle furnace with SPEX SamplePrep graphite crucibles. and will often attack platinum-gold crucibles. The sample is mixed with lithium or sodium nitrate and preheated to oxidize the sulfide to sulfate. 920˚ C). Most borate fusions are performed in crucibles made of 95% platinum and 5% gold. The latter is fine-grained and less dense than the “glass bead” fluxes. Each approach has its advantages. The larger flat-bottomed SPEX SamplePrep crucibles can be used to cast glass disks as well as perform fusions. SPEX SamplePrep guarantees both the purity and the quality of the fluxes and additives supplied to our customers. Additives for Fusions: Non-Wetting Agents. 845˚ C). M. Some borate fusions are done in graphite crucibles. carbides. many of these materials can be first oxidized with standard techniques and then successfully fused. or alloy with them. silicates. LiBr solution is available separately for quick addition of a non-wetting agent to a flux.g. The visible effect of a non-wetting agent is to increase the surface tension of the melt. The most popular blended flux. and the crucible and the glass together are placed in an acid solution to dissolve the glass. and is preferred for cement and most ores. Fluidizers. Melting point may be a factor in the selection of a flux. sodium metaphosphate (NaPO3). How to Select a Fusion Flux Most fusions involve the use of lithium tetraborate (Li2B4O7. It is possible to achieve great sample throughput with an automated. The sample is heated past the melting point of the flux in an inert. which greatly increase the “stickiness” of a melt. heat-resistant crucible. 126 Order Online 24/7: www. pre-fused and coarse-grained for maximum homogeneity and ease of use.com Order Online 24/7: www.g. 2:1 “tet:met. Alternative fluxes and fluxing techniques are discussed in Bock (1979) and in Sulcek and Povondra (1989). These have lower melting points than lithium borate fluxes and more specialized applications. heating is maintained and the crucible regularly agitated until the sample has completely dissolved in the molten flux. or poured into dilute mineral acid (e. sodium tetraborate. and 1 to 2 grams for a solution.com 127 . However the utility of lithium tetraborate and lithium tetraborate/metaborate mixtures is so great that most analytical fusions are carried out with these fluxes at temperatures between 1000˚ and 1150˚ C. require additional NWA. when programmed for cement samples. Many of these fluxes are available in pure and ultra-pure grades.” is also available with added LiBr non-wetting agent for greater convenience. the greater the degree of volatilization. somewhat longer fusions (as for some technical ceramics) may also need greater amounts of NWA. 12 mg of NWA for 6 grams of flux. these lithium borates will dissolve oxides. Other fluxes include sodium tetraborate (Na2B4O7). a non-wetting agent. a standard non-wetting alloy. A fused disk with too little NWA will have a concave upper surface and may be difficult to remove from the mold. programmable fluxer. while the crucibles are handled and agitated with SPEX SamplePrep tongs. As a rule lithium tetraborate is better suited for the dissolution of basic oxides. cannot be fused directly in lithium borate fluxes. When glass disks for XRF are being made. with the addition of a non-wetting agent to prevent the flux from sticking to the crucible and the mold. Individually or together. lithium metaborate (LiBO4. At this point the melt is either poured into a mold and annealed to form a glass disk for XRF. Most SPEX Fusion Flux are of the “glass bead” type. both cited in the bibliography at the back of this Handbook. All fusion fluxes sold by SPEX SamplePrep are manufactured to the highest standards available.P. All are supplied with a certificate of analysis for trace metal impurities. or a mixture of the two. The ideal amount of NWA for a specific procedure is usually determined by experiment.spexsampleprep. nitrates. please contact our applications specialists to determine the optimum equipment for your requirements. However. This includes lithium tetraborate. The 5-position Katanax K2 Prime. and minimum absorption of moisture.2% of the weight of the flux. Metals. and a lithium tetraborate/lithium carbonate mixture. can produce up to seven fused glass disks in an hour. M. The exceptions are the lithium borate/carbonate flux (a physical mixture) and so-called “fluffy” lithium tetraborate. Certain samples such as iron ores. When this has been done the fusion can proceed as normal without any loss of sulfur from the fusion. several lithium tetraborate/metaborate blends. Again. The time per sample with the muffle furnaces is usually much longer than with an automated fluxer. The Katanax K1 Prime. As non-wetting agents gradually volatize during a fusion. Methods have been developed for fusing sulfide-rich material such as copper ore. sulfates. During the fusion. as the higher temperature of a fusion.spexsampleprep. a non-wetting agent is mixed with the flux and the sample before fusion starts. etc. sulfides. Typical amounts of flux/sample mixture are 6 to 7 grams for a 31 mm glass disk. SPEX SamplePrep offers the full line of SPEX Fusion Flux. In some cases (notably pyrosulfate fusions) the melt is left to harden in the crucible. phosphides. and Oxidizers Non-wetting agents (NWA) are iodides and bromides which can be added in small quantities to a fusion so the molten flux will not stick to the crucible or mold.Fusion Chapter 4 Section 2 Fusion Section 2 Chapter 4 How to Prepare a Fused Sample Fusions are accomplished in several steps. Typically the amount of NWA is about 0.

and Cu. Graphite. A quantity of flux plus sample not exceeding 2 grams might require 50 to 100 mg of NWA. and 40 mm. is relatively harmless but can leave a black film on a glass disk or even cause it to crack. or for fusions where the sample might be reduced. it is desired to have complete transfer from the crucible to the beaker. lowering the melting point of a flux and making it flow far more easily. sodium iodide. (7155 is the high-purity version of the 7156). Other sample components such as phosphides and sulfides may be corrosive enough to damage or wreck a crucible in a single fusion.) used to contain samples during fusions. the graphite converting to CO2. Oxidizers such as lithium nitrate and sodium nitrate can be useful in eliminating unoxidized components from a sample that will not fuse. Graphite can be oxidized to CO2. SPEX SamplePrep 7152 is the standard 9 mL fusion crucible found in most laboratories. This can require a much higher proportion of nonwetting agent than is necessary to pour a glass disk. for trace-level analytical work. SPEX SamplePrep also offers a complete line of borate fusion fluxes and non-wetting agents. Fe. While graphite is an ideal crucible material for many applications. contamination of the sample is minimal. However lithium bromide is hydroscopic. SPEX SamplePrep 7156 is a standard graphite crucible with about three times the capacity of the 7152. The crucible bottoms are flat but not polished. SPEX SamplePrep flat-bottomed graphite crucibles (7157– 7162) are designed both as fusion crucibles and as molds for XRF cast glass disks. eliminating both the need for time consuming cleaning procedures and the possibility of cross-sample contamination. so it is usually made into a saturated solution and added to the flux from a dropper bottle. Si. and 40 mm) produce disks which will fit the standard XRF masks of 31 mm. zirconium. and easier to use as solids. Note that non-wetting agents should be used with care when copper-bearing samples are being fused. good for most fusions. SPEX SamplePrep regular-purity graphite typically has from 10 to 100 ppm each of Mg. At 10% by weight. it lowers a flux’s melting point by about 100˚ C. As oxidizers have much lower melting points then borate fluxes. over a period of hours some erosion of the crucible can occur. SPEX SamplePrep graphite crucibles are disposable.Fusion Chapter 4 Section 2 Fusion Section 2 Chapter 4 When making solutions by pouring the molten flux into a dilute mineral acid. 128 Order Online 24/7: www. Lithium iodide. fusion of the sample and annealing of the disks can be completed in the same container. and cesium iodide are somewhat more air-stable. liquid NWA cannot be added to a hot crucible while a fusion is in progress.spexsampleprep. 35 mm. Graphite Crucibles and Handling Equipment SPEX SamplePrep graphite crucibles are a cost-effective alternative to the metal crucibles (platinum/ gold. graphite will not combine with samples during fusion. it does oxidize slowly above 430° C. These crucibles have tapered walls to facilitate removal of the glass disk. so that for greatest analytical accuracy the disks should be flat-lapped. For fusions where the 7152 is too small. If they are oxidized to phosphates and sulfates they will be comparatively harmless. and their cations will be present in the fused glass disk for analysis. SPEX SamplePrep high-purity graphite has total metallic impurity (TMI) limits of 10 ppm. Chemically inert and heat-resistant. any fusion including them should proceed at a low temperature until oxidation is complete. SPEX SamplePrep graphite crucibles are available in two purities: high-purity. the same crucible in purified graphite.com Order Online 24/7: www. etc. While it is simpler to add a drop or two of NWA than it is to weigh out 10 or 20 mg of a solid. 33.6 mm. Lithium iodide and bromide are popular non-wetting agents because they do not add an impurity to the flux. And SPEX SamplePrep’s unique nickel-chromium rack and tongs make handling easy. often present in cement mix. The three different crucible sizes (31 mm. Lithium fluoride can be used as a fluidizer. graphite is not recommended for extremely lengthy fusions. measured by DC arc spectrometry. long-time users should note the introduction of the 7152HP. as copper halides are extremely volatile. as these impurities are distributed throughout the graphite.spexsampleprep. and economical regular-purity.com 129 . Because of this. withstanding temperatures well in excess of any required for even the most difficult borate fusions. Al.

Then the homogenized material can be dissolved for analysis as a liquid sample. The 3527 40 mm X-Cell can also be used to hold crumbling 31 mm sample disks. the snap-post on the rear can be pushed to break the seal and to permit venting of trapped bubbles or expanded liquid while the sample is run. then the 3577 Micro X-Cell is the solution to your problems. uniform sample disks. dabbed. A roughened surface within the reservoir cup facilitates labeling. Collimate your beam down to reduce scatter and you’re ready to go. dependable. 3619 and 3619A Spec-Caps are ideal. if homogeneous. tar. The requirements of the application will dictate the type of X-Cell and which window material to use. automated borate fusions.com 131 . marked and stored than unclad disks. flat disk. After window film has been attached to one end of the cell. For solution residues. SPEX SamplePrep also provides an extensive line of sample preparation equipment particularly suited for XRF spectroscopy. the disks are resistant to chipping and breaking and are more easily handled. These and the related products listed here will save you time and money. The 3571 X-Cell has a body open at both ends. and forms an inverted-cone shelf under which air bubbles can be trapped once the cell is filled and sealed. ICP. or protected but allowed to “breathe” with a piece of 3524 Microporous Film. Several spectrometer manufacturers have shifted toward 35 mm and 40 mm sample disks. reproducible running of liquid samples in XRF spectrometers. polyethylene. Millions more liquid XRF samples have been run in SPEX SamplePrep X-Cells. The cell is turned over and. respectively. poured. as well as dies and presses capable of compressing those powders into flat. SPEX SamplePrep also supplies versatile Double Open End X-Cells which are ideal for many unusual or hard-to-handle samples: slurries.5 mL fills it up. directly against the window. These products are described elsewhere in this handbook. or cast as a glasslike solid. X-Cells can also be used to run solution residues and small quantities of pastes or powders. For special applications there are 31 mm Double Open End and Micro X-Cells. so any bubbles rise to the back of the cell and do not interfere with the analysis. Bruker. In many XRF systems. The top of the 3571 X-Cell can then be left open. or planchet). Bubble-Free Cell Insert The Bubble-Free Cell Insert is a simple. then the snap-ring is pushed down over the cup to form a flat drum-like window. The sample holders of most X-ray spectrometers will accept 31 mm (11/4 in. and a collar to hold film in place while the ring is being applied. please feel free to consult our sample preparation specialists to determine the optimum equipment and techniques for your application. The Spec-Cap forms the bottom and partial sides of the completed sample disk (also called pellet. pressed into pellet form. They are designed to fit into the major suppliers of XRF spectrometers such as PANalytical. Each closed X-Cell consists of a cup and snap-on ring. can be machined to the proper shape and run directly. A drop of solution placed there and warmed under an IR lamp dries to a smudge for in situ analysis. The drawback of this “inverted optics” configuration Order Online 24/7: www.com X-Cells for XRF Liquid Samples SPEX SamplePrep X-Cells are used throughout the world for fast.spexsampleprep. thin-walled aluminum cups which are routinely used in the production of pressed-powder sample disks for XRF. The Micro X-Cell can be run with an open or window back. Thus reinforced. and fusion additives such as non-wetting agents and oxidants. and for these larger sizes we recommend 3615 and 3617 Spec-Caps. metal films and machine parts. Many solid samples. Liquid samples. Rigaku. if desired. viscous materials such as glue. etc. What they have in common is that they must all be presented to the XRF spectrometer in the form of a homogeneous. There are laboratory mills and grinding containers capable of converting most solid samples into homogeneous powders. two snap-on rings. The 3527I Bubble-Free Cell Insert is pushed into a cell before the sample is added. Others. are too inhomogeneous and must be pulverized or fused. and assure you of reproducible. yet guards against spillage in inverted-optic spectrometers. ores.3 mm in diameter. If you deal with small air-sensitive or hazardous samples. This assures the analyst of a smooth. contamination-free results. The filled X-Cell is then positioned in the spectrometer mask. or otherwise located in the cell. closed X-Cells are avail­able in both 31 mm and 40 mm sizes to fit most spectrometers. the cup is filled with liquid. purging. a piece of film is spread over the top. and biological materials. it can be inverted. and the sample placed. from water to oil. millions of powder samples for XRF have been pressed and protected in SPEX SamplePrep Spec-Caps. The patented closed X-Cell design features a snap-open seal for vent­ing volatile samples and a reservoir cup for catching any liquids that expand through the vent. yielding XRF glass disks. liquid cells are run in an inverted position. or solutions for AA. then dished slightly with the rounded end of a glass rod. sealed with film. pastes. and Thermo Instruments. are run in sample cells covered with a thin film.) sample disks.spexsampleprep. ready for XRF analysis. SPEX SamplePrep manufactures disposable sample-handling accessories for powder and liquid XRF samples.XRF Accessories Chapter 5 Section 2 XRF Accessories Section 2 Chapter 5 Introduction The XRF spectroscopist is confronted with an almost infinite variety of samples. etc. briquette. For further fusion work there are also full lines of graphite crucibles. the window is 6. and only 0. If powder or paste is spread on the surface and another piece of film overlaid before snapping on the ring. Over the last twenty years. Reinforcing XRF Pellets with Spec-Caps SPEX SamplePrep Spec-Caps are shallow. or the isolation of special samples. such as refractories. flat window for improved precision. Made of contaminant-free 130 Order Online 24/7: www. borate fusion fluxes. but it will also accept a 7 x 13 mm serum bottle closure for injection. the sandwiched sample is ready for X-ray analysis. and a 43 mm Closed Cell for Horiba Sulfur Analyzers. the film window is prepared as for solutions. While it fits in the standard 31 mm sample holder. or RTV sealant. For routine liquid samples. sludges. There are also the Katanax K1 and K2 Prime Automated Electric Fluxers for rapid. patented insert for the 40mm XRF liquid cell (3527) which prevents trapped air from forming a bubble under the window film when the cell is used in the upright position. For these instruments.

Inc. some samples outgas when heated by the X-ray beam. 8 µm Kapton is the least transparent to X-rays. and purity. polyethylene begins softening at temperatures well below 100°C.com 133 . Mylar is vulnerable to strong acids and strong bases and resistant to organic chemicals. Whenever there is a question about whether a SPEX SamplePrep X-Cell. The remaining films (5 µm Polypropylene. Kapton is clean in most respects but now includes a phosphate-based surface coating to improve its handling characteristics. Some samples simply attack some films. but is essentially impervious to chemical attack. Kapton is highly resistant to acids and organic chemicals and almost everything except strong bases. Bubbles trapped during assembly of the cell can collect against the window. Zn. or will it heat up during analysis and perhaps soften the film? Will it release volatiles and put pressure on the film from inside the cell? Often the final choice of film balances several requirements. Window films. Cu. Our cleanest film overall is Ultralene. Tests have shown that a pinhole near the edge of the window film will allow such gases to escape without bulging or rupturing the film. When choosing a thin film window for your application. 132 Order Online 24/7: www. and tap it. consider the following film characteristics: 1. Your choice of a window film depends on your analytical priorities and the nature of the sample. so if you are working with hot samples. Zn. Is strength more important than X-ray transmission. Transmission: X-ray transmission through polymer films is affected by the thickness of the film as well as its composition. and should be considered for lightelement analysis in particular. bases. Zr. We recommend comparing films. it may contain trace levels (ppm) of Ca. All SPEX SamplePrep XRF window films except Kapton are weakened by heating much above 100° C. heat-resistant to over 300° C. Any bubbles should rise through the hole in the insert. Most but not all bubbles get into an X-Cell during assembly. SPEX SamplePrep films are selected for uniform thickness so your results are reproducible. 2. Ti. To use an X-Cell fitted with a SPEX SamplePrep Bubble-Free Cell Insert.spexsampleprep. the films offered by SPEX SamplePrep have been selected for their strength and durability. While SPEX SamplePrep accepts no responsibility for damage resulting from window leakage. All of these films are attacked by strong oxidizing agents. However. Microporous Teflon is not used as a window film as such. away from the window film. or otherwise cause the X-Cell to leak or come apart. The film must effectively contain the liquid while allowing uniform transmission of the X-rays to the sample. and most organic chemicals except halogenated hydrocarbons. 5. and Shimadzu Scientific Instruments.com Selecting Thin Film Windows for XRF An X-Cell liquid sample cell must be covered by a thin film which serves as the sample window. P. or combination Order Online 24/7: www. It is much stronger than any other SPEX SamplePrep film. and can stretch a film to bursting or (rarely) cause slow leakage by migrating through the joint between the film and the cell. Fe. capable of weakening or penetrating certain films? Is it hot when you pour it into the X-Cell. Chemical Attack: Your sample’s chemical characteristics may dictate your choice of window film.spexsampleprep. Six micron (6 µm) Mylar is also unusually strong for its thickness. Thus you will get uneven fluorescent intensity with an uneven film. an increasing number of samples are being run in so-called “normal optics” XRF spectrometers. You are welcome to call us for further information at 1-800-LAB-SPEX x465. strength. but differ in other key properties. you test them together outside the spectrometer. CAUTION: SPEX SamplePrep window films and X-Cells are not intended to be used in vacuum-path XRF systems. as is 5 µm polypropylene. Uniform Thickness: The absorption of X-rays at a given wavelength is directly proportional to the thickness of the film. window film. bases. 6 µm Mylar is more transparent.XRF Accessories Chapter 5 Section 2 XRF Accessories Section 2 Chapter 5 is that if the window film ruptures. but they are not meant to replace actual testing. being much thinner than X-Cell bodies. The thinnest films (4 µm Ultralene. X-Cells are made of polyethylene. displacing the sample and attenuating the X-rays reaching the sample and emitted by it. 4. Kapton is the closest thing to a bombproof XRF window film. and 3 µm Mylar) have the greatest degree of X-ray transmission. The tables which follow may be of some help in selection. Our best advice is that you run a blank from every new roll or box you open since impurities can be different not only between types of film but also between different lots of the same material. Rigaku/USA. Strength: Leakage or rupture of the window during a run could cause damage to spectrometers with inverted optics. the sample can spill and potentially contaminate or damage the spectrometer. which is generally resistant to acids. 4 µm Ultralene. Fe. For each new sample. or vice versa? Are there certain impurities you cannot tolerate in the film? Is the sample chemically aggressive. where the X-ray source is above the cell instead of underneath. SPEX SamplePrep cannot be held responsible for variation in film composition. assemble the cell. Purity: No XRF window film is absolutely free of metallic impurities. While Mylar film makes a suitable window for most analyses. exposing the spectrometer to possible damage if the window leaks. P. or Sb. and Al. Of the SPEX SamplePrep XRF window films. Inc. and chemically impervious to almost everything except strong alkali solutions. It should also be noted that some volatile chemicals have the ability to generate pressure inside an X-Cell. Cu. We also suggest strongly that if there is any question about the compatibility of a sample with certain films and/or X-Cells. In general. pre-test the X-Cell body as well as the window film. and 3 µm Mylar ) have roughly comparable mechanical strengths.The 3527I Bubble-Free Cell Insert coupled with the 3527 X-Cell will fit normal optics XRF spectrometers made by Diano. but some are cleaner than others. invert it. with samples of the films and X-Cells we supply. Ultralene remains our best film in its balance of X-ray transmission. are likely to perforate long before the X-Cell is affected. and when the cell is turned right-side-up the bubbles will be trapped below the insert’s shelf. chemical resistivity. and for that purpose we offer the SPEX-Pack. However. and many organic chemicals. Polypropylene and Ultralene are reasonably resistant to acids. we strongly recommend that you test the window film by exposure to the sample for several times your longest anticipated running time. Polypropylene film has been known to contain trace levels of Ca. 3. An abrupt pressure change in an XRF spectrometer’s sample chamber can stretch or burst window film. but can be attacked by aromatic and halogenated hydrocarbons.

365 days.l.. You are welcome to discuss any such problem with our applications specialists by calling (732) 623-0465. 100°C 14 days. 5 days. 190 days.spexsampleprep. 100°C 14 days. 150°C 14 days. 134 Order Online 24/7: www. Chemical Resistance of Kapton® Substance Acetic Acid.9 pH = 10. du Pont de Nemours & Co.T. 100°C 166 days. R.T. R. Kapton. 365 days.T.2 pH = 7. 100°C Thin Film Transmission Characteristics Reprinted by permission of E. 10% Toluene Transformer Oil Water: pH = 1 pH = 4. Summary of Properties E-50533.com 135 . 100°C 4 days. 200°C 365 days. R. 22 days. 365 days.0 pH = 8.com Order Online 24/7: www. 365 days. R. 180 days. R.T.T. Glacial Acetone Benzene Chlorofrom p-Cresol Hexane Jet Fuel Methanol Sodium Hydroxide.spexsampleprep. R.T.T. 110°C 365 days. R.XRF Accessories Chapter 5 Section 2 XRF Accessories Section 2 Chapter 5 thereof is likely to perform properly in a particular analytical situation.T. R.0 Percent Retained (typical) Tensile Strength Elongation Tensile Modulus 85 67 100 93 100 97 86 100 - 94 100 65 65 65 65 60 62 62 82 74 77 89 92 73 Degrades 66 100 30 30 20 20 10 102 160 100 96 102 100 84 140 97 100 100 100 100 100 100 Conditions 36 days. the analyst should first test these products in a way which does not risk contaminating the spectrometer.

