Microreport the Science and Technology of Small Particles™ M I C R O M E R I T I C S I N S T R U M E N T C O R P O R a T I O N Volume 18 No

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e h t microReport The Science and Technology of Small Particles™ M i c r o m e r i t i c s I n s t r u m e n t C o r p o r a t i o n Volume 18 No. 2

In This Issue Micromeritics Proudly Announces Its Second Micromeritics Proudly Announces Its Second Instrumentation Grant Award Instrumentation Award AutoChem II 2920 Awarded Winner to the University of South Carolina ...... 1 icromeritics re- Mcently launched Micromeritics Appoints New an Instrument Grant Manager of Market Program that is in- Development...... 2 tended to provide particle characteriza- Scientific Theory Posters tion instruments to are Now Available...... 3 non-profit universities and research organi- Micromeritics Extensive zations for the pur- Bibliography Surpasses pose of fostering and 25,000 Downloads supporting meritori- AutoChem II 2920 600 papers added since ous research projects. Chemisorption Analyzer January 2007...... 3 The initial grant was awarded to the Berkeley Catalysis Center at the Pulse Chemisorption University of California-Berkeley. Dr. Alan Katz, the with AutoChem II 2920: principle investigator intends to use the instrument Isopropylamine on Zeolites (an AutoChem 2920) to determine the concentration Guest article by and acid/base characteristics of catalytic active sites Andrew D’Amico...... 4 on solids in a fashion that cannot be accomplished by other techniques. In particular, this will be used What’s New at to investigate the chemisorption of H2, CO, CO2, and Micromeritics Analytical N2O, as well as reactive che- Services ...... 6 misorption using hydrogen and alkanes as reductants. Also... After careful consideration of Training Courses...... 7 many deserving applications, Events...... 7 the special Grant Selection Committee has selected the second grant award winner. An AutoChem II 2920 Cata- lyst Characterization System has been awarded to the De- partment of Chemical Engi- Dr. John Monnier neering at the University of South Carolina. Dr. John Monnier, Research Professor and Principal Investigator states, “One of the primary emphasis www.micromeritics.com areas of the University is nanotechnology, and the

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Grant Award continued efforts are being led by responsible for catalytic endar quarter. Remaining the USC Nanocenter. Na- transformations. All other grant deadline dates for noscale catalysis is a focal analytical tools measure 2007 are: point, or thrust area, of only physical and/or Application deadline the Nanocenter which chemical correlations re- 6/30/07; includes not only the tra- lated to concentrations of Grant decision prior to ditional areas of catalyst active sites.” 9/30/07 synthesis and evaluation According to Preston Hen- Application deadline for environmental and drix, Micromeritics’ Presi- 9/30/07; chemical processes, but dent, “This program is TM Grant decision prior to also the Future Fuels designed to promote and 12/31/07 initiative at USC which advance the acquisition Applications may be is heavily focused on and use of particle char- submitted at any time fuel cells and alternative acterization instrumenta- in accordance with the energy sources, of which tion not generally avail- application instructions catalysts and electrocata- able through other means and will remain active for lysts are key components. to non-profit universities a period of one year from Selective chemisorption and institutions. We are the date of submission. is the single most impor- very proud and excited to For more information, go tant analytical tool used present this award in an to www.micromeritics.com for the study and appli- ongoing grant program to and click on Grant Pro- cation of materials em- support important re- gram for a detailed grant ployed in these catalytic search.” processes, and is the only description, application A maximum of one instru- technique that directly requirements, and appli- ment/integrated system measures the concentra- cation. will be awarded per cal- tion of active surface sites