75°C 100 100 Dimethyl Formamide 100 100 Sodium Sulfide. 40% 75 50 Sulfuric Acid. vis. (immersion) 96 67 Silicone. 20% Carbon Disulfide Carbon Tetrachloride Chlorine Gas Chlorobenzene Chloroform Chromic Acid.E B B A A C B B C D C C A.E B B C A B A A B 137 Acids Glcial Acetic Acid 24 hours. 10% Amyl Acetate Amyl Alcohol Amyl Chloride Aniline Aqua Regia Aviation Fuel Benzene Benzyl Alcohol Brine Bromine.4) 24 hours. 10% 80 50 Nitric Acid.l. 2% 90 65 Sodium Hydroxide. du Pont de Nemours & Co. 900 hours. Glacial Acetic Acid. 4% 72 45 Tricresyl Phosphate 100 100 Impregnants Hydrocarbon Oil.com . 30% Ammonium Hydroxide. 50% Acetone Acetophenone Ammonia.spexsampleprep.spexsampleprep. Aqueous Calcium Hypochlorite. 2% Ethyl Acetate Ethanol Ethylene Glycol Ethyl Ether 80 80 60 20 20 60 20 60 20 60 20 20 20 80 60 20 60 20 20 20 20 20 60 60 20 20 100 60 80 60 20 Order Online 24/7: www. 75°C 100 100 Hydrochloric Acid. low. 10% 0 0 Solvents Dioxane (1. 10% 100 100 Hydroflouric Acid. hi. Con.XRF Accessories Chapter 5 Section 2 XRF Accessories Section 2 Chapter 5 Chemical Resistance of Mylar® Substance Conditions Percent Retained (typical) Tear Strength Elongation Tensile Strength 100 75 0 50 75 100 40 40 0 100 100 100 100 100 100 125 40 87 123 97 113 60 73 100 97 Chemical Resistance of Polypropylene Substance Temperature (°C) Acetic Acid. 75°C 85 65 Hydroxide. 150°C 92 18 Glyptal Resin GE2480 (baked) 90 80 Phenolic Resin GE1678 92 3 Silicone Resin GESR80 58 230 Silicon Resin GESR28 100 54 Reprinted by permission of E. 30% 100 100 Bases Ammonium 24 hours. vis.com Effect B A A B A A B B C A B. DC 200 79 141 Varnishes Asphalt Base GE9466 168 hours. 100°C 92 88 Hydrocarbon Oil.. Bulletin M-3C. 0 0 Nitric Acid. 25% 24 hours. 50% Cyclohexanol Cyclohexanone Decaline Detergents. 75°C 100 100 Ethyl Acetate 100 100 Ethanol 100 100 Methyl Ethyl Ketone 100 100 Toluene 100 100 Trichloroethylene 100 100 Miscellaneous Detergent. 136 Order Online 24/7: www.

com Order Online 24/7: www. 20% Hydrogen Peroxide Iodine Tincture Ketones Linseed Oil Lubricating Oil/Motor Oil Nitric Acid.. 50% Sulfuric Acid. 10% Paraffin Petroleum Ether Phenol Plating Solutions Pyridine Silicone Oil Sugars and Syrups Sulfamic Acid Sulfuric Acid. Bulletin PPD-32E Effect A C B B. 70% Nitric Acid.XRF Accessories Chapter 5 Section 2 XRF Accessories Section 2 Chapter 5 Chemical Resistance of Polypropylene (con’t) Substance Temperature (°C) Formaldehyde Gasoline Hexane Hydrochloric Acid. 30% Hydrochloric Acid. 10% Toluene Trichloroethylene Turpentine Whisky Wine Code: A-Negligible Effect B-Limited Absorption or Attack C-Extensive Absorption or Permeation D-Extensive Attack E-May Produce Cracking Under Stress Reprinted by permission of Hercules Inc.spexsampleprep.spexsampleprep. 98% Sulfuric Acid.E A B C A A A A A A C B A C C C A A Chemical Elements and Their Symbols Element Symbol Element Actinium Aluminum Americium Antimony Argon Arsenic Astatine Barium Berkelium Beryllium Bismuth Boron Bromine Cadmium Calcium Californium Carbon Cerium Cesium Chlorine Chromium Cobalt Copper Curium Dysprosium Einsteinium Erbium Europium Fermium Fluorine Francium Gadolinium Gallium Germanium Gold Hafnium Helium Holmium Hydrogen Indium Iodine Ac Al Am Sb Ar As At Ba Bk Be Bi B Br Cd Ca Cf C Ce Cs Cl Cr Co Cu Cm Dy Es Er Eu Fm F Fr Gd Ga Ge Au Hf He Ho H In I Iridium Iron Krypton Lanthanum Lawrencium Lead Lithium Lutetium Magnesium Manganese Mendelevium Mercury Molybdenum Neodymium Neon Neptunium Nickel Niobium Nitrogen Nobelium Osmium Oxygen Palladium Phosphorus Platinum Plutonium Polonium Potassium Praseodymium Promethium Protactinium Radium Radon Rhenium Rhodium Rubidium Ruthenium Samarium Scandium Selenium Silicon Symbol Ir Fe Kr La Lr Pb Li Lu Mg Mn Md Hg Mo Nd Ne Np Ni Nb N No Os O Pd P Pt Pu Po K Pr Pm Pa Ra Rn Re Rh Rb Ru Sm Sc Se Si Element Silver Sodium Strontium Sulfur Tantalum Technetium Tellurium Terbium Thallium Thorium Thulium Tin Titanium Tungsten Uranium Vanadium Xenon Ytterbium Yttrium Zinc Zirconium Symbol Ag Na Sr S Ta Tc Te Tb Tl Th Tm Sn Ti W U V Xe Yb Y Zn Zr 60 60 60 60 60 60 20 20 60 60 20 100 60 20 60 60 20 60 60 80 20 60 100 20 20 20 100 60 138 Order Online 24/7: www.E A B A A A B C.com 139 .

spexsampleprep. Or try out our sample preparation equipment in your laboratory for one week. Products Available For Demo: Katanax K1 Prime Electric Fluxer 8000D & 8000M Mixer/Mill 6770/6870/6970EFM Freezer/Mill 2010 Geno/Grinder 8530 Shatterbox 3635 X-Press Contact (732) 623-0465 Email: SamplePrep@spexcsp. Once you try our quality products you’ll ask yourself how you ever lived without them.XRF Accessories Chapter 5 Section 2 Would you like to test our sample preparation equipment with your own samples? Section 3 Application Notes Now You Can With SPEX SamplePrep’s Demo Program Contact SPEX SamplePrep to arrange a test grind in our labs by our experts. Best of all. We recommend test samples be sent to us directly to be processed in our demo lab.com Katanax K1 Prime is only available for local demos. 140 Order Online 24/7: www.com 141 . our demo program is complimentary! You only pay shipping and handling to and from your facility.

The Geno/ Grinder is a purpose-built ball mill that was originally conceived for the disruption of plant seeds but can also be used for animal and human samples. However.5 – 2 ml wells were placed next to each other in the Geno/Grinder clamp assembly. Results and Discussions The results show that the Geno/Grinder 2000 is well suited for cell disruption of muscle and internal organs. Institute for Plant Cultivation and Plant Breeding The mechanical homogenization for extraction of fatty acids is traditionally performed with an Ultra-Turrax in a buffer solution. A further reduction of the DNA amount is possible. homogeneous sample dispersion within each well.com 143 .com Order Online 24/7: www. Sample preparation is often the bottleneck in the process of efficient analysis work. Experiment During the first project year.e. several rinse steps and drying the samples are finally eluted. In contrast to this. The use of 96-well micro titer plates and deep well plates is suitable for this process. i. To establish a TILLING platform with automated DNA extraction and PCR amplification of target genes.Section 3 : Application Note SP001: Cell Disruption :: APPLICATION: Cell Lysis SP001 Section 3 : SP011 Application Note SP011: DNA Extraction :: APPLICATION: Leaf Material Mechanical Disruption for High-Throughput Fatty Acid Extraction from Animal Tissue Samples With kind permission of Sanofi-Aventis Germany GmbH Extraction of Nucleic Acids from Sugar Beet Leaves With kind permission of the University of Kiel. The research in biotechnology/ gene technology also often demands the handling of a considerable number of samples. For a routine PCR 1ng of highpure DNA is used. all wells are moved uniformly. The Geno/Grinder® 2000 is currently the first available mill specifically designed for cell disruption. Then two grinding balls were added. Afterwards the samples can be stored long-term at -20°C. Düren). The selection of the mutant population is carried out with DNA pools. (NucleoSpin Multi. This method is no longer suitable for high sample throughput. Machery & Nagel.well micro titer plate kit.spexsampleprep. After mixing.spexsampleprep. Therefore it makes sense to combine the increased sample throughput with mechanical cell disruption. The effective detection of point mutation occurs via hetero duplex formation between DNA molecules of wild type and mutant.96 Plant. both the purification and the slow sample preparation process in the analytical laboratory are labour-intensive. Thus prepared. the “Biomek micro centrifuge 24 position tube rack” for Eppendorf Safe-Lock reaction tubes. Up to now efforts to mechanically disrupt cells through grinding have been based on the modification of traditional ball or swing mills with an adapter for micro titer plates. e. This resulted in a fine. Following lysis. Only 2% of the samples did not yield an adequate amount of DNA. The maximum yields were around 16 μg. DNA from 2688 individual plants was isolated by using a 96. Using several small Zirconium oxide beads with a diameter of 2mm does not give a satisfactory result. This results in uniform and reproducible homogenization yields for all samples. However. it was possible to successfully homogenize the frozen material with stainless steel grinding balls of 4mm diameter. As well as using titer plates with 96 wells it is also possible to use other formats. The sheer force is not sufficient to grind frozen muscle tissue. With a pool composition of 8 different samples the utilized DNA amount is reduced to 0. Freeze dried rat muscle or livers were placed in each plate well and spiked with 100mM KH2PO4 buffer at pH 2 or trichloro-acetic acid. used for collecting and storing of biological materials with 1.5-1 g) was freeze dried in a 2ml Eppendorf vessel and then ground in the Geno/Grinder 2000 with two metal balls at a setting of 1000 (1000 strokes min-1) for 2 x 1 minute. First a representative range of EMS (Ethyl methane sulfonate)-mutants is produced from 2000-5000 M2 plants and identified through TILLING. Within the framework of a TILLING project (Targeting Induced Local Lesions In Genomes) nucleic acids from leaf material are to be isolated from potential mutants. liver. The plant tissue (0. Materials and Methods Two deep well plates (PP). The in vitro reproduction of linear DNA with GenomiPhi (GE Healthcare) allows further DNA analyses with small sample sizes. The samples were shaken vigorously for one minute at 1700 strokes per minute. Because of the vertical movement of the Geno/ Grinder clamps. and clamped into the Geno/Grinder. 142 Order Online 24/7: www. TILLING technology is a new and very effective method of reverse genetics for the production and identification of loss/gain of function-mutations of commercially valuable genes without genetic modification. filtration.g. each holding 24 Eppendorf vessels. four mounts (plastic blocks) were produced in-house. This type of sampling allows a flexible configuration of the individual samples. the deep-well plates were clamped into the Geno/Grinder. nucleic acid extraction of consistent yield and good quality is necessary. After grinding the tissue to a fine powder the samples were charged with 300 μl C1-buffer and homogenized in the Geno/Grinder for 30 seconds at a setting of 1000 (1000 strokes min-1). DNA quantification is carried out by photometry and gel electrophoresis. For this.125ng/individual plant so that with 100ng DNA. the quality of the results depends on the grinding accessories. the plate was covered with a sealing mat. the centrifuged samples are transferred into micro titer plates (round wells). When all wells were filled. the selection of DNA pools with 800 different target sequences becomes possible. Yields Approximately 40% of the samples yielded between 100 and 1500ng DNA.

Place and secure holder containing tubes into machine as per Geno/Grinder instructions.PC) suitable for use in 2000 Geno/Grinder® instrument. the neutralised solution can be used for assay of soluble metabolites.com 145 . UK Experiment The harvested plant material (up to about 300 mg) is pre-weighed into 5ml polycarbonate vials (SPEX SamplePrep cat no.7M perchloric acid to each tube. Conclusion Homogenization of sugar beet leaves for the purpose of extracting and isolating DNA for subsequent PCR amplification requires a sufficient amount of good quality nucleic acid yield (>1ng). Cap the tubes securely and place into the grinder foam holder.000 xG.spexsampleprep. 144 Order Online 24/7: www. into each vial. Norwich. 2240.4 M KCl. 1342-1345. Transfer the tubes to ice immediately after grinding. After centrifugation to remove the insoluble perchlorate.com Order Online 24/7: www.4 M MES. Then transfer the tubes to dry ice to keep material frozen and add 500 μl ice cold 0. All steps should be carried out at 0-4 ºC. After washing with water to remove the perchloric acid. 0. The tubes are then capped and placed immediately into liquid nitrogen (the time from harvest to freezing should be as short as possible) NB: Plant material can be harvested and frozen in any cryo-vial. Reference Smith AM and Zeeman SC (2006) Quantification of starch in plant tissues. Nature Protocols 1. Marilyn Pike from The John Innes Centre. Grind samples for 90 sec at 1500 strokes per minute (500 on the dial at x1 speed) — or until sample is smoothly pulverized. Department of Metabolic Biology.spexsampleprep.Section 3 : Application Note SP011: DNA Extraction :: APPLICATION: Leaf Material SP011 Section 3 : SP013 Application Note SP013: Grinding / Disruption :: APPLICATION: Starch and Soluble Metabolite Measurement in Leaves Perchloric Acid Extraction of Leaves for Measurement of Starch and Soluble Metabolites With kind permission of Dr. it can be used for assay of starch according to Smith and Zeeman (2006). 0. Place one good quality stainless steel ball. This demonstrates the excellent suitability of the Geno/Grinder 2000 for high throughput processing of sugar beet leaf material. Centrifuge for 10 min at 4º C and14. then transferred to the Geno/Grinder tubes just before grinding if necessary. With a basic grinding process of 2 x 1 minute grinds of dry leaf material and subsequent wet homogenization of 30 seconds only 2% of more than 2600 did not yield suitable DNA material.7M perchloric acid to each tube and vortex briefly. Add an additional 2500 μl ice cold 0. Allow the acid to freeze. Remove and neutralise the resulting supernatant to pH 6-7 by addition of 2 M KOH. 10 mm diameter in 316 grade material. The pellet contains the starch.

Lanes 2-5. P. More than adequate RNA for both microarray experiments and subsequent real time validation were isolated using this protocol. 24 and 48 hours after shift from Yeast Extract Method to Yeast Extract Sucrose Media. Lane 6-9.0% Agarose gel. 19-22. Box 9650.Section 3 : Application Note SP014: RNA Extraction from Aspergillus parasiticus mycelium :: APPLICATION: RNA Extraction SP014 Section 3 : SP014 Application Note SP014: RNA Extraction from Aspergillus parasiticus mycelium :: APPLICATION: RNA Extraction RNA Extraction from Aspergillus parasiticus mycelium With kind permission of J. During this final homogenization the Puresol buffer and ground mycelium thawed and mixed completely. with a A260/280 ratios varying from 2. In that context we describe here RNA isolation of A. The sample tubes containing the homogenized sample buffer mix were transferred to a room temperature foam holder before homogenizing for an additional 2 minutes in the Geno/Grinder. This protocol allows simultaneous processing of large numbers of samples. The harvested fungal mycelium samples were flash frozen in liquid nitrogen and stored at -80ºC for RNA preparation and aflatoxin extraction. Yields Experiment For this experiment A. 6. 2600).80ºC for RNA preparation and the remaining aliquots were used to inoculate 100 mL of YES medium (60 g/L of sucrose and 25 g/L of yeast extract) and incubated at 30ºC with 150 rpm shaking until harvested at 3.5 μg/uL to 3. 12. No.19 or better. in a final volume of 50 μL. The harvested mycelia were divided into 1 gram aliquots. One sample was frozen in liquid nitrogen and stored at . parasiticus during a simple carbohydrate shift. parasiticus SU-1 900 ng of total RNA isolated from Mycelium grown 48 hours in Yeast Extract Media.1. NC) and incubated at 30ºC. 2240-PE) containing one 3/8” (9. replicates A-D of A. they were arranged within a 24-well aluminum Cryo Adapter block (SPEX SamplePrep catalog 2263) and pre-chilled for 15 minutes in a CryoStation (SPEX SamplePrep Cat. and 23-26 replicates A-D of A. Mississippi State. ATCC # 56775 and 201461) a wild-type strain used for biochemical and genetic studies in both B group (B1 and B2) and G group (G1 and G2) aflatoxins was chosen.com Order Online 24/7: www. However. Wilmington. Total RNA was extracted according to manufacturer’s protocols. The chilled samples and adapter block were clamped in the SPEX SamplePrep 2000 Geno/Grinder and ground at a rate of 1050 strokes per min (dial setting of 150) for 1 minute and 30 seconds. parasiticus SU-1 total RNA isolated from Mycelium collected at 3. Lanes 1 and 14. USA Introduction Recent genomic efforts on toxigenic and nontoxigenic Aspergillus species have advanced our understanding of the biology and genetics of these filamentous fungi. Wilkinson and R. 12. RNA concentration varied from 1. parasiticus SRRC 143 (or SU-1. 1 Kb ladder (Invitrogen). 146 Order Online 24/7: www.5 mm) stainless steel grinding ball per tube. No. parasiticus spores were inoculated to a final concentration of 105 spores/mL in 200 mL yeast extract (YE) liquid medium consisting of 25 g/L of yeast extract (DIFCO) and incubated for 48 hours at 30ºC with constant shaking at 150 rpm. we demonstrate here a highly reliable methodology capable of isolating high quality RNA from small quantities of fungal mycelium.spexsampleprep. For a routine qRT-PCR 500 ng to 1 μg of total RNA is used as compared to 3 to 5 μg for the typical microarray experiment. MS 39762.O. NJ) A. using the Aurum Total RNA fatty and fibrous tissue kit (Biorad). Mississippi State University. Gibbstown. 6. Total RNA was quantified using a ND-1000 Spectrophotometer (NanoDrop Technologies.R. After addition of Puresol the samples were homogenized in the SPEX SamplePrep 2000 Geno/Grinder for 2 minutes at 1050 strokes per minute. Conclusion Though several environmental factors can affect the final quality of RNA. Cryo-Station. Using a prechilled spatula 50 mg to 100 mg of the frozen fungal tissue was transferred to the pre-chilled tubes. thus demonstrating the suitability of the Geno/Grinder for high throughput processing of fungal mycelium. The spores were collected from 5-day cultures with sterile 0. 24. Fresh spores were generated by plating 50 μL of 108 spores onto Difco Potato-Dextrose Agar (PDA) (American Scientific Products.com 147 . and 48 hours post-inoculation.05% Triton X-100 (EMD Chemicals Inc. 10-13.spexsampleprep. To ensure that all ground tissue was suspended in Puresol the samples still housed within the adapter block was inverted 2-3 times and returned to the Figure 1. Shivaji. 15-18. Charlotte. The samples and block combination were quickly removed from the Geno/Grinder and returned to the Cryo-Station. Samples were removed from the Geno/ Grinder and incubated at room temperature for 10 minutes before transferring to sterile 2 mL Eppendorf tubes. DE) and visualized by gel electrophoresis (figure 1) to ensure quality.8 μg/uL. To each ground sample 1 mL of Puresol from the Aurum Total RNA fatty and fibrous tissue kit (Biorad) was added. The fungal mycelia were harvested by filtration in vacuo. it is clear that these complex experiments suffer greatly from the variability in the quality of RNA between each replicate and it is critical to establish a platform to isolate high quality RNA for use in both microarray and qRT-PCR.01 to 2. Sample Extraction Before samples were processed in 24-well polyethylene vials (SPEX SamplePrep Cat.. Department of Biochemistry and Molecular Biology. which directly affects both microarray and real time experiments.

at a rate of 2000 cyc/min. >1 gram of leaves were chopped into small pieces and mixed. Next.com Order Online 24/7: www. However.spexsampleprep. 100 mg fresh basil leaf. San Diego. Alvin. The 2000 Geno/Grinder® was compared with a competitive cell lyser (Competitor A) for extraction of DNA from fresh basil. harvested from live plant immediately prior to lysis. Incubate the samples in about 1in. while buffers. 100 mg of chopped leaf mixture was placed into each of 10 tubes. Dispense extraction buffer into each well and securely cap each well. Finding a quick method in which DNA could be extracted and used for PCR is essential. Dispense one 5/32 in. ABSTRACT Mechanical cell lysers are used for effective extraction of genomic DNA from samples containing plant or animal tissue. Conclusion The method described above is sufficient for PCR and it takes less time than the standard chloroform extraction. 2100).com 149 . grind them in the SPEX SamplePrep 2000 Geno/Grinder at 500 strokes/minute for two minutes.8. Described below is a quick “dirty” method that produces a high enough concentration of DNA that can be used for PCR. Tube # Homogenizer* Time (sec) Speed (cyc/min) 1 CA 40 6000 2 CA 40 6000 3 GG 40 4 GG 40 5 GG 60 6 GG 60 2000 7 GG 90 8 GG 90 9 GG 120 2000 10 GG 120 2000 2000 2000 2000 2000 2000 *CA = Competitor A Instrument *GG = Geno/Grinder® Instrument (SPEX SamplePrep LLC) 148 Order Online 24/7: www. add one seed to each well. Centrifuge again for 1 minute.. Transfer 300 μL of the supernatant to a clean 96-well plate. In addition. Results indicated that use of the Geno/Grinder provided DNA with higher molecular weight than the competitive instrument. DNA can be further purified with clean-up kits available on the market. homogenization time and operating rate were varied for the Geno?Grinder. Add neutralizing extraction buffer and seal the assay block with sealing film. SAMPLE SETUP : : TUBES: : : SAMPLE: : : LYSIS REAGENTS: : : HOMOGENIZATION: 2 ml conical-bottom screw-cap tubes on a standard 48 well rack. 400 ml of Buffer Ap1 and 4 ml of RNaseA from commercially available genomic DNA isolation kit were added to each tube. all mechanical lysers do not provide the same outcome. optimal homogenization conditions using the Geno/Grinder were found to be 90 sec.spexsampleprep. Yields The total concentrations yielded from the samples range from 3-7 ng/μL in a final volume of 200 μL with purities of 1. (4 mm) stainless steel bead into each well using the Grinding Ball Dispenser (SPEX SamplePrep Cat. No. : : GRINDING MEDIA: Garnet and single 1/4 inch ceramic bead (“Lysing Matrix A”). After the samples have been capped.Section 3 : SP016 Section 3 : SP017 Application Note SP016: Lysing / Homogenization :: APPLICATION: DNA Extraction from Rice Seeds Application Note SP017: Lysis Time and Other Variables on DNA Extraction :: APPLICATION: DNA Extraction from Fresh Basil Lysed Quick DNA Extraction from Rice Seed With kind permission of RiceTec Inc. TX Effect of Lysis Time and Other Variables on DNA Extraction from Fresh Basil Lysed in 2 ml Tubes With the Geno/Grinder® With kind permission of Sunrise Science. In addition. grinding media and tube size remained constant. Centrifuge for 1 minute to bring all liquid to the bottom of the assay block. CA Introduction DNA extractions can be a very time consuming and tedious process. Sample Extraction Samples are prepared using a 96-well 1 mL assay block.5-1. Centrifuge the samples for 10 minutes at 3000 rpm. Total time ranges from one to two hours. (25.4 mm) of water at 95ºC for 20 minutes then place them on ice for approximately 10 minutes or until samples are cool to the touch.

indicating that significant shearing or degradation had not occurred. The yeast remained intact after processing for 10 min. protoplasts generated from enzymatic digestion usually require lysis with detergents that will also denature many proteins to inactivity. the most popular yeast continues to be Saccharomyces. Furthermore. A range of glass bead sizes was used including 106 mesh (very small). did not appear to offer any benefit. 2% peptone.557 bp. and 425-600 mesh (large).. Optimal lysing conditions for the re-designed 2010 Geno/Grinder may differ somewhat from those reported here. DATA Outside Marker (lanes 1 and 14): Kb ladder Inside Marker (lanes 2 and 13): Lambda Hind III INTERPRETATION After homogenization for 40 sec. Little to no difference in the results was observed at these two processing times. in the Geno/Grinder. High Throughput Disruption of Yeast in a 96-Well Format The wealth of information generated from years of biochemical.spexsampleprep. While run times for 40 and 60 sec. can be used to disrupt yeast in a microwell plate format. individual processing is a major bottleneck and impractical. including Pichia. Yeast mRNA and intracellular proteins are often times difficult to extract intact from cells by traditional enzymatic methods. However. Further optimization of the processing time may be possible by varying the type and size of grinding media. on the Geno/Grinder yielded high molecular weight DNA. Mechanical disruption of yeasts has traditionally been accomplished by using either a press or bead mill (i. Negative Control yeast without glass beads. Though many yeast species are in use. 212-300 mesh.e. In addition. yeast are a popular host for gene expression studies and for the production of recombinant proteins. The Geno/GrinderTM (SPEX SamplePrep. Materials and Methods Saccharomyces cerevisiae was cultured overnight in YPD medium (1% yeast extract. Metuchen.. bead beater). mechanical cracking/fracturing of the yeast cell is often required to liberate the molecules. 2% glucose) at 30°C with agitation (150 rpm). At both 90 and 120 sec. 100 ml of culture broth was added to each well along with 50 mg of acid washed glass beads (Sigma.com 151 . Hansenula. use of the Geno/Grinder gave higher quality DNA than was obtained using the competitive lyser. using the competitive cell lyser. nearly all the DNA isolated using the Geno/Grinder was higher than 6. Therefore. at 2000 cyc/min with the 2000 Geno/Grinder. G-8772). Consequently. and molecular analyses has made yeasts both model biological systems and tools for biopharmaceutical scientists.com Order Online 24/7: www. genetic. 150-212 mesh. Figure 1. a method is needed that combines mechanical disruption of cells in a high throughput format.spexsampleprep. In both approaches. Using a sterile 96 well microtiter plate (Corning Life Science Products). but also the molecules of interest. and Debaryomyces. Culture broth without glass beads was also prepared as a 150 Order Online 24/7: www. a bead mill originally designed to smash seeds in deep well plates.Section 3 : Application Note SP017: Lysis Time and Other Variables on DNA Extraction :: APPLICATION: DNA Extraction from Fresh Basil Lysed SP017 Section 3 : SP018 Application Note SP018: High Throughput Disruption of Yeast in a 96-Well Format :: APPLICATION: DNA/RNA and Other Extractions DNA PURIFICATION Post-lysis purification was performed using a commercially available plant kit according to the kit manual. Consequently. Lysing enzymes are often crude preparations containing RNases and proteases that will not only attack the cell wall. samples are processed individually. DNA of lower molecular weight (lower quality) was obtained than for samples processed at any of the four run times using the Geno/Grinder. that was beyond the scope of this project and was not attempted. insufficient quantities were obtained. Increasing the processing time to 120 sec. NJ). even at the longer processing time. For experiments where large numbers of yeast clones must be examined in a high throughput screening environment. CONCLUSIONS The best conditions for processing fresh basil were found to be 90 sec.