eter Bouza has been of Science in Electrical Micromeritics Appoints Pnamed Manager of Engineering and is final- New Manager of Market Market Development for izing a Master of Science Micromeritics Particle in Industrial Engineering Development Size, Count, and Shape from Florida Internation- Business. al University in Miami, In his new role, Mr. Bou- Florida. za will be responsible for Mr. Bouza’s comprehen- expanding the Particle sive expertise in the area Size, Count, and Shape of particle analysis is business of Micromerit- especially relevant with ics. Micromeritics’ Saturn Peter joins Micromerit- DigiSizer High Resolution ics from Beckman-Coul- Laser Particle Size ana- ter where he worked in lyzer and recent introduc- varying roles for over 15 tion of the Elzone II Par- years in their Particle ticle Size analyzer. His Characterization Divi- knowledge and experience sion. For the past seven will be instrumental in years he has held the helping Micromeritics to Mr. Peter Bouza position of General Man- build stronger relation- ager for Global Opera- ships with the biotechnol- tions. He has a Bachelor ogy and pharmaceutical industries.

Vol 18 No 2

Scientific Theory Posters are Now Available.

icromeritics Instru- Mment Corporation is releasing a series of posters illustrating the theories behind the technolo- gies of our broad line of automated particle characterization analytical laboratory instruments. In this series of posters, the various theories used to determine particle characteristics such as surface area, particle size, pore volume, pore size, absolute density, envelope density, bulk density, catalytic activity, and active surface area will be presented. These posters are now available through our on-line catalog or by calling customer support or your sales representa- The Electrical Sensing Zone Theory and the Mercury tive. Porosimetry Theory posters are currently available.

Micromeritics Extensive Bibliography Referencing More Than 6,000 Scientific Papers Surpasses 25,000 Downloads his bibliography has In this series of peer-re- those papers that are Tbeen updated to in- viewed papers, various available from various clude approximately 600 particle characteristics sources on the Internet. papers referencing Mi- such as surface area, We have often been asked cromeritics instruments particle size, pore vol- for references to papers published since January. ume, pore size, absolute in which a scientist uses density, envelope density, For those interested in a Micromeritics instru- bulk density, catalytic ac- ment to study the same the physical characteris- tivity, and active surface tics of powders and solids or similar materials as area are determined for a the new user intends to for fundamental research, wide variety of materials. product development, study. This document will Each of these technical satisfy that need. It also quality assurance and papers references one or control, production, or serves as a powerful ref- more Micromeritics prod- erence resource for those process control applica- ucts. The list by no means tions, this bibliography is engaged in particle char- represents a complete and acterization. an indispensable tool. exhaustive search of the literature, but includes

Vol 18 no 2

Pulse Chemisorption with AutoChem II 2920: Isopropylamine on Zeolites Andrew D’Amico

Introduction Several ZSM-5 zeolite samples were analyzed The Hoffman elimination reaction: using the AutoChem II 2920. By pulsing iso- propyl amine onto the zeolites, the concentra- NH2 H H tion of acid sites can be determined for a particular zeolite. This is very C C + N important for catalytic H reactions. For example, the reaction that occurred H3C CH3 CH2 CH3 H H during these analyses proceeded through an in- termediate due to an acid- base reaction between the amine and the zeolite, followed by a specific type of E2 elimination, known as Materials: the Hoffman elimination. The samples used are listed below. Due to the second order kinetics involved in this Zeolite Type SiO / Al O reaction, a high concen- 2 2 3 tration of acid sites would ZSM-5-30 30 allow the reaction to pro- ceed much more quickly. ZSM-5-55 50 Preparation ZSM-5-80 80 While there was no preparation of the sample as far as degassing is concerned, it could be by heating the sample to were twenty loop injec- said that the sample was high temperature. These tions of isopropylamine ‘prepared’ by heating. The samples were ‘prepared’ occurring at four-minute ZSM-5 samples contained by first being heated to intervals. The last part various cations, including 500 °C and then cooling of the analysis involved a ammonium (NH +). These 4 back to 200 °C. temperature-programmed cations were not as desir- desorption (TPD). At this able for the analysis as Analysis step in the analysis, the the hydrogen cation (H+). The preparation part of mass spectrometer began Since samples contain- the analysis was followed scanning for propylene, the ing the hydrogen cation by the pulse chemisorp- product of interest. Data are more expensive, the tion step of the analysis. were collected during a tem- sample can be converted During this step, there perature ramp to 500 °C. to the hydrogen cation

Vol 18 No 2

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Data 0.08 These graphs show how the intensity of the TCD 0.06 signal changes for various zeolite samples. Notice TCD Signal (a. u.) 0.04 that a direct proportionality exists between the 0.02 peak intensities and the concentration of alumi- 0.00 num oxide (Al2O3), and 100 150 200 250 300 350 400 450 500 an inverse proportionality Temperature oC exists between the peak intensity and the silica- to-aluminum oxide ratio 0.12 (SiO2/Al2O3). 0.10

Legend: 0.08

0.06 ZSM-5-30

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ZSM-5-55 TCD Signal (a. u.) ZSM-5-80 0.02

0.00 240 260 280 300 320 340 Temperature oC

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0.06 Attention Authors We welcome articles and informa- 0.04

tion concerning particle technol- TCD Signal (a. u.) ogy applications performed with Micromeritics instrumentation. 0.02 See the back page for further information. 0.00 240 260 280 300 320 340 Temperature oC

Vol 18 no 2

What’s New at MAS he mission of Micromeritics Analytical Services T (MAS) is to provide all our customers with the best in contract analytical services. We will continually strive to improve and expand the services provided to Look for Micromeritics meet our customers’ needs. Analytical Services at these upcoming events In keeping with our mission statement, MAS has a and meetings: new shipping address (One Micromeritics Dr., Suite 200, Norcross, GA 30093) that will allow us to quick- American Chemical ly and efficiently receive your important samples. Society - Fall 2007 Samples are now received at our front door by our lab August 19 - 23 coordinator, who is ultimately responsible for booking Booth 1007 the samples into the LIMS and starting them on their Boston Convention journey through the lab. The time savings for your Center samples could be as much as one entire day. Boston, MA

MAS is pleased to offer average primary particle size American Council of analyses for those working with dried or aggregated Independent Labs nanoparticles. The analysis method is based on knowl- October 13 - 16 edge of the particle shape and measurement of the surface Annual Meeting area, density, and mass of the sample. The part number Intercontinental Hotel for this new testing service is 005 – 70 and the cost is Atlanta, GA $235 per sample. Reports will include the measured BET surface area, true density of the material, and the calcu- lated average particle diameter. For more information, ALMA 28th Annual download the nanoparticle size poster at www.particle- Conference testing.com/downloads. November 7 - 9 In the coming months, MAS plans to offer particle shape Wyndom St. Anthony analysis and nanoparticle size by dynamic light scatter- Hotel ing. Look for information on the web site, www.particle- San Antonio, TX testing.com.

Micromeritics Analytical Services is pleased to introduce three new employees.

L to R Yanette Cunningham, Shanita Jones, Luminita Dudu, B.S. Chemical Engi- B.S. Chemistry, is our B.S. Chemistry, is respon- neering, is responsible new lab coordinator who sible for measuring gas for chemical adsorption is responsible for receiv- adsorption isotherms and analysis which includes ing, invoicing, and storage BET surface area analy- the AutoChem 2920 and of samples and analysis ses. ASAP 2020 Chemisorp- results. tion instruments.