. The resulting pulp can then be used as a source of DNA for genetic analysis. an approach that is not practical for high throughput screening of seeds as manual grinding is slow and reuse of mortar and pestles may lead to cross-contamination. The plate was sealed with a rubber-sealing mat and locked into the Geno/Grinder. 2150) and soaked for 12 hours in distilled water prior to processing. The isolation of nucleic acids from intact seeds requires mechanically disrupting the seed followed by the extraction and subsequent purification of the nucleic acid. Soybeans that are soaked overnight in water are effectively and uniformly homogenized in less than 3 minutes. Figure 3. Qiagen Plant DNeasy. namely the CTAB. with 425-600 mesh glass beads. Figure 2. A piece of adsorbent paper was placed on top of the plate and the plate was locked into the grinder. The efficiency of seed disruption is dependant upon the type of ball mill used in the grinding process. Conventional isolation methodologies can then be used to purify the nucleic acids from the seed homogenates. Yeast disrupted for 5 min. the probability of well to well cross contamination of genetic material is greatly increased. Wizard Genomic. Four different DNA methods were compared for the isolation of DNA from the soybean homogenates. the lid is carefully removed. This motion allows glass beads to impact the cells more directly than standard mills where beads impact the well walls in addition to the cells.com 153 . Most yeast have been effectively disrupted as is demonstrated by cell ghosts and cellular debris. Comparison of Methods for the Isolation of DNA from Soybeans With kind permission David Burden. This motion is not believed to lead to uniform cell disruption. President of BT&C Incorporated Results and Discussion The efficiency of yeast disruption is dependent upon the size of the glass beads and the duration of the grinding. Lower mesh glass beads were less effective in cracking cells with the 106 mesh beads being particularly ineffective.D. The yeast cells were disrupted for 5 and 10 minutes at 1500 rpm. It is concluded that 425-600 mesh glass beads are most suited for disrupting Saccharomyces. Using a grinding ball dispenser a grinding ball was also placed on top of each seed. with 425-600 mesh glass beads. The deep well plate with lid was then centrifuged at 1500 rpm to pellet lysate and condense liquid from the rim and walls of the well.0 mL deep-well of a 96-well plate containing a 4 mm stainless steel grinding ball (Cat.spexsampleprep. Following disruption. Figures 1-3 demonstrate the efficiency of cell disruption with 425600 mesh glass beads at 5 and 10 minutes.Section 3 : Application Note SP018: High Throughput Disruption of Yeast in a 96-Well Format :: APPLICATION: DNA/RNA and Other Extractions SP018 Section 3 : SP019 Application Note SP019: Comparison of Methods for the Isolation of DNA from Soybeans :: APPLICATION: DNA/RNA and Other Extractions negative control. The plate was sealed with a fitted Teflon®/silicone mat and placed in the Geno/Grinder. The Geno/Grinder® is designed to effectively disrupt cellular materials by oscillating the plate vertically. Once centrifuged. the yeast cultures were examined by phase contrast microscopy and photographed. Standard bead mills adapted to microwell plates are modeled after “paint shakers” and move the plates in a “figure eight” motion. No.5 minutes at 1500 rpm. Standard bead mills adapted to microwell plates are modeled after “paint shakers” and move the plates in a “figure-eight” motion. This motion does not lead to uniform seed disruption. This motion allows balls to impact the seeds more directly than standard mills where balls impact the well walls in addition to the seed.spexsampleprep. Without centrifugation. nucleic acids can be isolated from seeds in a microwell plate format using a ball mill that mechanically disrupts the seeds. and Qiagen Genomic methods. Each of these methods is summarized briefly below. Alternatively. Materials and Methods Soybeans were placed in each 2. Some intact yeast remain. 152 Order Online 24/7: www. The mechanical disruption is often performed manually with a mortar and pestle.com Order Online 24/7: www. The design of the Geno/Grinder is also believed to be a factor in the disruption process. Ph. The seeds were disrupted for 2. Yeast disrupted for 10 min. The Geno/Grinder is designed to effectively disrupt cellular materials by oscillating the plate vertically. Cracked yeast appear as dark “ghosts” while intact yeast continue to refract light and appear as bright.

The genomic DNA was tested for genetically modified sequences. The solution was then frozen for 20 minutes at -80° C. The DNA pellet was resuspended in TE buffer. Buffer AP2 (130 µL) was then added to the lysate. 0. It was then centrifuged for 10 minutes at 9000 rpm. The sample was thawed at room temperature and centrifuged. The mixture was incubated for 10 minutes at 65° C. lower yields of large sized fragments (e.Section 3 : Application Note SP019: Comparison of Methods for the Isolation of DNA from Soybeans :: APPLICATION: DNA/RNA and Other Extractions SP019 Section 3 : SP019 Application Note SP019: Comparison of Methods for the Isolation of DNA from Soybeans :: APPLICATION: DNA/RNA and Other Extractions DNA Purification Using the Qiagen DNeasy™ Plant Kit After grinding. Comparison of methods for DNA isolation from Soybean. the soy sample was applied to the column. Agarose gel electrophoresis of the genomic DNA (Fig. The upper layer (aqueous phase) was transferred to a new tube and 0. 2) illustrates a significant difference in yield and fragment size of the DNA. The flow-through is discarded. and incubated for 5 minutes on ice. The upper layer was extracted with an equal volume of chloroform..4 M NaCl. Analysis of the reactions was done electrophoretically (1X TAE with 3% agarose) and is illustrated in Figure 2. The sample was thawed at room temperature and centrifuged to pellet the DNA.com 155 . After mixing for 30 seconds. The ethanol was removed. 20 mM EDTA). Depending upon the application of the DNA. and any residual ethanol was removed by centrifuging in the DNA Speed Vac.04 M NaCl) were added. using PCR. the DNA binds to the column. mixed. the soy was suspended in 10 mL of Buffer G2. A comparison of the DNA yields for the isolation procedures was made by agarose gel electrophoresis (0. The resulting DNA pellet was washed with ice-cold 70% ethanol and centrifuged. the mixture was centrifuged for 10 minutes at 9000 rpm. but fragment size is extremely small as compared to the other DNA preparations and measured against the molecular weight markers. The DNA was then resuspended in 50 µL Buffer TE. This solution was chloroform extracted. The supernatant was transferred to a new tube. the soy was mixed with 600 µL Nuclei Lysis Solution and incubated for 15 minutes at 65° C. Figure 1.7 volumes of isopropanol was added. PCR analysis of isolated DNA from soybean Results and Discussion The isolation method used to extract DNA from soybean homogenate affects the quantity and quality of the genomic DNA isolated. The sample was mixed gently by inversion and then centrifuged at 9000 rpm. The DNA was eluted with 50 µL Buffer AE by incubating for 5 minutes at room temperature and then centrifuging for 1 minute at 9000 rpm. Lanes 1.1 M Tris/HCl. A Qiagen genomic tip 100 column was equilibrated with Buffer QBT. the CTAB method produced the greatest yield. and the column was washed two times with Buffer QC. Samples were analyzed for the soy lectin gene and Cauliflower Mosaic Virus 35S promoter/Petunia transcription sequence marker found in genetically modified soybean (Roundup ReadySoya). and then centrifuged at maximum speed in order to dry the membrane. The supernatant was removed. 4 and 7 – Lambda HindIII digest. The tube was centrifuged and the ethanol was decanted. Lane 2 – Qiagen Genomic DNA Kit. After mixing. the lysate was applied to the DNeasy mini spin column and centrifuged at 9000 rpm for 1 minute. The mixture was incubated for 60 minutes at room temperature and then centrifuged for 5 minutes at 9000 rpm. RNase was added followed by a15 minute incubation at 37° C and a 5 minute cooling to room temperature. Elution of the DNA was done with 5 mL Buffer QF.spexsampleprep.spexsampleprep. Figure 2.com 154 Order Online 24/7: www. Based on the fluorescence of the DNA smear in the ethidium bromide stained gel. This mixture was incubated for 30 minutes at 65° C. PCR analysis of the samples was positive for the soy lectin gene and negative for the 35 S promoter/ Petunia TS sequence.7% agarose in 1X TAE buffer) which is illustrated in Figure 1. The DNA was resuspended in 50 µL DNA Rehydration Solution during incubation for 1 hour at 65° C. DNA Purification Using a Qiagen Genomic Column DNA Purification with the Promega Wizard® Genomic DNA Purification Kit After grinding. The column was washed with Buffer AW.2 M NaCl. Following equilibration. and residual ethanol was removed with a DNA SpeedVac. the Wizard method or Genomic Column method) may be preferred. This is particularly useful for high throughput PCR analysis in agricultural biotechnology laboratories or laboratories performing GMO analysis.e. and two volumes of CTAB precipitation solution (5 g CTAB/L. CTAB Method for DNA Purification The ground soy was diluted in 500 µL CTAB buffer (20 g CTAB/L. The precipitates were removed with the QIAshredder™ spin column. Lane 3 – CTAB Methood. The DNA was precipitated with 0. During this step. The eluent was mixed with 0.7 volumes of isopropanol and freezing at -80° C for 20 minutes. Lane 5 – Promgea Wizard Kit. The ethanol was discarded. 1. The pellet was washed with 70% ice-cold ethanol and then centrifuged.g. the soy was mixed with 400 µL Buffer AP1 and 4 µL RNase stock solution. and the precipitate was dissolved in 1. The supernatant was removed and the pellet was washed with 70% ethanol. Order Online 24/7: www. After grinding.. Excess ethanol was removed by inverting the tube onto absorbent paper and air-drying for 15 minutes. 0. i. Protein Precipitation Solution was added followed by centrifugation to pellet precipitated proteins.5 volume of Buffer AP3 and 1 volume of ethanol (96-100%). GMO analysis. The supernatant containing the DNA was transferred to another microfuge tube containing isopropanol. This analysis demonstrates that soybean homogenates generated from the Geno/ Grinder are suitable for genetic analysis. Lane 6 – Qiagen DNeasy Kit.

156 Order Online 24/7: www. the cell pellet was suspended in 20 ml of sterile 8% NaCl solution. in one-minute intervals for periods ranging from one minute to twelve minutes. Conclusion The 2000 Geno-Grinder is capable of lysing bacterial cells in 96-well titer plates with 400-600 μ silica beads as grinding media. With increased grinding time culture filtrate shows a definite increase in optical density.4 grams of silica beads were added to each well.4 grams of silica beads per well. salt-tolerant Halomonas elongata. Cells were washed once with sterile 8% (w/v) NaCl solution to remove spent growth medium. The delivery of the beads into each cell of the titer plate can be accomplished in a number of ways. and the plate was sealed. indicating release of nucleic acids during grinding.5 ml of this suspension.com Order Online 24/7: www. Each well of the test plate was filled with 0. In this case micropipette tips were filled to the mark with grinding beads. Both organisms were grown to late log state at 370 C. gram-positive Bacillus. Standard 96-well titer plates were used with 400-600 μ silica grinding beads (Molecular Biology Grade. cat. and each tip emptied into a titer plate well.com 157 .spexsampleprep. The average data for three separate “well sets” is shown in Figure 1. Other delivery systems are commercially available. then harvested via centrifugation at 7000 RPM for 10 minutes. 2166). Vreeland. 0. Experiments were performed with 250 – 500 ml of bacteria: in one case the gram-negative. with shaking.spexsampleprep. This technique will deliver approximately 0. January 2003 The SPEX SamplePrep 2000 Geno/Grinder was tested to determine if this technology could be used to lyse bacterial cells. After washing.Section 3 : Application Note SP020: Lysing of Bacterial Cells in the Geno/Grinder :: APPLICATION: DNA/RNA and Other Extractions SP020 Section 3 : SP020 Application Note SP020: Lysing of Bacterial Cells in the Geno/Grinder :: APPLICATION: DNA/RNA and Other Extractions Lysing of Bacterial Cells in the Geno/Grinder With kind permission of Russell H. Culture filtrate from the shaken plates was then measured for optical density at 260 nm. it was important that the cells to be lysed were present in high concentration. West Chester University. and in the other. Grinding times of 6 to 9 minutes appear to be suitable for producing measurable amounts of nucleic acid. The filled titer plates were then shaken in the Geno/Grinder at a setting of 1450 strokes per minute. no.

Davis. Piechaczyk. The quality of the cDNA is judged according to the CT value obtained with a endogenous control TaqMan PCR system from a defined amount of tissue. 1993).. 0. The gDNA quality from a defined amount of tissue is judged according to the CT value using a TaqMan PCR system targeting a single copy gene. Smith. Calcified Tissue International. Garcia-Meunier. we normally use TaqMan PCR systems targeting species specific glyceraldehyde-3-phosphate dehydrogenase (GAPDH) or ribosomal genes (such as 18S rRNA or ITS-2). 10 U RnaseOut (Rnase inhibitor). Online Journal.com 159 . Samples with values above a certain threshold indicate impaired sample quality and degradation of total RNA and warrant re-extraction of a back-up sample.. Amplification conditions were 2 min at 50°C.M. To assess the quality of extracted genomic DNA. The samples were placed in 96 well plates and amplified in an automated fluorometer (ABI PRISM 7700 Sequence Detection System. Each real-time TaqMan PCR reaction contained 400 nM of each primer. C. 1999. Leutenegger. 1990. M. Akens. Alluwaimi. Conditions were optimized for an Applied Biosystems 6700 automated nucleic acid (ANA) workstation. W.M. as well as fish and clams.D.M. 2001. complementary DNA (cDNA) was synthesized using Invitrogen products: 200 units of SuperScript III.M. J. cmluetenegger@ucdavis. Quantitation of bovine cytokine mRNA in milk cells of healthy cattle by real-time TaqMan polymerase chain reaction. 72:759-62.3). To assess the quality of cDNA.625 U AmpliTaq Gold DNA polymerase per reaction. After 30 minutes at 40º C. Fort. the tissues were transferred frozen to a deep-well titer plate standing on a block of dry ice. Each well contained two 4-mm stainless steel balls (SPEX CertiPrep cat. Jan 1. and D. P. After addition of 60 µl of water. 40 cycles of 15 s at 95°C and 60 s at 60°C.. 2. mouse. the reaction was terminated by heating for 5 minutes to 95ºC and cooling on ice.spexsampleprep.. The reverse transcription reaction took place for 50 minutes at 500 C..25 U AmpErase UNG per reaction and 5 µl of the diluted cDNA sample or the gDNA in a final volume of 25 µl. K. C. 2150) and 500 microliters of buffer (Applied Biosystems nucleic acid purification lysis buffer). 158 Order Online 24/7: www. Leutenegger. GAPDH TaqMan systems can be used to target the single copy GAPDH pseudogene (Galland et al. Mamm. M.. and horse. Birnbaum. Veterinary Immunology and Immunopathology. C. P. Auer. The plates were sealed with a plastic cover and subjected to grinding in the 2000 Geno/ Grinder for 2 minutes at a setting of 1000 strokes per minute. and H. Leutenegger. M. snap-frozen in liquid nitrogen. Preparation and Tissue Grinding Fresh samples of animal tissue were collected. 1993. An overview of TaqMan systems used for gDNA quality control is given in Table 1. Biochimie. 50 mM KCl. Pirisi. Concerted evolution in the GAPDH family of retrotransposed pseudogenes. J. Perani. L. University of California. 77: 275-287.spexsampleprep. 600 ng of random hexadeoxyribonucleotide (pd(N)6) primer (random hexameter priner). 1990.com Order Online 24/7: www.. January 2003 Sample Collection. 0. C. Genome. Samples with values above a certain threshold indicate degraded DNA and warrant re-extraction of a back-up sample. M. Etienne-Julan. References GAPDH pseudogenes: Galland.edu. Stefanova. The real-time TaqMan PCR and applications in Veterinary Medicine. Zlinsky. 80 nM of the TaqMan probe and commercially available PCR mastermix (TaqMan Universal PCR Mastermix. Quality Control of Extracted RNA/cDNA and Genomic DNA Using Real-Time Taqman® PCR To assess the quality of the extracted RNA. . 4:695-703. Ph. V. Mislin. The animals were man. Veterinary Sciences Tomorrow. 10 min at 95°C. trimmed to approximately 50 – 100 mg of wet weight. 5 mM MgCl2.M. Applied Biosystems) containing 10 mM Tris-HCl (pH 8. cow. dog. Leutenegger. no. 2001. and F. Cullor. Characterization of a murine glyceraldehyde-3-phosphate dehydrogenase pseudogene. lysates were used for either gDNA extraction or total RNA extraction. 65:378-383. according to the manufacturer’s instructions. The final amount of tissue subjected to RNA and/or DNA extractions was between 10 and 20 mg. B. Lutz: Quantitative real-time PCR for equine cytokine mRNA in nondecalcified bone tissue embedded in methyl methacrylate.5 mM deoxynucleotide triphosphates. Garcia-Meunier et al. von Rechenberg. Before DNA and/or RNA extraction. cat. see Table 1.Section 3 : Application Note SP021: Extraction of RNA/cDNA and Genomic DNA from Tissue with Real-Time PCR APPLICATION: DNA/RNA and Other Extractions SP021 Section 3 : SP021 Application Note SP021: Extraction of RNA/cDNA and Genomic DNA from Tissue with Real-Time PCR APPLICATION: DNA/RNA and Other Extractions Extraction of RNA/cDNA and Genomic DNA from Tissue with Real-Time PCR With kind permission of Christian M. A. species specific TaqMan PCR systems were developed targeting single copy genes to allow the quantitation of genome equivalents and cell numbers. Applied Biosystems). Bonhomme. and 1 mM dNTPs in a final volume of 40 l. F. and stored at –800º C.

25 10 ml Ad 25 ml IL10 12.spexsampleprep.25 10 ml Ad 25 ml 12.5 1x 5 300 300 300 300 400 400 80 0.25 10 ml Il16 12.25 10 ml 12.75 0. 100 mM EDTA.5 1x 5 300 300 300 300 400 400 80 0.5 1x 5 300 300 300 300 400 400 80 0. passive reference ROX. species and TaqMan systems used to assess quality of cDNA and gDNA Tissue Skin Skeletal Muscle Lung Brain Lymph Node Spleen Thymus Tonsil Cartilage Heart Tail Fin Gill Spine Tissue Mussel Liver Cranium Gill Liver Digestive Gland Mussel Liver Skeletal Muscle Kidney NA: Not Available CT Value: Cycle Threshold Value: PCR cycle at which the fluorescent intensity exceeds the threshold Table 2: Composition of real-time fluorogenic Taqman PCR assay 2x Mastermix 10x Buffer A MgCl2 (mM) dATP (mM) dCTP (mM) dGTP (mM) dUTP (mM) Forward primer (nM) Reverse primer (nM) TaqMan probe (nM) AmpliTaq Gold (U) AmpErase UNG (U) Template (cDNA) H2O GAPDH 12.3 at room temperature 160 Order Online 24/7: www.25 10 ml Ad 25 ml IL4 12.75 0. 100 mM Tris-HCl.Section 3 : Application Note SP021: Extraction of RNA/cDNA and Genomic DNA from Tissue with Real-Time PCR APPLICATION: DNA/RNA and Other Extractions SP021 Section 3 : SP021 Application Note SP021: Extraction of RNA/cDNA and Genomic DNA from Tissue with Real-Time PCR APPLICATION: DNA/RNA and Other Extractions Table 1: Overview of tissue samples.5 1x 5 300 300 300 300 400 400 80 0.spexsampleprep.75 0. 600 nM.5 1x 5 300 300 300 300 400 400 80 0.5 1x 5 300 300 300 300 400 400 80 0.com 161 .5 1x 5 300 300 300 300 400 400 80 0.25 10 ml Species Dog Dog Cow Cat Cat Cat Cat Cat Horse Mouse Mouse Rainbow Trout Rainbow Trout Rainbow Trout Rainbow Trout Rainbow Trout Rainbow Trout Koi Koi Clams Clams Human Human Human RNA/cDNA Target Gene GAPDH GAPDH GAPDH GAPDH GAPDH GAPDH GAPDH GAPDH GAPDH GAPDH GAPDH ITS-2 ITS-2 ITS-2 ITS-2 ITS-2 ITS-2 ITS-2 ITS-2 18S rRNA 18S rRNA GAPDH GAPDH GAPDH CT Value <21 <24 <24 <24 <21 <21 <21 <21 <24 <24 <21 <14 <14 <14 <14 <14 <16 <14 <14 <11 <11 <21 <24 <24 Genomic DNA Target Gene GAPDH GAPDH GAPDH CCR5 CCR5 CCR5 CCR5 CCR5 IGF-I IGF-I IGF-I IGF-I IGF-I IGF-I IGF-I IGF-I IGF-I Glucokinase Glucokinase NA NA IL-2 IL-2 IL-2 CT Value <24 <25 <25 <25 <22 <22 <22 <22 <26 <24 <21 <26 <24 <24 <26 <21 <24 <24 <21 NA NA <21 <24 <24 Ad 25 ml Ad 25 ml Ad 25 ml 10 x TaqMan Buffer A contains 500 mM KCl.25 10 ml Ad 25 ml IL 12 p35 IL 12 p40 IFN-g 12.75 0.75 0. pH 8.com Order Online 24/7: www.75 0.75 0.

Tanos is a fungicide containing both famoxadone and cymoxanil and the cumulative effect of these two active ingredients offers even better control of late blight potatoes. Sample Prep for LC/MS Analysis There are approximately 20 clean-up steps in the AMR 3705-95 procedure. over twenty steps are required to get the sample in a convenient form for analysis. Acetonitrile is added and samples are ground with a laboratory homogenizer. Keith Tucker. DuPont de Numours and Co. AMR 3705-95.” (2) In this procedure. cucumbers and leafy vegetables. Cymoxanil is not retained on either of these columns. carefully taken to dryness. the acetonitrile aliquot is back extracted with hexane. Discussion Three of the leading pesticides sold by DuPont are Famoxate®. Its protection mechanism is to penetrate the surface to induce host defense response to stop lesion growth and sporulation. Based on the sensitivity and selectivity of LC/MS. Under this method. and sodium sulfate. concentrated.Section 3 : APPLICATION NOTE SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis APPLICATION: Pesticide Residue Extraction SP022 Section 3 : SP022 APPLICATION NOTE SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis APPLICATION: Pesticide Residue Extraction The Benefits of the Geno/Grinder® High-Throughput Tissue Homogenizer to Increase Sample Throughput for Pesticide Residue Analysis by LC/MS/MS With kind permission of: Joseph McClory. The eluate is concentrated. Famoxate is a fungicide containing the active ingredient famoxadone and is mainly used to control early blight tomatoes. The extract is then cleaned further using a hexane liquid/liquid extraction followed by an Envi Carb SPE column. and inverted to aid in the dissolution of sodium chloride and then allowed to stand while the acetonitrile (upper layer) and water phases separated. the number of clean-up steps can be significantly reduced. The goal of this study was to take advantage of recent developments in sample preparation with the 2000 Geno/Grinder® and instrument sensitivity and selectivity using the API 5000 LC/MS/MS system to increase the number of samples analyzed per day by a factor of three.. diluted with water and passed through a conditioned strong anion exchange (SAX) solid phase extraction (SPE) cartridge stacked on top of a conditioned carbon black SPE cartridge. the number of sample clean-up steps is reduced to approximately 10. tomatoes. Inc. which limits the number of samples to 8-10 per day. Cymoxanil passes through the SAX cartridge and is retained on the carbon black cartridge. It protects from spore germination and fungal growth by its strong adhesion to leaf and stem surfaces. I. which has been developed by the United States Environmental Protection Agency (USEPA) Office of Prevention. selectively eluted. It shows that by automating the sample preparation procedure. for use in the testing of pesticides and toxic substances.spexsampleprep. For the analysis of famoxadone. ground-up samples are weighed into extraction jars. Cymoxanil and Famoxadone Analysis For the analysis of cymoxanil. Revision 2. to extract various pesticide residues from different kinds of plant materials and to identify and quantitate the active ingredients by LC/MS/MS. “Analytical Method for the Determination of Famoxadone and Cymoxanil Residues in Various Matrices. allowing for the analysis of up to 16 samples per day. SPEX SamplePrep LLC. Each column is washed with additional 10% ethyl acetate/90% hexane (v/v). and the acetonitrile layer containing cymoxanil is passed through a SAX SPE column. which limits sample throughput to typically 8 samples per day. Summary The high-throughput analysis of pesticides has been hindered by the slow and laborious sample preparation stage. AMR 3705-9. Using traditional clean-up procedures. but is also applied to grapes. Robert Thomas. Order Online 24/7: www. It is then selectively eluted off the cartridge and the concentrated cymoxanil residues are dissolved in a hexane/ethyl acetate mixture. The plant matrix is then allowed to settleout and liquid extracts are filtered and collected in mixing cylinders containing sodium chloride. laid out in DuPont 13753 -“Analytical Method for the Determination of Cymoxanil and its Metabolites in Leafy Vegetables Using LC/MS” (3). significantly reduces the number of clean-up steps. shaken. For cymoxanil. so the eluent is passed directly into an LC/MS system for analysis. and concentrated into a methanol/water mixture adjusted to pH 3. test data must be submitted to the Agency for review under Federal regulations and dictates that average recoveries have to be 70-120% with a coefficient of variation (CV) or RSD of less than 15%. The methodology follows OPPTS 860-1360 Multiresidue Test Method (1). Pesticides and Toxic Substances (OPPTS). The mixing cylinders are capped. E. Scientific Solutions Sample Preparation Sample preparation for pesticide residue analysis has typically followed DuPont Report No. the acetonitrile fraction is concentrated to approximately 2 mL and carefully taken to dryness. A modification to this procedure.com 163 . the acetonitrile aliquot is back extracted with hexane. Cymoxanil is retained. Florisil. followed by the addition of water to allow them to re-hydrate prior to extraction.spexsampleprep. The resulting solutions are passed through silica SPE cartridges. reconstituted in acetonitrile and water and analyzed by LC/UV. samples are extracted using an acetonitrile/water mixture as described in DuPont Report No. resulting in an increased sample throughput over traditional approaches. In this procedure. The aqueous phase is discarded. Curzate® and Tanos® to control various fungal diseases in crops. Curzate is a fungicide that contains cymoxanil as the active ingredient and is mainly used for late blight potatoes.com 162 Order Online 24/7: www. NaCl is added to an aliquot to separate the aqueous phase from the organic phase. Samples are filtered and analyzed by HPLC with UV detection. This study evaluates a new approach using an innovative laboratory tissue homogenizer.. Separate acetonitrile aliquots are taken for cymoxanil and famoxadone analysis. The typical pesticide residue set at DuPont contains 8 samples and usually takes an 8 hour workday to complete. The residue is dissolved in 10% ethyl ether/90% hexane (v/v) and passed through a glass chromatography column packed with a layer of sodium sulfate.

NJ).0 mL by adding acetonitrile. Due to the strength of the vertical shaking motion of the equipment. Cymoxanil. will lead to better confirmation of the parent molecules. The Geno/Grinder is a laboratory mill and tissue homogenizer specifically designed for vigorous vertical shaking of deep-well titer plates.0 mL in an HPLC vial with mobile phase. These species are then compared to reference spectra/data in order to produce unambiguous identification of the biomolecules of interest. particularly when small amounts of sample are being analyzed. The ability to switch between both modes is very important. which means the laborious process of cleaning the homogenizer probes is eliminated. In this mode. This instrument is coupled with an HPLC system to first separate the biological species of interest. separated by another 164 Order Online 24/7: www. Foster City. quadrupole. The samples were than extracted by shaking at high speeds in a Geno/Grinder at approximately 700-1200 cycles per minute.spexsampleprep. which is used in the mass resolving mode. molds. steel balls were added to the samples to pulverize the plant material. This technique. the first quadrupole is used in a mass.com Order Online 24/7: www. proteins. to collect both the molecular and fragmented information. which is slightly pressurized by the introduction of a collision gas like hydrogen or helium. Sample material that can be prepared includes bacteria. The collision cell is also used in the rf-only mode. There is no question that the higher number of daughter or fragmented ions that are being identified. roots.Section 3 : APPLICATION NOTE SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis APPLICATION: Pesticide Residue Extraction SP022 Section 3 : SP022 APPLICATION NOTE SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis APPLICATION: Pesticide Residue Extraction Geno/Grinder® To further reduce the clean-up steps. This is especially important when analyzing data from an LC separation. leaves. To ensure complete extraction of the compounds from the plant material. seeds. It was originally designed to prepare plant tissue for extractions of nucleic acids. Once identification is made in the MRM mode. The application of this tool can be expanded to include microorganisms when small silica beads are used instead of steel grinding balls.resolving mode to select the precursor ion. quantitation of unknown samples is normally carried out in the SIM mode. Experimental To evaluate the efficiency of the sample prep and clean-up stage described above. depending on the sample. cymoxanil. based on their elution times off a column. a new piece of technology was evaluated. The second quadrupole (or pressurized multipole collision cell) is used to produce fragmentation of the precursor or parent ion. many seeds and other forms of plant tissue can also be pulverized dry in plates with the help of one or two grinding balls per well. over a period of 20-30 seconds. yeasts. For this reason it is very important to be able to switch very rapidly between SIM and MRM mode. for example. steel balls and a buffering agent together in each well of a titer plate. The sample extract was brought to 50. stems. and certain animal tissue. and analyzed directly by LC/MS/MS. but this time no collision gas is flowing. in order to maximize the amount of data being generated. The principle of this technology is based on confirmation of a particular molecular ion by the generation of its daughter species using collisionally-induced dissociation or fragmentation (4). commonly known as multiple reaction monitoring (MRM). Another benefit of this technology is that additional time savings are achieved because the sample vials are disposable. The final quadrupole is used in a mass-resolving mode to provide mass analysis of the resulting fragmented or daughter ions. uses two resolving quadrupole mass filters. All samples generated were analyzed using the API 5000 LC/MS/MS (Applied Biosystems. The LC/MS/MS instrument used for this study is shown in Figure 2. In the MS/MS mode. Using the Geno/Grinder has cut down the number of clean-up steps to 3. the first quadrupole is typically used in the rf-only mode.spexsampleprep. The eluent is then introduced into the mass spectrometer for ionization to identify and quantitate the species using triple quadrupole MS technology. were determined in a number of wet and dry crop/plant materials. the active ingredient in many of the fungicides. which is an aliphatic nitrogen compound with a formula of C7H10N4O3 and molecular weight of 198 typically elutes off the column after 10-15 minutes. Microbes can also be disrupted in standard 96-well titer plates as opposed to deep-well plates. 10 g of sample was extracted twice with 20 mL of a 90/10 mixture of acetonitrile/water solution. for positive and unambiguous identification of these species. The benefit of the MS/MS design is that it can also be used in MS mode for quantitation purposes. Sample Clean-Up Using the Geno/Grinder For the leaves of watery crops like tomatoes and potatoes. and its various metabolites. and other constituents by shaking the tissue. as a wide bandpass filter to transmit molecular ions of a wide mass range. Approximately 1 mL of the extract was filtered and 100 μL of sample diluted to 1. compared to 20 with the AMR 3705-95 method and 10 with the DuPont 13753 method.com 165 . CA). called the 2000 Geno/ Grinder® (SPEX SamplePrep. Metuchen. so the cell is just used to transmit ions to the last quadrupole. using strong anion exchange (SAX) and the solid phase extraction (SPE) process described earlier.

Confirmation of the compound is then made by measuring the intensities of the fragmented daughter ions in the MS/MS mode. A brief summary of the HPLC and LC/MS/MS conditions are shown in Table 1.spexsampleprep.0 and 10.2. the relative intensities of the fragmented ions were measured using the MRM mode. 1.spexsampleprep. Brief Summary of the HPLC and LC/MS/MS instrumental conditions used for this study Figure 4. HPLC System: Agilent 1100 Series HPLC Settings: Injection Volume: LC Column: Column Temperature: Mobile Phases: 40 μL Agilent Zorbax® XDB-C8 (15. Peak area was used for quantitation.5.01 M Acetic Acid and Acetonitrile LC/MS/MS System: Applied Biosystems API 5000 LC/MS/MS Settings: Ionization Source Polarity: Mode: Monitoring Mass/Charge: Elution Timeframe: Electrospray Negative Selected Ion Monitoring (SIM) and Multiple Reaction Monitoring (MRM) 197 Daltons (Cymoxanil. The LC/MS/MS instrument was operated in single ion monitoring MS negative ion mode for quantitative analysis.0 cm x 4. The MRM spectrum for cymoxanil showing the fragmented ions 166 Order Online 24/7: www. while the resulting calibration curve for 0. 5. which corresponds to the cymoxanil.01 ppm cymoxanil LOQ Fortification Sample (DuPont .com 167 . The MS/MS spectrum (60. It can be seen very clearly that there is a significant peak eluted at about 15 minutes.d. M-1) 0-17 min Figure 3. Elution of cymoxanil using the LC/MS mode Table 1.6 mm i.300 Daltons) of cymoxanil in MRM mode is shown in Figure 4. For confirmation of the presence of the analyte in unknown samples.13753) and control (blank) in the SIM mode is shown in Figure 3.com Order Online 24/7: www. 5 μ) 30°C 0. 0.0..Section 3 : APPLICATION NOTE SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis APPLICATION: Pesticide Residue Extraction SP022 Section 3 : SP022 APPLICATION NOTE SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis APPLICATION: Pesticide Residue Extraction Instrument Methodology Reversed-phase liquid chromatography was used to separate cymoxanil and its metabolites from the rest of the extractants. by comparing them to known ratios in a data base of pesticides.0 μg/L is shown in Figure 5. A 0.

oily and acidic crops for the active ingredient together with its metabolites. the following Geno/Grinder sample preparation and clean-up procedures were used for comparison purposes with traditional sample preparation methods.4 (n=5) Geno/Grinder (% Recovery) 78 ± 3. almonds (oily crop) and wheat straw (dry crop) and achieved similar spike recoveries and precision values.Section 3 : APPLICATION NOTE SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis APPLICATION: Pesticide Residue Extraction SP022 Section 3 : SP022 APPLICATION NOTE SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis APPLICATION: Pesticide Residue Extraction Results The LC/MS separation of the experimental new insecticide under investigation and its metabolites (A-G) are shown in Figure 6.5 (n=2) DuPont-13753 (% Recovery) 93 ± 3. 0. which states that test data must have average recoveries between 70-120% with a precision of less than 15% RSD.2.0. The LC/MS separation of the experimental compound (DuP-1) and its metabolites (A-G) Table 2: % Recovery data and RSD for a 0. 5. Although they will not be presented here. dry. This methodology was then used to analyze a variety of wet.4 (n=4) 68.1 (n=6) 78 ± 6. It shows quantitative data (ppm in sample) for the experimental new compound and one of its metabolites (D).5.50 ppm (10xLOQ) reference samples Sample Preparation Once the methodology was optimized for the separation and quantitation of cymoxanil. Figure 5. Reference Value 0.com The MRM (1-298 Daltons) of a 0.0 µg/L cymoxanil Table 2 shows % recovery data and RSD for a 0. The basis of this method was then used to investigate an experimental new insecticide (DuP-1) and to identify and quantitate its active ingredient and metabolites in various wet/dry plant and crop materials • • • • • • 168 Extract twice with Acetonitrile/H20 in Geno/Grinder for 2 minutes at 1200 cycles/min Dilute 1ml of extract to 5ml with H20 (adjust to pH 2. Order Online 24/7: www.7 (n=5) 89 ± 2.0 and 10.spexsampleprep.9 (n=4) Figure 6. Table 3 compares the Geno/Grinder sample preparation and clean-up method with a traditional homogenizer (Tissuemizer® probe) sample preparation using Dupont-13753 methodology described earlier.05 ppm and 0.spexsampleprep.50 ppm (10xLOQ) AMR-3705-95 (% Recovery) 84 ± 3.0ml Filter through PTFE membrane into an LC vial Analyze by LC/MS/MS Order Online 24/7: www.com 169 . Calibration curve for 0. showing that DuP-1 and all its metabolites are within the guidelines stated in EPA OPPTS 860-1360 Multiresidue Test Method for testing of pesticides and toxic substances. the study also looked at other crops including limes (acidic crop). for various crop samples. Table 4 shows spike recovery and RSD data for one of the watery crops (tomato).50 ppm reference samples. 1.05 ppm (LOQ) 0.2 ppm standard of the metabolites D and E together with a tomato sample spiked at the LOQ is shown in Figure 7.05 ppm (LOQ) and 0.5) Filter through SAX SPE and collect extract Dilute extract to 10.5 ± 1.

003 0. Douglas.A.002 0.009 Geno/Grinder Method 15. AMR 3705-95: “Analytical Method for the Determination of Famoxadone and Cymoxanil Residues in Various Matrices.0 107+6. 1696-1704 (1995) DuPont .5 98+ 1. Literature Cited Table 3.003 Geno/Grinder Method 0.14 N/D N/D N/D 0. Office of Prevention. Analytical Chemistry. The MRM of a 0. Figure 7. rugged and high throughput analytical method. W.spexsampleprep.13753 Method 0.com Order Online 24/7: www. sample throughput was increased by a factor of 3.Section 3 : APPLICATION NOTE SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis APPLICATION: Pesticide Residue Extraction SP022 Section 3 : SP022 APPLICATION NOTE SP022: The Benefits of the Geno/Grinder for Pesticide Residue Analysis APPLICATION: Pesticide Residue Extraction Table 4.4 0. 13753: “Analytical Method for the Determination of Cymoxanil and its Metabolites in Leafy Vegetables Using LC/MS” 4) B.J.1 76+ 4.8 82+ 6.2 ppm standard of the metabolites D and E (top) together with a tomato sample spiked at the LOQ (bottom).5 82+ 6. provides an extremely efficient. Compared to the traditional sample preparation.8 97+ 7. Comparison between the Geno/Grinder and DuPont-13753 sample preparation methods for a variety of wet and dry crop samples Crop Alfalfa Corn Stover Cucumber Green Onion White Straw 1) Environmental Protection Agency. Hager. Thomson. D.” 3) DuPont Report No.6 101+6.0 85+ 4. Joliffe. Corr.002 DuP-1 (ppm) Metabolite D (ppm) 170 Order Online 24/7: www.0075 DuPont .8 83+ 8. The transition is shown at a molecular weight of 1-298 Daltons.6 860-1360 “Multiresidue Test Method for Pesticides and Toxic Substances” Conclusion It has been shown that the extraction of pesticide residues with the Geno/Grinder and identification and quantitation of its active ingredients and metabolites using LC/MS/MS.8 78+ 8. cleanup and detection methods.1 100+9. A. J.012 0.022 0. C.9 77+ 9. from 8 samples to 24 samples per day. Spike recovery and precision data for tomatoes showing that DuP-1 and all its metabolites are within the guidelines stated in EPA OPPTS 860-1360 Multiresidue Test Method % Recovery & RSD of LOQ Sample % Recovery & RSD of 10xLOQ Sample DuP-1 Met A Met B Met C Met D Met E Met F Met G 78+ 4. 67.13753 Method 14.7 93+ 4.7 0. Pesticides and Toxic Substances (OPPTS) Method 2) DuPont Report No.5 113+7.com 171 .spexsampleprep. Improved collisionally activated dissociation efficiency and mass resolution on a triple quadrupole mass spectrometer system.002 0.J.0015 0.6 80+ 5. J.15 N/D N/D N/D 0.

05 and Enviroquant G1701 BA Ver.0 m x 0. To the strawberry and apple samples. 172 Order Online 24/7: www. SPEX SamplePrep.0 minutes. strawberry and apple contained Flutianil. the measured pesticide concentration was greater when the Geno/Grinder was used to shake the samples. samples of strawberry. recovery of the pesticide Etoxazole increased 35%. Following this treatment. a lab worker can shake a sample approximately 200 times in one minute. and anhydrous Magnesium Sulfate (75 mg/ml sample) and the tubes were capped. GC-MS results of samples prepared using both methods were compared. GC-MS Conditions An HP 5890 gas chromatograph coupled to a 5972 mass selective detector was used for the analysis of the samples. homogenized strawberry. Experimental Sample Preparation Mason jars of frozen. To the green pepper samples. Lea Anderson-Smith. In this study. apple. 6. the QuEChERS method1 (quick. Method 2 – Mechanical Mixing Two angle cut ceramic cylinders (3/8” x 7/8”) were added to each tube in Sample Set B. The samples were analyzed by GC-MS using a SIM method. rugged. at 1500 spm. and green pepper (a blend of bell and non-bell) were obtained from UC Davis (IR-4 Project). 18% and 20 % respectively. Results and Discussion The results are shown in Table 1 and graphically in Figure 1. Set A was shaken manually. The GC oven temperature program was set to an initial temperature of 70º C for one minute. while Set B was shaken mechanically using the Geno/Grinder. To each sample was added Primary Secondary Amine (PSA. For pepper. Sample Set A was shaken by hand for 30 sec. For all three matrices. University of California. 6. mixing should be more thorough than can be achieved manually and it is not surprising that extraction is improved over the manual method. The MS was operated in electron impact ionization in the SIM mode a scan range of 35-450 m/z.spexsampleprep. The Geno/Grinder is a mechanical disrupter that grinds and mixes materials using a rapid vertical motion.25 mm x 0. and raised to 230º C at 20º C/min with a total run time of 15. The jars were thawed at room temperature prior to measuring out 15 g samples into 50 ml centrifuge tubes. The supernatant liquid was again removed from each sample and transferred to a clean 15 ml centrifuge tube.com 173 . The GC-MS was equipped with an HP 7673 GC/SFC injector.5 g Sodium Acetate were added.Section 3 : APPLICATION NOTE SP023: Comparison of Pesticide Extraction in Agricultural Products APPLICATION: QuEChERS/Pesticide Extraction SP023 Section 3 : SP023 APPLICATION NOTE SP023: Comparison of Pesticide Extraction in Agricultural Products APPLICATION: QuEChERS/Pesticide Extraction Comparison of Pesticide Extraction in Agricultural Products Using a Manual Shaking Method and Mechanical Mixing with the Geno/Grinder With kind permission of: Matt Hengel..spexsampleprep. Graphitized Carbon Black (GCB. applied to the crop in the field. all samples from Sets A and B were centrifuged at 3500 rpm for 3 min. Samples were evaporated to near dryness using a slow stream of nitrogen gas and gentle heating. easy. At a setting of 1500 strokes/min. All samples were centrifuged at 3200 rpm for 30 sec. safe) has proven to be effective and convenient for analysis of multiple pesticides in agricultural products. cheap. and green pepper) was shaken by hand for 1 minute. Each sample set consisted of 5-7 samples.0 g Sodium Chloride were added. and green pepper contained Etoxazole. Patricia Atkins. Sample Set B was shaken on the Geno/Grinder for 30 sec. apple. The analytes were separated on a HP-5 capillary column (3. The tubes were capped and shaken on the Geno/Grinder at 1500 strokes/min (spm) for 1 minute. Both of these fruits contained the pesticide Flutianil.0 g anhydrous Magnesium Sulfate and 1. 25 mg/ml sample). Due to the more rapid and vigorous agitation using the Geno/Grinder. The QuEChERS method has allowed analysts to process a greater number of samples in a shorter period of time than with previous methods. An aliquot (12-13 ml) of the supernatant liquid was taken from each sample and transferred to a clean 15 ml centrifuge tube. ABSTRACT Since its introduction in 2003 by Anastassiades and Lehotay et al. To each tube was then added 15 ml Acetonitrile containing 1% Acetic Acid. The total volume of each sample was brought to 1 ml in toluene and an internal standard mix (SPEX CertiPrep: CLPS-190) was added. A and B. Order Online 24/7: www. effective. samples are shaken in a complete up and down motion 1500 times during a one minute run. The increase in recovery was similar for apple and strawberry. B. This indicates that use of the Geno/Grinder improves pesticide extraction from the fruit or vegetable matrix.01.com Method 1 – Manual Mixing Sample Set A (from each material: strawberry. both sample sets were visibly lighter in color. Increasing concern over the health effects of residual pesticides on fruits and vegetables has led to increased testing of these products to determine the levels of pesticides on produce when it goes to market.0 g anhydrous Magnesium Sulfate and 1. apple. Each fruit or vegetable contained a known pesticide. The GC-MS interface and MS source were both 250º C The injected volume of sample extract was 2 µL with splitless injection. 5 mg/ ml sample). Chemstation B. In contrast.25 µm).02. and green pepper were prepared for analysis using both the standard QuEChERS method and a modified method involving mechanical mixing using the Geno/ Grinder. Davis. SPEX CertiPrep Clean Up After mixing. All sample tubes were capped and the samples of each fruit or vegetable were divided into two sets.00 were used for the data collection and analysis of samples.

In 2003. The ceramic cylinders mash and grind the fruit or vegetable matrix further during the shaking process. Stajnbaher. Anastassiades. while offering faster and easier handling over previous methods. While a lab worker can shake 2-4 samples (50 ml tubes) simultaneously by hand. J. 2) apples – dense and tough. the QuEChERS method for pesticide analysis was introduced by Anastassiades and Lehotay et al. and Safe and allows for analysis of multiple pesticides. Dev. As a worker becomes tired from shaking multiple samples. While celery is not as dense as apple. However. (ppb) Std. since the operating rate and run time can be set on the Geno/Grinder. the Geno/Grinder can accommodate 16.8 2.spexsampleprep.S. and celery were purchased from a local supermarket and cut 174 Order Online 24/7: www. QuEChERS method developed by the USDA Eastern Regional Research Center. Effective. If two are more people are preparing samples. The tubes are capped and shaken by hand for one minute to mix the contents and extract the pesticide into the solvent. Again.4 7 12 10 20 18 35 An additional benefit of using the Geno/Grinder for sample preparation is elimination of variation in shaking technique. shaking conditions can vary and this can affect how well the samples are mixed. much of the produce sold in the U. the Geno/Grinder was employed to homogenize the fruit/vegetable samples and to mix the produce rapidly and thoroughly with the salts and solvent in an effort to improve the extraction step.0 0.com 175 . use of the Geno/Grinder allows for greater sample throughput. RSD (%) Increase using Geno/Grinder (%) Strawberry Apple Pepper 20 9 17 1. liquefied substance using the Geno/Grinder (grinding method described below). (ppb) Std. M. Also.01 “Determination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate.Section 3 : APPLICATION NOTE SP023: Comparison of Pesticide Extraction in Agricultural Products APPLICATION: QuEChERS/Pesticide Extraction SP023 Section 3 : SP024 APPLICATION NOTE SP024: Pesticide Anaylsis: Standard QuEChERS vs Modified Method APPLICATION: QuEChERS / Pesticide Extraction The addition of two ceramic grinding cylinders to each tube shaken on the Geno/Grinder also may have aided the extraction process. Finally. he/she will likely slow down and later samples may not be as well shaken as earlier one. Matrix Conc. such as acetonitrile. p. and analyzed by GC/MS or LC/MS. Apples are tougher and denser and.com Order Online 24/7: www.spexsampleprep. thereby increasing surface area and allowing a more complete extraction of pesticide from the matrix.J.7 1. not surprisingly. RSD (%) Conc. SIJ. For a typical analysis. The samples are then treated with clean up materials. In fact.AOAC International 86. the matrices in the samples shaken on Geno/Grinder visibly appeared more thoroughly ground than samples shaken by hand. Comparision of GC-MS Results for Samples Prepared Manually and Using the Geno/Grinder Manual Geno/Grinder Introduction Pesticide residues in agricultural food sources are widely considered to cause adverse health effects when consumed by humans. Cheap. a longer grinding time was required to effectively mash the fruit to an applesauce-like consistency. Thus. Experimental Three fruit and vegetable matrices were chosen for the purpose of evaluating materials with differing density and toughness: 1) strawberries – soft. Dev. With kind permission of: Lea Anderson-Smith. and 3) celery – fibrous. Easy.5 5 9 15 24 11 23 1. when samples are shaken manually. Lehotay. Patricia Atkins. Rugged. QuEChERS is an acronym for Quick.4 2. Samples are held vertically in a foam support and every sample within a run is subjected to the same shaking conditions. In this study. SPEX CertiPrep Table 1. 1.” In Europe. is imported and concern over pesticide levels in these fruits and vegetables in comparison to those grown domestically has resulted in increased testing for pesticide residues. manual QuEChERS method. the official method is EN 15662. there is also the possibility that the workers will not shake the samples in the same manner. SPEX SamplePrep. 10-15 g samples of chopped and homogenized agricultural produce are placed in 50 ml centrifuge tubes and an extracting solvent. 412-431 (2003). F. Fresh strawberries. more samples can be prepared in a given amount of time. concentrated. In particular. apples (Granny Smith). Schenck. it is fibrous and tough and therefore difficult to grind effectively. The goal of the study was to determine whether the use of the Geno/Grinder during the extraction step would increase pesticide recovery over the traditional. The QuEChERS method is now widely used and has been adopted by the AOAC as method 2007. Analysis of Pesticides in Fruit and Vegetable Products using a Standard QuEChERS Method and a Modified Method Involving the Geno/Grinder. identical conditions from run to run are ensured. D. this can affect the effectiveness of the extraction. Strawberries are quite soft and preliminary tests verified that they could easily be ground to a mushy. and anhydrous magnesium sulfate and sodium acetate or sodium chloride salts are added.

1. addition of the full 15 ml of solvent prior to grinding provided too much fluid and the grinding media were not able to make sufficient contact with the produce to achieve effective grinding. During preliminary test runs. total). and 15 ml acetonitrile containing 1% glacial acetic acid. but some visible chunks remained. the supernatant removed. and the celery extract a very saturated green color. shaken on the Geno/Grinder for 30 sec. the strawberry samples were well ground to a pulpy. Primary secondary amine (PSA) (25 mg x Vol (ml) supernatant) and graphitized carbon black (GCB) (5 mg x Vol (ml) supernatant) were added to each tube.1 g quantities. After 2 min. Without solvent.1 g) were collectively transferred into a single-serve blender and homogenized to a smooth consistency. 6 g anhydrous magnesium sulfate. The tubes were capped and gently shaken by hand for 15 sec. mushy consistency. it was found that addition of a small amount (5 ml) of solvent improved the grinding process by aiding the movement of the produce in the tube. Thus. weighed out in 15. Each sample was spiked with 250 µl of a 40 µg/ml solution of CAL-CARB-13 (a mix of 13 common pesticides available from SPEX CertiPrep) in dichloromethane (10 ppm per sample).1 g of chunked strawberry.5 g anhydrous sodium acetate. measured. liquid consistency. it was determined that addition of 5 ml of solvent was optimal for effective grinding of a 15 g sample. The supernatant liquid was removed from each tube. using the Geno/Grinder. the apple extract was pale yellow. The liquid in the strawberry tubes was observed to be pink in color. and the celery extract a very saturated green color. fruits and vegetables tended to become packed down in the bottom of the tube and effective grinding was difficult to achieve.com Order Online 24/7: www. and 15 ml acetonitrile (1% glacial acetic acid) were added to tubes containing 15. of grinding at 1500 rpm the strawberry was fairly well ground. measured.com 177 . at which point the strawberry was very well ground and thoroughly mixed with the salts and solvent. All tubes were then centrifuged at 3500 rpm for 3 min. The tubes were capped and clamped on the Geno/ Grinder. Modified QuEChERS Method using the Geno/Grinder – All-In-One Additional samples of spiked strawberry were handled in a second manner. Through experimentation. then centrifuged at 3200 rpm for 1 min. and concentrated down to near dryness (approximately 100 µL) by gently heating the tubes while passing a slow stream of nitrogen over the sample. When the salts were combined with small chunks of produce.5 g anhydrous sodium acetate. placed back on the Geno/ Grinder and shaken for 1 min. at 1500 rpm. The tubes were capped and placed into a tube holder. impact of the grinding media on the produce was impeded and only partial grinding was achieved. a tube was filled to capacity and the produce and grinding media could not move freely. Samples of 15. To each tube was then added 6 g anhydrous magnesium sulfate. Modified QuEChERS Method using the Geno/Grinder To centrifuge tubes containing spiked produce samples were added 3 ceramic grinding cylinders (3/8” x 7/8” angle cut) and 5 ml acetonitrile containing 1% glacial acetic acid. The tubes were capped and shaken by hand for 1 min. Traditional QuEChERS Method The spiked strawberry samples from four centrifuge tubes (each containing 15. pesticide after this step) and transferred into 15 centrifuge tubes. Attempts to combine the homogenization and extraction steps for apple and celery were less successful. the apple extract was pale yellow. The liquid in the strawberry tubes was observed to be pink in color. The samples were centrifuged. then centrifuged at 3200 rpm for 1 min. To each tube of homogenized produce was added 6.spexsampleprep. transferred to a clean 15 ml tube (all methods). The tubes were recapped. The sample tubes were capped and shaken by hand for 30 sec. taking care to control the flow of pesticide solution onto the fruit/vegetable sample. The pesticide mix was introduced into each tube by syringe.. After grinding for 2 min. and divided into two equal samples (5 ppm max. The supernatant liquid was removed.Section 3 : APPLICATION NOTE SP024: Pesticide Anaylsis: Standard QuEChERS vs Modified Method APPLICATION: QuEChERS / Pesticide Extraction SP024 Section 3 : SP024 APPLICATION NOTE SP024: Pesticide Anaylsis: Standard QuEChERS vs Modified Method APPLICATION: QuEChERS / Pesticide Extraction into 1/4-1/2 inch-sized chunks. and clean up was conducted as above. and placed into 50 ml round-bottomed LDPE centrifuge tubes. The samples were ground an additional 2 min. and ground at 1500 rpm. to ensure an even distribution of the pesticide solution over the entire sample. 6 min. The samples were then centrifuged at 3500 rpm for 3 min. Alternatively. (4 min.0 g anhydrous magnesium sulfate. In an effort to determine whether the pre-homogenization step can be eliminated for soft fruits. Toluene was added to each sample to bring the total sample volume to 1 ml. 1. In many cases a viscous drop of material settled to the 176 Order Online 24/7: www. 1. The samples were placed in a refrigerator at 4°C and stored overnight. the supernatant was removed from each sample. and divided into two equal portions (5 ppm maximum pesticide per sample after this step) and transferred into 15 ml centrifuge tubes.. Since apple and celery are tougher materials.1 g were re-measured from this mixture and transferred back into the same centrifuge tubes. grind times at 1500 rpm were required to achieve a well ground. Care was taken to transfer out liquid as well as solid material. The sample tubes were capped. the harder Preparation of Samples Following clean up and centrifugation.spexsampleprep. Apple and celery samples were spiked and homogenized in the same manner as the strawberry. PSA (25 mg x Vol (ml) supernatant) and GCB (5 mg x Vol (ml) supernatant) were added to each tube.5 g anhydrous sodium acetate. and the remaining 10 ml acetonitrile (1% glacial acetic acid). at 1500 rpm. All material was well mixed and free-flowing. clamped in place on the Geno/Grinder.

8 6.4 3.6 2. the green bars (All in one) show the results for the samples that were ground and mixed with the salts and acetonitrile simultaneously (no pre-homogenization). After extraction and centrifugation.8 3. The poorest recoveries were obtained for Dichloran and Chorothalonil.1 2.4 2. while for standard QuEChERS samples a pale yellow drop was observed.8 1.2 Celery Geno/Grinder QuEChERS Geno/Grinder All in one QuEChERS Geno/Grinder QuEChERS Carbofuran Carbaryl Diphenylamine Chlorpropham Dichloran Chlorothalonil Pirimicarb Vinclozolin Metalaxyl Parathion Systhane Azinphos-Methyl *ND = Not Detected ND* ND ND 0. each sample was divided into two and the maximum concentration of each pesticide in a sample at this point was 5 ppm.5 1.6 2. Results and Discussion At the beginning of the study. For celery.5 0.1 2.2 ND 0.2 3.1 2.1 1.2 3. than the samples that were ground on the Geno/Grinder before addition of the salts.8 1.3 0. Because the method used in this study was not optimized for a particular type of pesticide. Therefore.1 ND ND ND 1.8 ND ND 0.9 3. or in some cases better.9 1.4 2. For all pesticides detected.spexsampleprep.1 2.2 1.4 Sample Analysis Samples were analyzed using an HP 5890-GC with a CV-5 capillary column and a 5972-MSD detector.5 3. This was the case for all matrices evaluated. for celery Chlorothalonil was not detected. the samples ground simultaneously with the salts and solvent (All in one)performed as well. 10 ppm of each pesticide was introduced into each produce sample. Interestingly.1 1.2 1. each sample was spiked with 250 µl of a solution of 13 pesticides.2 2. This indicates that this method is viable for soft produce matrices.8 2.9 1. Thus.com 179 . The material appeared to be soluble in aqueous solvents. In fact.0 0. Recovery results for all three produce matrices are shown in Table 1 as total concentration recovered in ppm.4 ND 1. The toluene solution was removed by syringe and injected into GC sample vials.0 1.3 1.1 ND ND ND ND 1.0 3.8 2.0 3.7 0.9 2.1 Apple 1.0 ND 0. For strawberry the residue was red for the samples that had been prepared using the Geno/Grinder and yellow for samples prepared using the standard QuEChERS method. the residue was golden for Geno/Grinder samples and brown for standard QuEChERS samples.5 2.33 1.4 3. Table 1 – Recovery of Pesticides in Produce Samples (ppm) Pesticide Strawberry 2. Figure 1 – Recovery of Pesticides in Strawberry Samples 178 Order Online 24/7: www.3 2. Scan range was 35-450 m/z with signal-to-noise of 3:1.3 1. the supernatant was removed and divided into two equal replicates to continue the study.8 1.0 3. even when the Geno/Grinder was used. significantly higher recoveries were obtained for the samples prepared using the Geno/Grinder than for those prepared by hand.8 2.7 0. The blue bars represent the samples that were prepared by manually shaking homogenized samples with the salts and acetonitrile.3 3. a yellow residue remained for Geno/Grinder samples.7 0. it is not surprising that some pesticides were not stable under the conditions used.com Order Online 24/7: www.3 ND ND ND 0.3 3.Section 3 : APPLICATION NOTE SP024: Pesticide Anaylsis: Standard QuEChERS vs Modified Method APPLICATION: QuEChERS / Pesticide Extraction SP024 Section 3 : SP024 APPLICATION NOTE SP024: Pesticide Anaylsis: Standard QuEChERS vs Modified Method APPLICATION: QuEChERS / Pesticide Extraction bottom of the centrifuge tube after addition of toluene.9 1.7 1. Finally. each present in a concentration of 40 ppm/ml. Injected sample size was 1 µl. Results for strawberry are shown graphically in Figure 1.4 1.9 2.4 1.spexsampleprep. while the residue material was left in the tube.2 0.2 3. In the case of apple.4 1. The red bars represent the samples that were homogenized using the Geno/Grinder prior to the addition of the salts. but not in non-polar solvents and had a syrupy consistency.

which is greater than the 5 ppm that was introduced to the sample. eliminating variability. the Geno/Grinder shakes a tube in a complete up and down cycle 1500 times. Greater recoveries were obtained for all detected pesticides when the Geno/ Grinder was used to grind the apple and mix the resulting pulpy mass with the salts and acetonitrile. In addition. but also grind the produce. In addition to improved pesticide recovery. for soft produce matrices. Again.8 ppm) was also higher than for the other pesticides for these same samples. it is not surprising that extraction was more effective. the recovery is on par with Metalxyl and Systhane for samples prepared using the Geno/Grinder.spexsampleprep. with the exception of Azinphos-Methyl where the recovery for the two methods was similar. the Geno/Grinder method outperformed the standard manual method.com 181 .Recovery of Pesticides in Apple Samples Results for celery are shown in Figure 3. whereas a maximum of four tubes were shaken by hand at one time. the recoveries for the Geno/ Grinder samples are much higher than for the manually prepared samples. thus increasing sample 180 Order Online 24/7: www. Figure 3 . Particularly noteworthy in the case of celery is Vinclozolin. Diphenylamine is commonly used in crop protection for apples and the high concentration for this pesticide is likely a result of its presence on the apple before the addition of the pesticide spike. Thus. angle-cut grinding cylinders. During the clean-up step. the Geno/Grinder accommodated twenty-four 15 ml tubes. but was completely undetected in the standard QuCEhERS samples.spexsampleprep.com Order Online 24/7: www. since run time and operating rate are automatically controlled by the Geno/Grinder. For most pesticides. the Geno/Grinder extracted some pesticides that were not detected in the samples prepared by hand. Figure 2 . while a maximum of six were shaken manually. These aid in mixing the sample thoroughly with the solvent and salts. it may be possible to eliminate the pre-homogenization step. twelve 50 ml tubes were shaken simultaneously on the Geno/Grinder. whereas a human can shake a tube about 200 times in 1 minute. The recovery for this pesticide using the manual method (3. During a 1 minute run at a setting of 1500 rpm. the use of the Geno/Grinder increases throughput since a greater number of samples can be homogenized and extracted at one time.Section 3 : APPLICATION NOTE SP024: Pesticide Anaylsis: Standard QuEChERS vs Modified Method APPLICATION: QuEChERS / Pesticide Extraction SP024 Section 3 : SP024 APPLICATION NOTE SP024: Pesticide Anaylsis: Standard QuEChERS vs Modified Method APPLICATION: QuEChERS / Pesticide Extraction Figure 2 shows the recovery results for apple.Recovery of Pesticides in Celery Samples It is clear from the preceding graphs that use of the Geno/Grinder significantly increased pesticide recovery in this study. However. For all three matrices evaluated.2 ppm. The Geno/Grinder can also shake up to sixteen 50 ml centrifuge tubes in one run. In this study. the sample tubes run on the Geno/Grinder each contained 3 ceramic. thereby further reducing sample preparation time. Since the Geno/Grinder shakes the samples so much more vigorously and rapidly than can be accomplished by hand. the Diphenlyamine results from the Geno/Grinder samples gave a recovery of 6. Conclusion Produce samples of varying density and toughness were evaluated and in all cases significantly greater pesticide recovery was obtained for samples prepared using the Geno/Grinder than for samples shaken manually. As with strawberry and apple. the results for the Geno/Grinder samples were significantly higher than for the standard QuEChERS samples. Nevertheless. ensuring a thorough extraction of the pesticide. all samples within a run and from run to run are shaken in a consistent manner. the recoveries were similar to those obtained from the strawberry samples. In addition.

After the samples have been capped. such as strawberries. Sample Extraction Samples are prepared using a 96 well 1ml assay block. Finding a quick method in which DNA could be extracted and used for PCR is essential. Centrifuge for 1 min to bring all liquid to the bottom of the assay block. Add neutralizing extraction buffer and seal the assay block with sealing film.Section 3 : APPLICATION NOTE SP024: Pesticide Anaylsis: Standard QuEChERS vs Modified Method APPLICATION: QuEChERS / Pesticide Extraction SP024 Section 3 : SP025 APPLICATION NOTE SP025: Lysing / Homogenization APPLICATION: DNA Extraction from Rice Seeds throughput. DNA can be further purified with clean-up kits available on the market. # 2100). Next. Yields The total concentrations yielded from the samples range from 3-7ng/µL in a final volume of 200µL with purities of 1. add one seed to each well. possibly eliminating the need to pre-homogenize the produce. This not only reduces time spent on sample preparation. but also reduces fatigue for laboratory workers. Dispense one 5/32” stainless steel bead (4mm) into each well using the Grinding ball dispenser (SPEX SamplePrep cat.5-1. grind them in the Geno/Grinder2000 (SPEX Sample Prep 2000-115) at 500 strokes/minute for two minutes. 182 Order Online 24/7: www. Quick DNA Extraction from Rice Seed (Wet) With kind permission of RiceTec Inc. Centrifuge again for 1 minute. Conclusion The method described above is sufficient for PCR and it takes less time than the standard chloroform extraction.com 183 . Finally. Soft fruits. Total time ranges from one to two hours.8. Described below is a quick “dirty” method that produces a high enough concentration of DNA that can be used for PCR.spexsampleprep.spexsampleprep. Dispense extraction buffer into each well and securely cap each well. Transfer 300µL of the supernatant to a clean 96 well plate. Alvin TX ABSTRACT DNA extractions can be a very time consuming and tedious process.com Order Online 24/7: www. Incubate the samples in about 1” of water at 95ºC for 20 minutes then place them on ice for approximately 10 minutes or until samples are cool to the touch. can be ground in the presence of the salts and extracting solvent used in the QuEChERS method with no negative impact on pesticide recovery. produce samples can be ground in 50 ml centrifuge tubes using the Geno/Grinder. Centrifuge the samples for 10 minutes at 3000rpm.

the cylinder can crack or break. To this end the roughly pre-ground sample can be pre-cooled in the grinding vial or poured into it already cooled. and N. which can be very tough. ash analysis after incineration of domestic waste samples gives information about the remaining residues that have to be disposed of. The quantity to be ground in a 6751 Vial can vary from less than half a gram up to four or five grams. The optimum sample size and quantity for your samples should be determined empirically.V. grinding can take anywhere from 1 minute to 10 minutes. Depending on the quantity and size of the bone pieces. wet or dry.H. if the impactor is deflected sideways or wedged against the polycarbonate cylinder by a large piece of bone. In order to use this domestic waste in a useful way it is burned in waste incinerating plants to gain heat combustion. The impactor must be able to move freely back and forth. of the waste sample can be calculated and thus ascertained if and how much fuel has to be added for optimum combustion in the incinerating plants.H. and the joints between the end plugs and steel cylinder should be sealed by a piece of Teflon plumber’s tape wrapped around the shank of each end plug. 184 Order Online 24/7: www. the impactor can jam. Brittleness Through Cooling The Freezer/Mill (a cryogenic mill) is effective where these grinding processes fail. To grind bone in the standard 6751 vial. Apart from polymer synthetics and organic substances like cork.V.com 185 . The quantity of sample per load and the size of the sample pieces can heavily affect the grinding efficiency of the mill. The obtained powders displayed good particle size and homogeneity. we recommend the use of the 6752 steel center cylinders. (gross and net heat value) is of interest. particularly with bone. If the 6751C polycarbonate center cylinders persist in cracking or breaking. or smaller. we recommend cutting it before grinding into pieces approximately 5 mm in diameter. A simple test is to load the vial. The variable composition does not allow the use of a traditional ball mills or swing mills.minute grinding periods separated by 2 minutes of cooling. depending on the toughness of the sample and the size of the pieces.spexsampleprep.V. and this includes all bone: fresh or aged. For bone in the 6751 vial we recommend at least 10 minutes of Pre-Cool time. As the Freezer/Mill is driven magnetically there is no wear and tear on moving parts. Freezer/Mill grinding vials are immersed in liquid nitrogen (LN) before and during grinding. and N. This cycle was repeated three times. Results Cryogenic grinding with the Freezer/Mill showed good results with the homogenization of domestic waste.H. Grinding times longer than 2 minutes should be split into 2.Section 3 : Application Note SP002: Ginding/Homogenization :: APPLICATION: Domestic Waste SP002 Section 3 : HT001 How To Subject: Grinding Bone in the Freezer/Mill Preparation of Domestic Waste for Elemental Analysis With kind permission of IBU-tec GmbH & Co. Flexible materials like plastics and biological samples embrittle at liquid nitrogen temperatures.H. Grinding can be speeded up by increasing the grinding rate from the factory setting of 10 to as much as 14 or 15. The sample is hermetically sealed in the grinding vial and immersed in liquid nitrogen. first to make the sample brittle enough to grind. If the sample pieces are too large or there is too much sample in the vial. KG HOW TO Guidelines: Cryogenic Grinding of Bone in SPEX SamplePrep Freezer/Mills Any plant or animal tissue can be ground in a SPEX Freezer/Mill. Non-Uniform Composition As well as the elemental analysis the G. or not move far enough to grind effectively. then shake it back and forth to make sure the impactor can move from end to end of the vial. wood. In extreme cases.com Order Online 24/7: www. To this end the waste has to be ground and homogenized as well as possible. The actual grinding is done by a rod-shaped steel impactor that is magnetically shuttled back and forth between two steel end plugs. Cutting mills could possibly grind these samples but not to the particle size necessary for organic elemental analysis. suitable for elemental analysis. After 20 minutes of pre-cooling the sample was ground for three minutes.spexsampleprep. For the best possible grinding results the sample has to be cooled to the optimum. Finally. These do not form a tight seal with the end plugs when chilled (as do the polycarbonate cylinders). and then to keep it brittle during the actual grinding. followed by one minute of ‘inter-cooling’ to ensure good brittleness and then ground further. It may be possible to grind one or two large pieces of bone at a time – for example. so cross contamination is eliminated. a 2-gram chunk in one end of the vial – but the uniformity of the results will be better and there will be much less risk of cracking a cylinder if the bone is cut into smaller pieces first. and paper there may be inorganic materials and metals present.V. Success in Freezer/Mill cryo-grinding depends on two main things: The sample must be cold enough to be brittle. With sulfur analysis information regarding a possible environmental impact can be gained. Domestic waste presents a very inhomogeneous mix made up of very different substances. Following the results of organic elemental analysis the G.

all components of Freezer/Mill vials can be cleaned with hot water and detergent or soap.com Order Online 24/7: www. com. After adding the reagent the grinding vials were placed in upright position into liquid nitrogen until the buffer solidified. or 732-549-7144 x465. snap-frozen in liquid nitrogen and stored at -80°C. Preparation The RNA was subsequently purified using a phenol-chloroform extraction method according to the producer’s protocol. 523Grinding Procedure / Homogenization For technical reasons. 2 to 2. Erlangen. For further advice about Freezer/Mill applications and maintenance. Germany) used for further preparation had already been added to the samples (approx. With the multi-vial adapter option up to four samples can be homogenized simultaneously in the Freezer/Mill® 6850. This assured sufficient cooling and therefore optimum brittleness.spexsampleprep. Total RNA was isolated from cartilage tissue and the activity of certain genes was analyzed via PCR or micro array analysis. 20ml). to let the sample and coil cool back down. pre-cut the sample into smaller. the samples were held at about -196°C for another two minutes. or grind for additional cycles. autoclaving. and decontaminated by dipping in a solution of 10% bleach or dilute mineral acids. peqLAB. Thus the whole procedure took 12 minutes. Bone will probably remain “grindable” for many minutes of continuous grinding.—due to the large surface area and the small particle size the cartilage powder showed a tendency to thaw quickly. Human Cartilage Tissue Knee cartilage tissue samples were taken from various patients as well as healthy probands. Then the cartilage samples and the impactor were added to the cooled vial.. To this end the expression profile of various genes in the tissue of healthy and diseased probands was compared.HOW TO Guidelines How To Subject: Grinding Bone in the Freezer/Mill Section 3 : HT001 Section 3 : SP005 Application Note SP005: DNA/RNA Extraction :: APPLICATION: PCR The large 6801 vial can grind up to 40 or 50 grams of bone. Generally speaking. The grinding rate can be left at the factory setting of 10 or increased until the impactor starts to “stutter. and for a large sample we recommend 15 minutes of precooling. and steel cylinders. the Freezer/Mill was started briefly to check the movement by listening to the sound of the mill. alcohol. which should be absolutely avoided (RNA degradation)—the phenol-chloroform reagent (peqGold RNAPure™. 10 minutes of pre-cooling for the 6751 vial and 15 minutes of pre-cooling for the 6801 vial ought to be enough for bone. please call Customer Service at 1-800-LAB-SPEX x465. the size of the sample pieces.” the maximum effective rate for the 6801 vial to run smoothly is usually 12. but for very large pieces of bone in the 6801 you may need to increase the pre-cooling time to 20 minutes.spexsampleprep.com 187 . Between grinding cycles samples were cooled for two minutes to achieve optimum brittleness again. and the size of the pieces is not important unless they are large enough to prevent the impactor from moving. grinding should be programmed for two minutes on and two minutes of cooling for as many cycles as necessary to grind the bone to the desired particle size range. 186 Order Online 24/7: www. In order to guarantee optimum RNA clean-up and quality the resulting liquid phase was applied onto RNeasy midi columns. more uniform pieces. As with the 6751 vial. the 6801 vial usually takes longer to grind a sample than the 6751 vial. may be sterilized by disinfectants. By utilizing the precool function of the 6850.5ml). It is possible to run the Freezer/Mill continuously. One to two grams of these samples were taken for RNA extraction and added frozen to the grinding container. The grinding was done in three cycles of two minutes each at maximum frequency. etc. decrease the overall sample quantity. However. RNA Extraction from Cartilage Tissue Using Cryogenic Grinding With kind permission of ALTANA Pharma AG The object of the study was to determine if there is a connection between the seriousness of arthritic diseases. The resulting powder was transferred into Falcon tubes and charged with more peqGOLD reagent (approx. In order to assure that the impactor not be frozen onto the reagent. Again. After cleaning they should be dried. we recommend running the Freezer/Mill for 2 minutes per grinding cycle with 2 minutes of cooling between cycles. Polycarbonate cylinders can be damaged by excessive heat (as in autoclaving) or exposure to organic solvents including alcohol. it is probably better to keep them as cold as possible during grinding. Steel impactors and end plugs. but should not be left in contact with water and aqueous fluids for any length of time. You can also contact us via email at sampleprep@spexcsp. especially of the knee joint and certain genes. as magnetic steel can rust under these conditions. Grinding performance in the Freezer/Mill is affected by the quantity of sample. To improve performance. but as the coil heats up it becomes less efficient. and grinding time. but for difficult-to-grind samples like synthetic fibers and polymer sheets.

the samples were analyzed either by quantitative PCR after reverse transcription or alternatively with the Affymetrix GeneChip® system. Results All in all very good homogenizations of the rice husks were obtained. this assembly is then placed into the coil assembly within the mill.spexsampleprep. After rinsing with water they were again rinsed with 70% alcohol. Grinding is accomplished by alternating the magnetic field in the coil assembly forcing the impactor into the end caps. Preparation of Rice Husks for the Analysis of Their Contents With kind permission of IBU-tec GmbH & Co. This impactor is inserted into the vial along with the sample to be ground. To this end the filled vial is inserted into the opening of the coil assembly and immersed into a liquid nitrogen bath. Cool Grinding The Freezer/Mill has a magnetically driven impactor. then with soap suds. B3 and K the husks also contain important minerals (calcium. the bran and the germ are removed. As well as the vitamins B1. Yield of cartilage RNA was between 2 and 20 μ/g RNA depending on the patient’s samples. i. The low temperature causes brittleness of the material and any generated heat. B2. zinc).com 189 . which is lowered into the liquid nitrogen bath.e. This was shown by the fineness of the resulting powder (analytical fineness) on the one hand and the analysis results which exhibited good reproducibility on the other hand. It has been known for a long time that this can cause deficiency diseases. which corresponds to a grinding time of nine minutes. Prior to the next use the whole grinding set was autoclaved. This cleaning process should always be carried out promptly as the thawing phenolreagent corrodes the vials (the stainless steel accessories are not affected). which would have impeded effective grinding. The grinding vials were cleaned in several steps. using the large grinding vials. selenium. For the purpose of content analysis the rice husks were ground and homogenized in the Freezer/Mill® 6850. With the Freezer/Mill 6850 this can be done in units of a few grams. then after waiting for one minute to renew good brittleness. All in all three of these cycles were performed. almost everywhere the rice is eaten as white rice (polished). Outlook The Freezer/Mill has proved to be very suitable for milling and blending of slightly brittle yet flexible plant parts for analysis. Therefore the husks can be considered as a resource.Section 3 : Application Note SP005: DNA/RNA Extraction :: APPLICATION: PCR SP005 Section 3 : SP006 Application Note SP006: Milling/Blending (Homogenizing) :: APPLICATION: Plant Parts After photometric examination of the RNA. For this kind of grinding program approximately eight grams of starting material was used.spexsampleprep. KG For a very large number of the global population (approximately 50%) rice is the primary foodstuff. magnesium. 188 Order Online 24/7: www. The most important aspect for a successful grinding procedure is the sufficient cooling of the milling material to ensure brittleness of the sample. is avoided. People in Asia and Africa virtually exist only on rice. it was ground again. For brittleness the sample was left in the nitrogen bath for approximately 12 minutes. especially avitaminose (Beri-Beri). Health Aspect However. First they were cleaned mechanically with tissue paper and 70% alcohol. Subsequently the sample was ground for three minutes. As a result of this there are incredibly large rice crop areas especially in Asia.com Order Online 24/7: www.

Section 3 :

SP007

Section 3 :

SP007

Application Note SP007: Grinding/Homogenization :: APPLICATION: Polymer Yams & Fleece Materials

Application Note SP007: Grinding/Homogenization :: APPLICATION: Polymer Yams & Fleece Materials

Grinding Polymers for Qualitative and Quantitative Analysis
With kind permission of the Federal Institute for Materials Research and Testing (BAM)

B) Material Analysis: INOC-Test
Depending on the stabilizer content, about 200 to 400mg of sample material and 10.0mg of AIBN (initiator) are weighed accurately into the reaction vessel. 10.0ml of Cumol is then added with a pipette. The vessel is connected to the oxidation apparatus (see fig.) The Cumol efficiently extracts the stabilizer contained in the pulverized fleece material permitting AIBN oxidation. The INOC Test measures time dependent oxygen consumption during the reaction. From the data obtained, a diagram is generated enabling visual evaluation of the stabilizer content in the samples.1)

In the application discussed here, the 6750 Freezer/ Mill® was used for grinding compact synthetic (pellets, webbing fabric, textiles, etc.) as well as polymer yarns, fleece material, filaments (polypropylene (PP), polyethylene or polyester). Grinding was required for accurate qualitative and quantitative analysis of additives contained in synthetic materials (e.g. antioxidants using HPLC and INOC-Test). The Freezer/Mill is ideal for this application, providing the required particle size reduction in a relatively short time period.

Conclusion
The 6750 Freezer/Mill efficiently reduces the particle size of samples that are difficult to grind without thermal degradation of the material, for example fleece materials to a particle size of less than 500μm. Sample preparation time is drastically reduced to less than 15 minutes due to the increased brittleness of the samples at these very low temperatures.

Example: PP Fleece Materials
The material is first cut into approximately 2mm squares. The grinding vials are then filled half way with sample; then ground as per the program below: Pre-cooling : 15 min Run : 1.5 min Cycle cool : 2 min Cycles : 5 Rate : 10Hz For the analysis discussed here, the method above was found to be the optimum grinding program for PP fleece materials. The yield is high (80% - 90%) and during the short grinding times the material does not warm enough to lose its brittleness or decompose. The number of grinding cycles is dependent on the quantity of sample placed in the vial and the desired final particle size. In order to exclude particles that are too coarse the ground fleece material can be sieved, for example passed through a 500μm sieve.

Apparatus:
Valve Capillaries

Pre-set level (constant pressure)

A) Sample Preparation for HPLC Analysis of Additives
Approximately 2.0g of the ground material is weighed into a 125ml flask to an accuracy of 1mg and 40ml toluene is added. The sample is brought to a boil with constant stirring. After approximately 30 minutes the material has completely dissolved, the solution is than slowly cooled to 50°C. In order to precipitate the polymer, 40ml of methanol is added with further stirring. The mixture is then cooled to room temperature and filtered through a Nutsche (suction) filter. The filtrate is then passed through a 0.45μm filter. The stabilizers necessary for analysis are now in solution and ready for oxidation and HPLC separation.
Water bath

Flexible tubing

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Section 3 :
Application Note SP008: Structural Changes in Polymers :: APPLICATION: Polymer Blending

SP008

Section 3 :

SP009

Application Note SP009: Reduction/Homogenization :: APPLICATION: Polymers

Structural Changes in Polymers by Means of Cryogenic Grinding
With kind permission of Prof. Dr. U. Köster, Dept. of Chemical Engineering , University of Dortmund

Nafion®-Powder for the Production of Fuel Cell Electrodes
With kind permission of DLR (German Aerospace Center) Stuttgart; Electrochemical & Electrical Engineering

One goal in materials research is to develop new synthetic materials with characteristics that cannot be accomplished by the usual smelting process, as the polymers tend to separate during the heating process.

Pure Polymer
Trials to introduce permanent changes in polymers by means of Cryogenic Mechanical Milling (CMM) with the Freezer/Mill® were started with two polymers; isotactic polypropylene (iPP) and syndiotactic polystyrol (sPS). After melting and re-crystallization, both cryogenically ground (i.e.at–196°C) polymers showed characteristics that differ from the original polymers. DSC (Differential Scanning Calorimetry) tests showed changed crystallization temperatures, which indicates reduced molecular weight or a change in molecular weight distribution. The longer the samples were subjected to cryogenic grinding the bigger the change. Further experiments showed that the crystalline structure is increasingly destroyed during cryogenic grinding. Presumably CMM leads to chain fission and therefore to the formation of macro radicals. This can lead to cross-linking and an increased amorphic content in the partially crystallized polymers. Another explanation would be the formation of nano structures, small fragments of the original polymer compounds.

The Freezer/Mill®, a cryogenic mill is useful where other grinding procedures fail. Flexible materials like synthetics and biological samples are embrittled at Liquid Nitrogen temperatures. The sample is hermetically sealed and cross contamination is impossible. Since the Freezer/Mill is driven magnetically there is no wear and tear on the movable parts.

Special Polymer
Nafion® a polymer similar to Teflon (perfluorosulfonate polymer), which has been used for over 30 years as a proton conducting membrane in fuel cells, serves as an electrolyte. Because of its properties it proved very suitable for this application. The DLR has now developed a method to apply the Nafion in powder form. For the production of this Nafion powder, the Freezer/Mill, a cryogenic mill is utilized. As a polymer Nafion is very flexible and soft which obviously makes milling difficult. The Nafion granules (5mm particle size) are reduced to approx. 10μm during grinding. The resulting powder is mixed with a catalyst and sprayed dry onto to the 25 - 175 μm thick membrane.

Compounds
As well as the pure polymer results the behavior of cryogenically ground polymer compounds is, of course, very interesting. When mixing the two polymers iPP and sPS through melting (extrusion) separation occurs. Such polymer blends are dispersions of one part within the other. Some CMM sample tests suggest that re-combination of constitutive different macro radicals partly results in co-polymers. These copolymers could act as phasing facilitators between the incompatible blending components of iPP and sPS. Evidence of this is the altered morphology of CMM blends. Here the DSC experiments also showed changed crystallization behavior. More graphic are the morphology light microscopy pictures. While, after melting and re-crystallization, the extruded samples show morphology characteristics for roughly separated polymer blends, in a CMM sample the iPP is finely distributed within the sPS.

Fuel Cell
The fuel cell generates electrical output through electro-chemical oxidization of hydrogen into a proton and an electron as well as oxygen reduction as counter reaction. In order to reduce the necessary activation energy for this reaction a catalyst has to be used. In the PEM-MC (Polymer- ElectrolyteMembrane-Fuel Cell) platinum is used as a catalyst. The direct methanol fuel cell needs ruthenium as a catalyst in addition. These polymer membranes are utilized in various fuel cells.

Result (Conclusion)
Despite the special properties of Nafion, which as a polymer is very soft and flexible, it was possible to obtain a very fine powder after a combined grinding time of 20 minutes with the freezer/mill. No particle size determination was carried out, although because of the thickness of the applied layer the maximum particle size can be specified as less than 25μm.

Conclusion
CMM using the Freezer/Mill causes changes to structure, thermal behaviour and morphology of homopolymers and polymer compounds. While morphological differences through melting and recrystallization are partly reversible, structural changes remain. Aside of chain fission and the resulting macro radicals, cross-linking and reduced crystallization level has been observed. Polymer blends produced by CMM show a considerably improved dispersion of both polymers within each other. Exactly this changed degree of dispersion gives reason to hope for new materials with new and perhaps even predictable characteristics.
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Section 3 :
Application Note SP015: RNA Extraction :: APPLICATION: Molecular Effects of Pollution

SP015

Section 3 :

SP015

Application Note SP015: RNA Extraction :: APPLICATION: Molecular Effects of Pollution

Molecular Effects of Pollution in Cetacean Samples Using the Cytochrome P450, CYP 1A1, 1A2, and 1B1 as Biomarkers
With kind permission of Dr. Celine Godard-Codding, Ocean Alliance & The Whale Conservation Institute, Lincoln, MA

Materials and Methods
We have devised the following multi-step approach in preparing our samples and using the SPEX Freezer/Mill. • All SPEX microvials and other utensils used to extract the sample from the Freezer/Mill are autoclaved before use to avoid sample contamination. • The SPEX Freezer/Mill is pre-chilled before the grinding of the samples using liquid nitrogen. • The tissue samples are sliced into smaller pieces to improve the grinding. • Sliced tissue samples are pre-chilled in liquid nitrogen in order to prevent RNA degradation. • The pre-chilled samples are placed into a SPEX microvial and kept in liquid nitrogen until placement into the SPEX Freezer/Mill. • The SPEX Freezer/Mill is topped off with liquid nitrogen and the vials containing samples are put into the SPEX Freezer/Mill. • The following grinding process has shown to be effective in preventing heating the samples. The SPEX Freezer/Mill is turned on for 2 minutes and then off for 1 minute and the cycle is repeated for a total of 10 to 15 minutes of grinding. • Once the samples have been ground, they are kept in the SPEX microvials in liquid nitrogen until further analysis. • Samples are then ready for total RNA isolation by phenol and guanidium thiocyanate extraction.

Ocean Alliance is dedicated to the conservation of whales and the ocean environment through research and education. Ocean Alliance recently completed a fiveyear research voyage around the world known as the Voyage of the Odyssey (2000 to 2005). The Voyage of the Odyssey was launched to address the need for a globally integrated dataset allowing a consistent analysis of exposure to, and potential effects of, persistent organochlorines and other pollutants in marine life. Many marine mammals harbor large fatty reserves in their body where high levels of organochlorines and other lipophilic contaminants can accumulate.Marine mammals are subject to bioaccumulation and biomagnifications of those fat-soluble contaminants due to their relatively long life span and high trophic position within marine food chains. Therefore marine mammals can be considered environmentally relevant candidates for use as sentinel species when assessing marine pollution. The sperm whale (Physeter macrocephalus) was chosen as the indicator species for the Voyage of the Odyssey.A total of 960 sperm whale skin and blubber samples and over 100 samples from predatory fish were collected during the voyage.

Biomarker Project
The toxicology program of the Voyage of the Odyssey encompasses many projects. The biomarker project focuses on the use of the cytochrome P450 1 (CYP1) enzymes. CYP1 enzymes can metabolize and/or activate environmental pollutants, such as polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs). In many animal species CYP1 induction is used as a biomarker of exposure and molecular effects to the above contaminants. We recently validated the CYP1 biomarker in cetaceans (Godard et al., 2004). The goal of our project is the investigation of the molecular effects of pollution in cetacean samples using the cytochrome P450 CYP 1A1, 1A2, and 1B1 as biomarkers. Our methods include isolating RNA sequencing, cloning and quantifying the expression of the 3 CYP genes in sperm whale skin biopsies. The sperm whale skin samples available for this particular biomarker project weigh only between 50-100ug. The amount of total RNA that can be extracted from such small samples is low; therefore we investigated the use of the SPEX Freezer/Mill in order to increase the quantity of total RNA that can be extracted from each sample and its quality.

Conclusion
The SPEX Freezer/Mill has been a substantial asset to our research by allowing the isolation of total RNA from our small tissue samples with improved quality and less degradation than previous techniques.

References

Godard et al. (2004). Induction of Cetacean Cytochrome P4501A1 by -naphthoflavone Exposure of Skin Biopsy Slices. Toxicological Sciences. 80, 268-275.

Dr. Celine Godard-Codding and Carolyne LaCerte

194

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195

Heitjans. equipped with alumina and zirconia vials).Section 3 : Application Note SP003: Nano Technology :: APPLICATION: Production of Nano Powders SP003 Section 3 : SP003 Application Note SP003: Nano Technology :: APPLICATION: Production of Nano Powders Production of Nano-Crystalline Oxidized Ceramics with High-Energy Ball Milling S. LiBO2. Therefore TiO2 has only limited applications in high-energy ball milling experiments. Institute for Physical Chemistry and Electro-Chemistry. For hygroscopic materials the corundum grinding vial was filled in an argon atmosphere and put into an airtight stainless steel container. but a minimum particle size of approx. Particle size was determined by XRD analysis and TEM data. while new lines appear after 4 hours. B2O3. This indicates that the end product of the reaction does not depend on the composition of the mixture but the conditions on the boundary layers. After a short period of time only the lines of the original compounds are detected with XRD analysis.com Order Online 24/7: www. The characteristics of particle size reduction and subsequent growth was similar with all analyzed oxides. The average particle size was determined by the grinding time and subsequently analyzed by means of X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM). was obtained as pure Rutile (without impurities) in smaller particle sizes. The newly formed product was 196 Order Online 24/7: www. Conclusion High-energy ball milling is especially suitable for particle size reduction and the study of subsequent chemical and physical changes. exhibited an elevated proportion of these impurities after grinding. Process 8. Ball milling is particularly suitable for this task as it is easy to use and allows the grinding of a relatively large amount of material as well as a large variety of different materials. When subjected to ball milling Rutile. During analysis of a 50:50 mix of Li2O:B2O3 chemical changes due to this chemicalmechanical procedure were detected. The nano-crystalline samples are metastable and heating led to particle growth. In this study various nano-crystalline materials were produced using a ball mill (8000M Mixer/Mill®. which did not occur with the microcrystalline starting material.spexsampleprep. showed partial phase transformation during the grinding process.com 197 . TiO2 and Li2O:B2O3 mixtures. 20nm was obtained after 8 to 10 hours of grinding. TiO2. comprising additional impurities. Mater. Chemical Reactions Mixing of ceramic components and subsequent pressing produces a heterogeneous material with a multitude of different boundary layers. Particle Sizes The different oxides displayed different grinding characteristics. Prior studies by other groups showed the particular suitability of two-step sintering with a lower temperature during the second step. J. P. which was analyzed by two methods. Bork. which showed the same impurities. This was taken into account during the sintering process when a solid. The lithium containing materials were selected because of their potential use as solid electrolytes. Indris. Anatas. LiNbO3. Some materials showed phase transformations while others showed chemical reactions. Analyzing particle size effects in nanocrystalline materials requires a technique in which one can adjust the particle size. Synth. Heitjans.spexsampleprep. University of Hannover Li2B4O7. This network of different interfaces can be modified by varying the particle size. SPEX SamplePrep. D. TiO2 is interesting with regard to its use as a photo catalyst. 245 (2000) With kind permission of Prof. The analyzed media were: Li2O. compact ceramic was to be produced from the samples. which was shown by DSC. P.

5 Care must be taken when evaporating hexane. Evaporate the solvent on a steam-heated water bath under the hood (Note 5). 3 High oil content samples should be ground in a cutting mill (e. 7 It is customary to report the result as % oil when analyzing corn germ samples. the flask can be weighed and used for solvent evaporation as described later. Always insure that the hood is functioning properly before use. 4 Alternatively. Rinse the vacuum flask residue into the beaker with small portions of hexane.(g)x100 = (Note7) (asis) SampleWt. take care that no hexane is aspirated out of the flask on low oil samples. 2 Filter Funnel: Gleman Cat. operating at 100 °C. Reagents 1 n-Hexane: Reagent Grade or HPLC Grade (Note 2) Procedure Grind a 50-100 g sample to a uniform particle size (10 mesh) in a grinder or cutting mill (Note 3). a cellulose nitrate 5 micron filter which is hexane compatible. 4201 (47 mm) or Cat. Place a filter paper in the funnel and filter the milled sample slurry into a clean and dry vacuum flask (Note 4). Calculation % Crude Fat Dry Extract Wt. 5 Oven: Forced air or convection oven. 3 Filter Paper: Whatman Cat. 2 Hexane is a very flammable solvent and all work should be performed in a well ventilated area with no open flames. 198 Order Online 24/7: www.com Order Online 24/7: www. If the hexane is heated at too high a rate. Add one 12mm and two 6 mm steel balls and 25 mL of n-hexane. Weigh the beaker and calculate the dry extract weight. No. No. Quantitatively transfer the residual oil from the steel milling vial and cap with the aid of three 10 mL portions of hexane.g.Section 3 : How To Subject: Crude Fat (Hexane Extractables) HT002 Section 3 : HT002 How To Subject: Crude Fat (Hexane Extractables) HOW TO Guidelines : Feedstuffs Analysis – Crude Fat (Hexane Extractables) Principle Lipids are recovered by simultaneous milling and extraction with hexane in a sealed ball mill vial. equipped with a Cat. Brinkman Model ZM-1). and wash residual oil from the sample with another three 10 mL portions of hexane. No. Remove the beaker and cool in a desiccator. and both 12 mm and 6 mm steel balls. Special Apparatus 1 Mill: Model 8000 Spex Mixer/Mill. Seal the vial and mill in the Mixer/Mill for 15 mins. Place the beaker with residue in the air oven and dry it 1 hour at 100 °C (Note 6).spexsampleprep. 7195-004. No.(g) 1 The material for extraction should be at or below equilibrium moisture.spexsampleprep. Analytical Methods of the Member Companies of the Corn Refiners Association. the evaporation will occur with occasional violent boiling which will result in the loss of crude fat or oil. if desired. corn germ and other components derived from the milling of corn (Note 1). Inc. 6 Prolonged evaporation or drying of the extract at elevated temperatures may cause fat oxidation and high results. 8001 hardened steel vial for grinding. Transfer the filtered hexane and oil miscella into a dried and tared 150 mL beaker. 4 Bath: Steam-heated water bath in a well ventilated hood. or equivalent. low oil content samples may be ground in a cutting mill or attrition mill.com 199 . Also. Wet materials should be dried by a method which does not result in fat oxidation. 4230 (47 mm). Accepted 4-19-89 Scope The method is applicable to feedstuffs.. Mix the sample thoroughly and weigh accurately about 4-5 g into the steel grinding vial.

16 Bead 5 52.26 1. Metuchen.26 1. sodium.16 Bead 2 52.04 1. Fly Ash Composition (%) using FFB-6705-02 Analyte Average SiO2 Al2O3 Fe2O3 K2O CaO MgO P2O5 TiO2 Na2O SO3 52.08 26.46 2.76 6.52 4.06 1.46 2.47 2.26 1.15 3. Thus.15 3.46 2.com 201 .16 Bead 2 52. and sulfur were present in lesser amounts and comprised the remainder of the fly ash.52 4.52 4.45 2.11 26. at 750° C to eliminate residual carbon (~0. The results for the five beads within a set were then averaged again to obtain overall results for the set.26 1.16 Bead 4 52. Each bead was measured ten times. with the main fusion stage (Step 4) set for 15 minutes at 1035° C.24 0. with the results averaged for each bead.74 6.24 0.74 6.07 26.25 0. and then fused into two sets of glass beads using a Katanax K1 electric fusion fluxer.04 1.11 26.49 4. gently mixed by hand with a plastic laboratory spatula.50 4.spexsampleprep.04 1.80 g of fly ash (a flux/sample ratio of 8:1) were weighed into a Pt/Au crucible. magnesium. phosphorus. titanium.41 1. Slag & Fly Ash Preparation and XRF Analysis of Fly Ash Fused Beads ABSTRACT Fly ash is a waste product from the combustion of coal and is comprised of the mineral particles that rise with the flue gases.26 1.52 4.02 26.08 26.79 6. USA. Since both fluxes produced clear glass beads with the fly ash sample. The results are shown in Tables 1 & 2 as percentage of composition for each analyte.26 1. Table 1.48 2.16 Bead 4 52.16 Analysis The two sets of glass beads were analyzed by ED-XRF.16 3.04 1.04 1.26 1.48 2. indicating that the fly ash sample was homogenous and that the K1 prepares fused beads with a high level of reproducibility.42 1. In addition.46 2.26 1.52 4.09 26. Recovered fly ash is used as a component in certain cement mixes and improves the durability and strength of concrete. In this study. Two different lithium borate fusion fluxes from SPEX CertiPrep were used to prepare five beads with each flux.22 0.02 1.16 Bead 1 52. Complete data for this study are on file at SPEX SamplePrep.16 3.06 1.52 4.14 3. Measured results were also consistent for the ten scans of each bead.50 4. Table 2.50 4.23 0. a sample of fly ash was pulverized and blended.42 1. Five beads were prepared in this manner for each of two fluxes: SPEX CertiPrep FFB-5005-02 (1:1 lithium tetraborate:lithium metaborate with 0. LLC.76 6.50 4.com Order Online 24/7: www. 200 Order Online 24/7: www.05 26.15 3.47 4.24 0. The beads were then analyzed by energy dispersive X-ray fluorescence spectroscopy (ED-XRF) and the results were compared both within a set and between the two sets to evaulate consistency of beads produced using the K1 and effect of flux composition on the XRF measurements.2%).69 6.42 1.43 1.23 0.42 1. Fly Ash Composition (%) using FFB-5005-02 Analyte Average SiO2 Al2O3 Fe2O3 K2O CaO MgO P2O5 TiO2 Na2O SO3 52. NJ.75 6.13 3.25 1.16 Bead 3 52.16 Bead 3 52.26 1.25 0.24 0.06 1.40 g of flux and 0.14 3. it is apparent that the choice of flux composition had no effect on the XRF results.14 3.76 6.06 26.06 1.spexsampleprep.24 0.22 0.42 1. 6.23 0.47 2.43 1.46 2.75 6.48 2. with the major components being silica and alumina. Slag & Fly Ash SP026 Section 3 : SP026 APPLICATION NOTE SP026: Preparation and XRF Analysis of Fly Ash Fused Beads APPLICATION: Cement.26 1. the overall averages from Table 1 and Table 2 are nearly identical.16 Fusion Method The fly ash was roasted in a porcelain crucible for 2 hr.05 1.05 1.14 3. either is appropriate to use with this fly ash.42 1. XRF results show excellent consistency within a set. Oxides of iron. An example for one bead is shown in Appendix 1 and is indicative of results obtained from repetitive scans of the other nine beads.75 6.41 1.41 1.09 26. calcium.5% lithium bromide as a non-wetting agent) and FFB-6705-02 (2:1 lithium tetraborate:lithium metaborate with 0. and fused into a 32 mm glass bead using the K1.43 1.12 26. potassium.15 3.75 6.07 26.5% lithium bromide).15 3.16 Bead 1 52.45 2.25 1.74 6.16 Bead 5 52.Section 3 : APPLICATION NOTE SP026: Preparation and XRF Analysis of Fly Ash Fused Beads APPLICATION: Cement. The fusion program used was a modified version of the K1’s fixed OXIDE program.

05 2.46 3.52 6.26 1.05 2.45 1.47 3.46 1.47 3.15 4.74 Fe2O3 6.71 26.16 202 Order Online 24/7: www.71 26.45 3.08 Al2O3 26.04 52.18 1.53 6.03 2.spexsampleprep.26 1. Analyte Scan 1 Scan 2 Scan 3 Scan 4 Scan 5 Scan 6 Scan 7 Scan 8 Scan 9 Scan 10 Average SiO2 52.27 1. the high degree of bead to bead consistency within a set indicates that the elemental composition of the flux is uniform.81 26.26 1.07 2.26 1.Section 3 : APPLICATION NOTE SP026: Preparation and XRF Analysis of Fly Ash Fused Beads APPLICATION: Cement.07 2.27 1.42 1.16 0.27 1.42 1.15 4.80 26. Fly Ash results for 10 successive XRF scans of Bead 4 prepared using FFB-5005-02.spexsampleprep.14 CaO 3.com Order Online 24/7: www.26 1.42 3.04 P2O5 1.13 4. reproducible glass beads.14 52.com 203 .42 1.04 2.21 1.53 6.24 SO3 0.52 6.14 4.20 1.04 2.51 6. In addition.42 1. Slag & Fly Ash SP026 Appendix Conclusion The Katanax K1 electric fusion fluxer is easy to operate and produces high quality.15 4.09 52.14 4.26 1.21 1.25 1.75 26.04 52.07 52.15 4.16 0.52 6.23 1.42 1.81 26.16 0.46 3.12 4.26 Na2O 1.43 TiO2 1.24 1.26 1.31 1.51 6.16 0.76 26.16 4.67 26.46 Analyte Scan 1 Scan 2 Scan 3 Scan 4 Scan 5 Scan 6 Scan 7 Scan 8 Scan 9 Scan 10 Average MgO 2.47 3. The two fluxes used in this study gave XRF results that indicate that flux choice did not influence the analysis.48 3.71 26.15 4.16 0.46 1.42 1.16 0.51 6.46 3.51 6.52 K2O 4.11 52.07 52.48 3.02 2.24 1.02 2.67 26.52 6.03 2.29 1.16 0.42 1.16 0.05 52.14 52.05 52. Table 3.16 0.16 0.

204 Order Online 24/7: www. Handbook of X-Ray Spectrometry: Methods and Techniques.com Order Online 24/7: www. Sulcek. 2nd ed. Marcel Dekker. and Oliver. 1981. 1989. Inc. Chapter 7.. R. J. Quantitative X-Ray Fluorescence Analysis: Theory and Application. Occasional articles on sample preparation.. Chichester. New York. Or try out our sample preparation equipment in your laboratory for one week. Buhrke. V.... Plenum Press. 245–251. S. P. 1998.com 205 . 1992. Inc. Principles and Practice of X-Ray Spectrometric Analysis. R.com Katanax K1 Prime is only available for local demos. Fernand Claisse. New York.com. with methods for specific types of samples. Editors. Vols. available on CDROM and through the website of the International Centre for Diffraction Data®: www. Glasgow. R. JohnWiley & Sons. G. Boca Raton. Inc. The most thorough. Products Available For Demo: Katanax K1 Prime Electric Fluxer 8000D & 8000M Mixer/Mill 6770/6870/6970EFM Freezer/Mill 2010 Geno/Grinder 8530 Shatterbox 3635 X-Press Contact (732) 623-0465 Email: SamplePrep@spexcsp. Baffins Lane. Marcel Dekker. 1 (1957) to the present. Quantitative X-Ray Spectrometry. D. Z. D. and Markowicz. Bertin. New York.. Much useful information throughout on sample preparation methods and equipment. Quebec. CRC Press.Q. Specimen Preparation. New York.. Van Grieken.3. pgs. essential guide to the theory and practice of borate fusions.. New York. Inc. and Smith.. The annual proceedings of the Denver X-ray Conference. Chapter 13. JohnWiley & Sons.. Jenkins.. Works of a Periodical Nature Advances in X-ray Analysis. Specimen Preparation.spexsampleprep.spexsampleprep. Canada. Sample Preparation for XRF. Authoritative text on all decomposition techniques with many fusion methods given. A Practical Guide for the Preparation of Specimens for X-ray Fluorescence and X-ray Diffraction Analysis. and Povondra. England.. Comprehensive reference for XRF and XRD sample preparation. F. Physics and Chemistry of Borate fusion: Theory and Application.W. P. 1975. with papers on every aspect of X-ray analysis.. X-Ray Spectrometry. and Claisse.. 363–394... H. Once you try our quality products you’ll ask yourself how you ever lived without them. 2004. Best of all. E. G. and Gedcke.. Decomposition Methods in Analytical Chemistry. including sample prepartion. Most of the above publications have detailed bibliographies for further reading. pgs. 1995.. a bimonthly journal published by JohnWiley & Sons Ltd. Minerals and Allied Materials. R.. R. We recommend test samples be sent to us directly to be processed in our demo lab.icdd. JohnWiley & Sons. Inc. Methods of Decomposition in Inorganic Analysis. and Blanchette. A compact. Bock. Many specific fusion methods. A. Jenkins. International Textbook Co....Appendix Would you like to test our sample preparation equipment with your own samples? XRF Sample Preparation: Selected References Reference Books Bennett. practical work about borate fusions.. Section 9. Claisse. Lachance..West Sussex. F. our demo program is complimentary! You only pay shipping and handling to and from your facility. 1979. 1993. Gould. New York. Now You Can With SPEX SamplePrep’s Demo Program Contact SPEX SamplePrep to arrange a test grind in our labs by our experts. XRF Analysis of Ceramics.

Inc.spexsampleprep.®: • • • • Assurance Certi-Strips Claritas PPT Enviro-PT • • • • SPEXertificate SPEX CertiPrep Ltd Triple Checked for Quality VAL-U-CAL Registered Trademarks of International Centre for Diffraction Data®: • ICDD Registered Trademarks of Applied Biosystems: • TaqMan If contamination with certain metals or plastics is objectionable.com Order Online 24/7: www. DuPont de Nemours & Co.Appendix Appendix Trademark References Registered Trademarks of SPEX SamplePrep.: • Delrin • Teflon • Kapton • Vertrel XF Registered Trademarks of DuPont Teijin Films: • Mylar Registered Trademark of Katanax Inc: • Katanax Registered Trademarks of Qiagen: • QIAshredder • DNeasy Registered Trademarks of Roche Molecular Systems and Hoffman LaRoche: • PCR Mail to SPEX SamplePrep. and a report and recommendations will be returned within three weeks. LLC™: • • • • AutoExtractor Bench-Press ElectroFluxer Freezer/Mill • • • • Geno/Grinder Mixer/Mill PrepAid Shatterbox • • • • Spec-Cap UltraBind Ultralene X-Press Questionnaire for test grinding of Samples Up to 3 samples will be ground at no charge.com 207 .com Samples are required to be sent on customers account. 15 Liberty Street. Registered Trademarks of Promega Corporation: • Wizard 206 Order Online 24/7: www.I. excess sample that is considered to be hazardous will be returned. Metuchen NJ 08840 Please contact SPEX SamplePrep before sending in your test sample: 1-732-623-0465: sampleprep@spexcsp. SPEX SamplePrep Mill for Test: _______________________________________________ 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. 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: ______________________________________________________________ Registered Trademarks of E. if known: ______________________________________ Registered Trademarks of SPEX CertiPrep.spexsampleprep.

20-21. 204 Dewar. 97 Usage. 45 Application Notes. 19 Balls. 67 Crucible Tongs. 184-195 Mixer/Mill. 59. Balls. 48 Zirconia. 67 Cryo-­Block. 19-20. 39 Demo Program. 66 Zirconium. 48. 56 Alumina Ceramic. 19 Cleaning Grinding Containers. 48 Composition. 49 Agate. 27 Ceramic Grinding Media. 38-39 Die Sleeve­and ­Plunger. 25 Zirconium. 97 Vial for Mixer/Mill.com 209 . 48 Silicon Nitride.spexsampleprep. Tool Steel. 36 for Mixer/Mill. 21 Certified Reference Materials. 90 Container for Shatterbox. 133-138 Clamp Assembly for Geno/Grinder. Balls. 28-29 Cryogenic Gloves. 60-61. 119 Dies. 25-26 208 Order Online 24/7: www. 97 Vial for Mixer/Mill. 38 Ball Dispenser. 90 Contamination. 55 Auto­Fill System. 196-199 Katanax. 48 Beads. Geno/Grinder. 48 Tungsten Carbide. 114-116 Order Online 24/7: www. 131-132 Cap­-Mats. 140. 86. Evacuable. 146-147 Cryogenic Transfer Hose. 128-129 Platinum. 117-118 Borate Fusion Flux. Agate. 75-76. 111-112 Crucibles Graphite. 52 Grinding Application. 62-63. 62-63. 46 Air-­Actuated Press. 22-23 Cellulose Binder. 92-96 Cryo­Station. 28. 99-100 Composition of Grinding Containers. for Pelletizing. 99. 117-118 Centrifuge Tube Holder. 48 Composition. 56 Binders. for Freezer/Mill. 142-183 Freezer/Mill.spexsampleprep. 44. 75-76. Silica. 98 Cr-­Free Vial. 69-72. 34-35 Critical (Infinite) Thickness. 48-49 Alumina Ceramic. 200-202 AutoExtractor. 16.com Bench ­Press. 90 Usage. 81-84 Chemical Attack on Window Films.Subject Index Subject Index Adapters. 72 Bubble­-Free Insert. 48 Stainless Steel. 38 Cryogenic Grinding. 21. 35 Automated Press. 48 Methacrylate. 76.

130-131 Lithium Borate Fluxes. 97 Vials for Mixer/Mill. 3-4 Hydraulic Presses. 55-58 Infinite (Critical) Thickness. 133. 35 Mills. 52-53 Grinding Key Points. 120. 75. 111-112 Infrared Mulls. 49. 38 Graphite Crucibles. 100-101. Composition. XRF Analysis of. 133 KBr Dies. 111-112 Order Online 24/7: www.spexsampleprep. 62. 56-58 Mechanical Alloying. 72. 3-4 Paraffin Binder. 110 Mulls. 47 Micro X­-Cells. 43-45. 124 Geno/Grinder. 136 Non­Wetting Agents. 126-127 Fusion Machines. 100 Mylar XRF Window Film. 97-101 Hardened Steel. 86 Gloves. 30-32 Fusion. 55-58 Liquid Sample Cells for XRF. 67-68 Motorized Presses. 72.com 211 . 13 Microvial. 124-129 Fusion Fluxes. Cryogenic. 64-65 Freezer/Mill. 104 Methacrylate. 78-80. 130-132 DNA Extraction. Freezer/Mill. 93 Microvial Extraction Tool. 77. 64-65. 78. 59. 40-41 Shatterbox. 75 Edge­Flaring Tool. 126-127 Fluxers. 35-36 Films. 90 How To Order. 63. 48 Usage. 52-53 Usage. 130-131 Liquids. 78.Subject Index Subject Index Dispenser. 97 Vials for Mixer/Mill. 33. 117 Enclosed Shatterbox. 55. 153-155 Dual Mixer/Mill. 102-104 Molds. 64-73. 123 KBr Mulls. 18. 117-118 Particle Size Effects in XRF. 19 Disposable XRF Liquid Cells. 44-46 Hardness of Grinding Container Materials. 50. 76. 80. 40. 132-138 Flux. 128-129 Grinding Aids. 127-128 Ordering Information. 107-108 Extractor & Vial Opener. 19 Manual Presses. 76-78. XRF Window. 69-72. 100 Laboratory Presses. 73. 76-77. 100 210 Order Online 24/7: www. 62. 40-42. Balls.com Kapton XRF Window Film. 98-99 Grinding Containers. 103-104 Edge Flaring Tool. 80. 72.spexsampleprep. 126-127 Magnet. 30-32 Mixer/Mill. 5-6 Mixer/Mills. 50-51 Minimum Orders. 90 Containers for Shatterbox. 92. 54.

33-35 Mixer/Mill. Grinding Media. 132-138 Vial Comparison. 20. 46 Sleeve-­and-­Plunger. 55-63. 60-61. 75-76. 54. 99. 33-35 Vials for Geno/Grinder. 97 Vials for Mixer/Mill. Usage. 185-186 Vials for Freezer/Mill. 110-111. 61-62. 93-95 Vials. 90-91 Grinding Media. 43. Vials for Mixer/Mill.com Return Shipment. 25-26 Resin. 48 Pellets. 74. 59-61. 6 RoHS/WEEE. 62-63.spexsampleprep. 48 Films for XRF. 74-75. 76-78. 87 Usage. 49. of XRF Window Films. 33-34. 20-21 Pre-Filled Grinding Vials. 98-99. Shatterbox. for XRF (Spec­Caps).spexsampleprep.Subject Index Subject Index Pellet Caps. 130 SPEX SamplePrep­Carver Presses. Beads. 46 Polypropylene. 110-123 Propylene Glycol Grinding Aid. 47 Vials for Mixer/Mill. 43-46. 134 Transporter. 22-23 Transmission. 117 PrepAid. 97. 37 212 Order Online 24/7: www. Grinding Media. 79-80. 110-111 Pre­-Flared Spec­Caps. 49. 121. 21 Silicon Nitride. 60 Plastic. 5 Silica Grinding. 52-53. 110-111. 84 Spec­Caps. 45-47 Thin Films for XRF. 90-91 Geno/Grinder. XRF Window Film. 132-134. 107-109 Shatterbox. Liquid. 67-68 Polycarbonate. 83. 35. 54 Order Online 24/7: www. 27. 74-75. 117 Presses. 97 Vials. 116-117. 130-133 Shatterbox. 123 Pelletizing. 97 Platinumware. 76-77 Solid Reference Materials. for XRF. 116-117. 137 Polystyrene. 110 Pressing. 113. 97-98 Powder Samples. Analysis. 23-27 Freezer/Mill. 100. 33-34. 114 Stainless Steel. 54 Rack. 119 Snap­-On Rings for X-­Cells. 102-103 Vials for Freezer/Mill. 50-51. Grinding Containers. 109 Shipping. Comparison.com 213 . Composition. 132-138 Titer Plates. 115-116. 27 Vials for Mixer/Mill. 61. 130 Pellet Dies. 78-79. 34-35 Sample Cells. 110-123 Pellets for Pellet Dies. 43 Polyethylene Vials for Mixer/Mill. 110. 58-59. 24-25. 55-63. 55-58. 110. Preparation for XRF. 74. Center Section. 54 Freezer/Mill. 43-44. 78-80. 49 Usage.

78-80. 107 Container. 97. 146-147. 90 Containers. 132-138 X-­Cells. 68 Pre-filled Vials. 99-100. 52 Vial. 46-47. 74-80. 78-80. 52-53 Pellets. 45. 78-80. 99-100. 110. 90. 43. 132-133. Cr­-Free. 46-47. 60 Usage. 103. 90. 100. 76. 130 Window Films. 110-111. 49. 34-35. 97-98. 54. 55. 117-118. 44. 61-62. Beads. 25-26 Order Online 24/7: www. 130-131 Pellet Caps (Spec­Caps). 47. Balls. 90. 132-138 Yeast Extractions. 48 Composition. Thin Films. 107 Vials for Mixer/Mill. 110. 45. 35. For Freezer/Mill. 76-77. Agate. 93-94 Hardened Steel. 90 Crucibles. 45. 121. 44. Balls. 102 Vials. 44-45. 90. 102-103. 46-47. 90 Container Usage. 21 Composition. 132-138 XRF. 67 Heater Lid. 90. 196 Zirconium. 46-47. for XRF Cells. 86. 196 Warranty. 114 X-­Ray Transmission. 99. 99 Vials Adapter. 97. 36-37. Ultralene XRF Window Film.Subject Index Subject Index Tungsten Carbide. Vertrel XF. 187 For Mixer/Mill. 196 Tungsten Carbide. 90. 44-45 UltraBind.spexsampleprep. 97. 43. 113. 196. 44. 90. 62. 33-34. Silicon Nitride. 116-117. 74-75. 97.com 215 .com Zirconia. 47. 37. 130-138 Liquid Sample Cells. 113. 97 Stainless Steel. 80. 198-199 Plastic.spexsampleprep. 130-133 X­-Press. 79. 49. 151-152 214 Order Online 24/7: www. 48 Composition. 102-103. 6 Window Film. 97. 107 Zirconia. 47. 76-77. 97. 45-47. 47. 90 Racks. 97. 27. Accessories. 102-103. 102-103 Alumina Ceramic. 100.

................................................................................................................................. 3/8 in........................................ 50 mL............................................................... Case of 10................. Tall....................spexsampleprep...................... 22 Cap-Mat for 2210 Titer Plate....... 25 2 mL Tube with 400 μm Molecular Biology Grade Silica Beads....... 24 Pre-Cleaned Polycarbonate Vial Set.................................................................. 23 Cap-Mat for 2230 Titer Plate.............................. 15 mL............................................................................................. x 5/8 in....................... 24 Polycarbonate Vial.......... 24 Polycarbonate Vial.................................................................. 21 Zirconium Grinding Beads. 15 mL........................................ 23 Polycarbonate Vial......................... 22 96-Well Titer Plate................................................................. 5/16 in...................... 27 Holder for 50 mL Centrifuge Tubes................... 5/32 in......... 23 Cap-Mat for 2230 Titer Plate........................................................................ 5 mL........................................................... 15 mL................................... (9.. 200-400 μm.......................... 21 Ceramic Grinding Cylinder........ 800-1000 μm......................................... 28 Holder for 2 mL microfuge Tubes................................. 400-600 μm.......................... 27 Holder for 15 mL Centrifuge Tubes........... 22 Cap-Mat for 2200 Titer Plate............. 23 Frosted Polyethylene Vial............................................................................................................................................... 27 2 mL Tube with 100 μm Molecular Biology Grade Silica Beads......................................... 25 2 mL Tube with 100 μm Acid Washed Zirconium Beads........... 20 Silica Grinding Beads............................................................................................ Case of 100........................................ 200 μm.............. 100 μm.. Molecular Biology Grade.... Short................... 25 2 mL Tube with 1. 800-1000 μm....................... 23 24-Well Titer Plate.........................................................com 2211 2211-10 2220 2220-100 2221 2221-10 2230 2230-100 2231 2231-10 2231-10 2240-PC 2240-PEF 2241-PC 2241-PEF-200 2250 2251PC 2252-PC-30 2253C-48 2253-PC-48 2254-PE-48 2255 2255C20 2255C4 2260 2300 2301-100MB 2301-400MB 2301-800MB 2302-1000AW 2302-100AW1 2302-100AW2 2302-100LB 2302-1400AW 2302-1700AW 2302-200AW Cap-Mat for 2210 Titer Plate............ Square Wells.............................................................................. 23 48-Well Titer Plate....... 22 48-Well Titer Plate....................................... 25 2 mL Tube with 1................... x 7/8 in........................ 27 Large Capacity Clamp Assembly........................................ 21 Low Binding Zirconium Beads........... 27 Holder for 6133PC Vial......................................... 22 Cap-Mats for 2200 Titer Plates............................................................... x 5/16 in.................................................. 5/32 in............................................................................ 20 Grinding Balls....................................... 400-600 μm........................................... 21 Low Binding Zirconium Beads........ 23 Cap-Mat for 2220 Titer Plate............................................................... Case of 100.......................................................................................... 20 Low Binding Silica Beads................................................. 25 Polycarbonate Center Cylinder.......4 mm Acid Washed Zirconium Beads.... 100-400 μm.......................... 19 Grinding Balls... 21 Ceramic Grinding Cylinder...... 25 2 mL Tube with 800 μm Molecular Biology Grade Silica Beads.................................... 20 Low Binding Silica Beads......................... 5 mL.................................................................................................... 24 Cap for 2253-PC-48..........spexsampleprep........ 26 Order Online 24/7: www............... Case of 10........................................... 5 mL....... 22 Cap-Mat for 2220 Titer Plate.................................................................................com 217 ......... 22 Order Online 24/7: www..................... pack of 20......................................................................... 23 Pre-Cleaned Polycarbonate Vial Set......................................... Case of 10................................................................................................. Round Wells................. 21 Low Binding Silica Beads........ 21 Silica Grinding Resin...................................................................... (4 mm......................... 25 Cryogenic Grinding Vial Pack..................................................................................... 26 2 mL Tube with 200 μm Acid Washed Zirconium Beads..............0 mm Acid Washed Zirconium Beads................. 21 Ceramic Grinding Cylinder.. 25 Cryo-Block for 2255 Vial.................................. 25 2 mL Tube with 100 μm Low Binding Zirconium Beads.................. Square Wells.................. 19 24-Pin Magnet.................................................................... 20 96 Pack of 96 Magnetic Tips................................................. 20 Silica Grinding Beads................................ 3/8 in.... (11 mm... 26 2 mL Tube with 100 μm Acid Washed Zirconium Beads.... Molecular Biology Grade..... 23 Cap-Mat for 2230 Titer Plate...................................................................................... Case of 100................................................................. 24 LDPE Vial......................................... set of 2.................................................................. 5 mL....... 19 12 Pack of 12 Magnetic Tips... pack of 4...................................... 20 Separator for 24-Pin Magnet............................................ Case of 10......................................................................................................... 20 Silica Grinding Beads...................... Round Wells........................................ 20 Silica Grinding Beads.................................................................. 7/16 in............ 18 Grinding Ball Dispenser............... 50 mL.................................... Case of 10................ Molecular Biology Grade........ 800 μm..................... 22 96-Well Titer Plate. 20 Grinding Balls....... 100 μm...................................... 21 Silica Grinding Resin..................... 26 2 mL Tube with 1.............. Case of 100.................. 25 Polycarbonate Center Cylinder............. 24 Polycarbonate Vial...............................5 mm...............Product Index Product Index Product Number 2010 2100 2110M 2110M-12 2110M-96 2110S 2150 2155 2156 2160 2161 2162 2165 2166 2167 2168 2170 2171 2180 2181 2182 2183 2184 2185 2190 2196-16-PE 2197 2198-24-PE 2199 2200 2200-100 2201 2201-10 2210 2210-100 216 Product Name Page Number Geno-Grinder.................... 22 96-Well Titer Plate....................................................................................................................................................................................... 21 Vial Rack............... Case of 10......................................................... Case of 10................ 23 24-Well Titer Plate..................................... 19 96-Well Titer Plate............... Molecular Biology Grade......................... 400 μm..... 100-400 μm....................7 mm Acid Washed Zirconium Beads.................. 23 Pre-Cleaned Frosted Polyethylene Vial Set..........................................

... 60 Die Sleeve-and-Plunger Set – 40 mm............................................................................... 78 Mylar Window Film (Roll............................................................................................................................... 78 Order Online 24/7: www............................................................................................................................................................... 79 Polypropylene Pre-Cut Circles 0............ 26 2 mL Tube with Mixed Matrix 1............................................................................................................. 61 33 mm Spec-Cap................ 59 Die Set – 13 mm.............................................................................................................................................. 60 Steel Pellets – 40 mm.. 76 X-Cell......................................... 48 Hardened Tool Steel Vial Set.................................................. 61 Spec-Cap – 33 mm......................................................................... 31 mm Micro X-ray Cell with Collar...... 43 Stainless Steel Ball Set....................... 62 Edge-Flaring Tool..................................... 31 mm Universal Closed X-Ray Cell with Collar............ 44 Kapton® Window Film (Roll.. 27 Polycarbonate Vial........................................................................................................ 78 Mylar Pre-Cut Circles............................................................................................................................................................................. 79 Ultralene® Pre-Cut Circles.. 60 Die Set – 40 mm........................................................................................................................... 75 Spec-Cap – 38 mm............................................................................ 43 Hardened Tool Steel Vial Set..................... 26 2 mL Tube with Mixed Matrix 3............. 59 Steel Pellets – 13 mm............................. 61 30 mm Spec-Cap®.......................................................................................................................................................................................................... 27 Cryo-Station............................ 29 Cryo-Block for Micro-centrifuge or PCR Tubes................................................................................................................................................................................................ 79 Micro-porous Teflon® Film (Roll............................. 77 X-Cell.................................................................................................................... 59 Tungsten Carbide Pellets – 35 mm........................................................................................... 43 mm Closed X-Ray Cell For Horiba Sulfur Analyzers......................................... 75 Edge-Flaring Tool....................................................................................... 77 X-Cell............................................. 26 2 mL Tube with Mixed Matrix 2................................................................ 60 Die Sleeve-and-Plunger Set – 35 mm... 61 Spec-Cap – 38 mm...................................................... 77 X-Cell........................................................................................Product Index Product Index 2302-3000AW 2303-MM1 2303-MM2 2303-MM3 2304-100AW 2304-400AW 2304-800AW 2305-2800SS 2600 2650 2660 2661 2662 2663 2664 2665 2666 3111 3112 3114 3114SB 3116 3116PC 3116PC 3117 3117B 3118 3118A 3119 3127 3511 3512 3515 3516 3517 3518 218 2 mL Tube with 3 mm Acid Washed Zirconium Beads....................................................... 79 X-Cell... 74 Pre-Flared Spec-Cap – 31 mm.......................................................... 74 Order Online 24/7: www................................................................................................................................................................. 29 Polystyrene Vial... 78 Kapton Pre-Cut Circles...............................................................................................................................................................................................................2 mil (5 μm) thick................................................................... 44 Hardened Tool Steel Ball Set........................................................................................... 48 Agate Vial Set.............. 78 Mylar® Pre-Cut Circles (Large.......................................spexsampleprep................................................................................................. 79 Ultralene® Window Film (Roll............................. 75 Die Set – 35 mm........................................................................................... 44 Agate Ball...... 76 Bubble-Free Cell Insert............................... 26 2 mL Tube with 100 μm Acid Washed Silica Beads........................... 29 Cryo-Block for 50 mL Centrifuge Tubes.................................... 28 Cryo-Adapter for Titer Plates....................................... 29 Cryo-Block for 48 Micro-centrifuge or PCR Tubes...... 59 Tungsten Carbide Pellets – 40 mm......... 43 5 mL Polycarbonate Vial........................ 29 Cryo-Block for 4 mL Polycarbonate Vials......com 219 .............................................................................................................. 76 X-Cell................ 31 mm Double Open End X-Ray Cell with Collar........................................................................... 29 Cryo-Block for 4 mL Polyethylene Vials.................................. 62 38 mm Spec-Cap............................................................................................. 29 Cryo-Block for 15 mL Centrifuge Tubes.................... 43 Methacrylate Balls.............................. 31 mm Closed X-Ray Cell........................................8 mm Stainless Steel Balls............................................................................................................................................................................... 48 Stainless Steel Vial Set.... 26 2 mL Tube with 2........................................................... 26 2 mL Tube with 400 μm Acid Washed Silica Beads................................................................................................................................................................................................................................................ 60 Steel Pellets – 35 mm..................................................................................................................................................spexsampleprep..................... 28 Cryo-Block for 15 mL Polycarbonate Vials......................................... 77 Die Set – 10 mm.......................................... 62 38 mm Spec-Cap................................................................................................................................................................................................................................ 48 Polystyrene Vial......................com 3520 3521 3524 3525 3526 3527 3527I 3529 3561 3565 3571 3577 3610 3613 3613ST 3614 3614C 3614ST 3614W 3615 3615M 3615 3616 3616C 3616ST 3616W 3617 3617 3617M 3617M 3618 3618 3619 3619 3619A 3619A Polypropylene Window Film (Roll......................................... 75 Spec-Cap® ........................................................ 78 Mylar Window Film (Roll............................................................................................................................................................... 26 2 mL Tube with 800 μm Acid Washed Silica Beads.......................................................................................................................................................30 mm........................................................................................................................... 40 mm Closed X-Ray Cell......................................................................... 48 Methacrylate Balls......................... 61 31 mm Pre-Flared Spec-Cap............... 61 Spec-Cap – 33 mm.....................................................

........ 60 Edge-Flaring Tool.... 34 Mid-Size Vial Set....................................................... 43 Polycarbonate Vial..... 33 SPEX SamplePrep 6770 Freezer/Mill®.............................................................................................................................................................. 39 Long Cryogenic Transfer Hose.................................................................................... 74 Spec-Cap – 30 mm....... 61 30 mm Spec-Cap...................... 62 PrepAid Paraffin Binder – (CnH2n+2.............................................................................. 50 L Capacity........................................................................... 34 Mid-Size Cr-Free Vial............................................................................................................................. ..................................... 34 Mid-Size Polycarbonate Center Cylinder..................................................................................................................................................................................... 35 Auto-Fill System for the 6870 Freezer/Mill............................................................................................ 57 3622 SPEX SamplePrep-Carver Model M................................................................................................................................................... 34 Extractor/Vial Opener for Large and Mid-Sized Vials................................................................................................. 37 Small Vial Accessory Package.................................................................................................................................................................................................................... 35 Extractor/Vial Opener for Small Vials..................................................................................... 34 Large Steel Center Cylinder.......... 62 PrepAid UltraBind®.................................................................. 25 L Capacity..com 221 .................................................................................. 35 Mid-Size Vial Adapter for 6800-Series Freezer/Mills.................................................................................................................................................................... 42 Polystyrene Vial.................................... 49 PrepAid Propylene Glycol .................. 33 Microvial Sample Extraction Tool................. 37 Large Cr-Free Vial Set..........................................................................................................................Product Index Product Index 3619AM 3619AM 3619M 3619M 3621 3622 3623 3623C 3623ST 3623W 3625 3625 3626 3628 3635 3640 3640 3642-150 3642-450 3644-150 3644-450 3646-150 3646-450 3650 3650 5004 5004A 5004C 5100 6133 6133PC 6134 6135 6751 6751C20 6751C4 220 Pre-Flared Spec-Cap – 31 mm................................................ 54 Tungsten Carbide-Lined Vial Set............................................................................................. 46 Polyethylene Vial........ 34 Large Grinding Vial Set...................................................................... 75 3626 SPEX SamplePrep-Carver 12-ton Press......... 48 Methacrylate Center Cylinder................................................................. 35 Small Poly-Vial Set............................................ 61 31 mm Pre-Flared Spec-Cap............................. 30 Order Online 24/7: www............................................................................................................................................................................................................ 62 PrepAid UltraBind®.................................................... 36 Vial Rack for Large Vials............................................................................................................................................................................ 37 Mid-Size Vial Accessory Package....................................................com 6752 6753 6753C 6754 6755 6761 6770 6771 6781S 6801 6801C20 6801C4 6802 6804 6805 6806 6814 6820 6870 6870L 6870M 6870S 6871 6881 6881C20 6881C4 6883 6884 6885 6886 6900 6905 6906 6907 6910 6970D Small Steel Center Cylinder............ 59 Tungsten Carbide Pellets ................................................................................................................................................................................................................................................................. 39 Portable Pressurized Cryogenic Cylinder................spexsampleprep........................................... 35 Mid-Size Vial Adapter for 6804 Extractor/Vial Opener................................................................................................................................................................................................................ 49 PrepAid Vertrel® XF............................................................. 58 SPEX SamplePrep 3628 Air-Actuated Bench-Press®.......................................... 74 3621 SPEX SamplePrep-Carver Model C.......................... 32 Small Cr-Free Vial Set......... 39 SPEX SamplePrep 6970EFM Enclosed Freezer/Mill®– Dual Grinding Coils................................................................................. 33 Microvial Set...................................... 31 Large Vial Accessory Package..................................................................... 60 Die Sleeve-and-Plunger Set – 31 mm................... 62 Edge-Flaring Tool................................................................................................................................. 58 Die Set – 31 mm....................................................................................... 36 AutoExtractor™ for Freezer/Mill® Vial Sets......... 36 Vial Rack for Small Vials................................................................................................................................................................... 63 PrepAid Vertrel® XF............................................................................................................spexsampleprep................................................................ 38 Short Cryogenic Transfer Hose...................................................................................... 38 SPEX SamplePrep 6870 Freezer/Mill®....... 34 Small Stainless Steel Grinding Vial Set.. 35 Mid-Size Polycarbonate Center Cylinder............................... 33 Small Polycarbonate Center Cylinder............................................... 36 Mid-Size Poly-Vial.......... 33 Small Polycarbonate Center Cylinder..................................... 63 PrepAid Paraffin Binder – (CnH2n+2..................................................................................................................................... 33 Order Online 24/7: www............................................................. 62 PrepAid Cellulose Binder .................. 38 Portable Cryogenic Dewar............................................................................. 34 Large Polycarbonate Center Cylinder..........................................................................................................31 mm....................... 44 Tungsten Carbide Ball Set............................................................................................................................................................................................................................................. 34 Large Polycarbonate Center Cylinder........................................ 56 SPEX SamplePrep 3635 Automated X-Press®.............................. 36 Cryogenic Gloves..................................................................... 54 PrepAid Cellulose Binder ................................................................. 35 Multi-Vial Adapter........................... 44 SPEX SamplePrep 5100 Mixer/Mill®..................... 55 PrepAid Propylene Glycol ... 43 Polystyrene Vial............................... ......................................... 46 Small Grinding Vial Set............... 60 Steel Pellets – 31 mm........................

............................................................................................................................................................................................spexsampleprep...................................................................................................... 64 Katanax® K2 Prime............................................................. 45 Zirconia Ceramic Ball..................................................................................... for 32 mm molds.......... 48 Tungsten Carbide Vial Set......................................... 73 Katanax® K1 Prime................................................................ for 40 mm molds................... 51 Hardened Steel Grinding Container...................................................................................................................................... 49 Order Online 24/7: www........................................................................................................................................ 49 Vial Clamp Adapter for the 8000D Mixer/Mill...................... 49 Clamp for 8003 Vial Set................ 44 Steel Ball Set...........................................................Single Grinding Coil...................................................................................... 68 Mold – 40 mm....................................... 54 SPEX SamplePrep 8530 Enclosed Shatterbox®.............................................................................................................................................................. 50 SPEX Fusion Flux.................... 52 Zirconia Ceramic Grinding Container.......................................................................................................................................................... 52 Alumina Ceramic Grinding Container.................................................... 67 Mold Plate................................................................................... 67 Mold – 35 mm.................................................................. 65 Teflon® Beaker.. for 30 mm molds................................................... 45 Methacrylate Balls... 40 SPEX SamplePrep 8000M Mixer/Mill®..................................................................................................... 67 Rack................................................................................................................. 52 Small Hardened Steel Grinding Container.................................................................................................................................................................... 30 Rack and Tongs............................... 45 Alumina Ceramic Ball..................... 46 Silicon Nitride Ball.............................................. 48 Methacrylate Vial Set............................................................................. 54 Small Tungsten Carbide Grinding Container...................................................................................................... 45 Zirconia Ceramic Vial Set.............................................................. 45 SPEX SamplePrep 8500 Shatterbox®............................................................................................................. 70 Graphite Crucibles......................... 41 Hardened Steel Vial Set......................................................................................................... 71 Graphite Crucibles.............................Product Index Product Index 6970M 7151 7151R 7151T 7152 7152HP 7153 7154 7155 7156 7157 7158 7159 7160 7161 7162 8000D 8000M 8001 8001B 8002 8003 8003A 8004 8004A 8004SS 8005 8005A 8006 8006A 8007 8007B 8008 8008A 8009 8010 222 SPEX SamplePrep 6970EFM Enclosed Freezer/Mill®.................................................... 68 Regular Crucible........................................................................................................................................................ 67 Mold – 32 mm............................................................................................................................................................................................. 46 Multiple-Sample Adapter................................. 67 Heavy-Duty Mold – 35 mm.... 49 Agate Vial Set................................................ 72 SPEX SamplePrep 8000D Dual Mixer/Mill......................... 46 Stainless Steel Ball Set....................................................................... 52 Tungsten Carbide Grinding Container.......................................................................................................................... 68 Order Online 24/7: www............................................. 68 Mold Holder.............................................. 72 SPEX Fusion Flux Additives .................................................. 52 Rack......................................................................................................................... 53 Transporter............................................. 46 Agate Ball........ 68 Mold Holder.............. 71 Graphite Crucibles................................................ 69 Short Tongs......................................... 67 Graphite Crucibles.................................................................................. 48 Silicon Nitride Vial Set...................................................................... 44 Alumina Ceramic Vial Set......... 70 Graphite Crucibles.......................................................... for 35 mm molds........................................................................................................................................................... 68 Mold Holder..............................com 223 .. 67 Long Tongs....................................................... 68 Zirconium Crucible......................................................... 71 Graphite Crucibles.................... 45 Tungsten Carbide Ball.......................................................................................................................................................................................................................... 48 Stainless Steel Vial Set.................................................. 69 Graphite Crucibles......... 66 Mold – 30 mm........................................................................................................................................................................................... 69 Graphite Crucibles...................................................................................................................................................... 67 Graphite Crucibles....... 67 Heavy-Duty Mold – 30 mm.......................................................................................................................... for 35 mm molds...com 8011 8012 8014 8014A 8015 8500 8501 8504 8505 8506 8507 8507R 8508 8521 8525 8530 FFB FFB K1P K2P KP0010A KP0037A KP0038A KP0039A KP0040A KP0049A KP0235A KP1001A KP1002A KP1003A KP1004A KP1005A KP1006A KP1007A KP1008A KP1009A Multiple-Sample Adapter................ 48 Polystyrene Vial....................................................................................................................................................................................................................spexsampleprep.............................................................................................. 67 Heavy-Duty Mold – 32 mm............................................................................................................................................................................................................... 49 Round-Ended Hardened Steel Vial Set............ 70 Graphite Crucibles.................................................................. 53 Large Hardened Steel Grinding Container........................................................................................................................................................................................................................................ 48 Steel-Jacketed Tungsten Carbide Vial Set........... 71 Graphite Crucibles........................................................................................................................................................................... 68 Mold Holder.......................................................... 66 Heavy-Duty Crucible..........................................................................

................ 6-position..... 35mm...............................com ........ 6-position........................................................ 68 Mold holder................................................................... 30mm.... 32mm... 68 224 Order Online 24/7: www... 40mm............. 68 Mold holder...........................spexsampleprep........................................................................ 68 Platinum Crucible Heater Lid............................................................... 68 Mold holder............Product Index KP1010A KP1011A KP1015A KP5603A KP5604A KP5605A KP5606A Heavy-Duty Mold – 40 mm........... 68 Zirconium Crucible Heater Lid....................................... 68 Mold holder....................................... 6-position......................................................................... 6-position..