Vol 18 No 2

Micromeritics Instrument Training Courses Training 2007 Training is provided for most Report Generation and Micromeritics instrumentation Comprehension at the time of installation. This Learn to configure reports and AutoChem 2920 training presents all the infor- obtain more useful information, August 7 - 9 mation required for a new opera- as well as improve comprehen- Saturn DigiSizer 5200 tor to quickly become proficient sion of the reports produced. August 21 - 23 operating the instrument. In User Maintenance ASAP 2420 cases where personnel changes Practice routine maintenance August 28 - 30 occur or more advanced train- procedures which improve ing is required, Micromeritics AutoPore IV 9500 Series operation, reduce downtime, and conducts a variety of classes for September 11 - 13 increase data accuracy. many of our instruments. These TriStar courses are held at our head- Theory Overview September 18 - 20 quarters in suburban Atlanta, Learn about the scientific theory Georgia. The courses include: upon which each instrument is ASAP Physisorption and based and how it applies to the Chemisorption Detailed Operational critical factors relevant to suc- October 16 - 19 Procedures cessful sample preparation and Items covered are effective sam- ASAP 2020 Physisorption analysis performance. ple file creation, use of analysis October 16 - 18 parameters, and manual sample Enrollment For additional informa- entry. You´ll learn how to utilize Training courses last from 2 tion or to register for the the full power and flexibility of to 4 days and are designed to class of your choice, contact the operating software. provide hands-on, performance- the Micromeritics Training based instrument knowledge. Automatic Analysis Department at 770.662.3607. Small classes guarantee close Develop correct analysis pro- Early registration is recom- individual attention. Included cedures to optimize collection mended since class space is in the course materials are a of accurate, reproducible data. limited. Much of the class time is spent Study Guide, an instrument performing analyses in a con- Operator´s Manual, and other See our website for a complete trolled, tutorial environment. handout materials. Certificates course schedule. of Completion are also awarded. www.micromeritics.com Systems Utilities to all trainees. Discover all of the instrument software utilities which help you manage sample information files Students attending a recent and directories, protect data, training course: (L to R) and select system options. Trainer Mack Spivey Troubleshooting John Fomica Learn techniques that enable Leonel Sierra you to locate and quickly resolve Devon Preston instrument problems. S.C.V. Moorthy

Events 20th Interphex - Japan International Carbon Pacific Coast Catalysis Society June 20 - 22, 2007 Conference September 8, 2007 Tokyo Big Site July 15 - 20, 2007 University of Washington Tokyo, Japan Sheraton Hotel and Towers Seattle, WA Seattle, WA Ninth International Workshop American Chemical Society M. S. & T. 2007 on Physical Characterization August 19 - 23, 2007 September 16 - 20, 2007 of Pharmaceutical Solids Boston Convention Center Cobo Center June 24 - 30, 2007 Booth 1007 Detroit, MI Crown Plaza Boston, MA Boston, MA See our website for a complete Event schedule www.micromeritics.com Attention Authors How To Reach Us We welcome articles and information Micromeritics offers over 50 sales, service, and distribution offices through- concerning particle technology appli- out the world. For additional information, a free product demonstration, or cations performed with Micromeritics the location of the office nearest you, call or write: instrumentation. Everything from a single plot with operating conditions HEADQUARTERS: to an in-depth article on physisorp- Micromeritics Instrument Corporation Micromeritics GmbH tion, chemisorption, etc. with sup- One Micromeritics Drive Erftstrasse 54 porting graphs will be considered. Norcross, GA 30093-1877 D-41238 Mönchengladbach, GERMANY If your material is published in The USA Tel: (+49) (0)2166-98708-00 microReport, you will receive a copy Telephone: Fax: (+49) (0)2166-98708-88 of Analytical Methods in Fine Particle U.S. Sales (770) 662-3633 Technology by Paul A. Webb and International Sales (770) 662-3660 Micromeritics Ltd. Clyde Orr. Fax: (770) 662-3696 Unit 2, Chestnut House WEB: www.micromeritics.com 178-182 High Street North Dunstable, Bedfordshire LU6 1AT Send your article to: SUBSIDIARIES: ENGLAND James Kerce, Editor Micromeritics China Tel: (+44) (0)1582-475248 The microReport Apt. 5H, No. 1 Building Fax: (+44) (0)1582-475252 MICROMERITICS Hua-Ao (Epoch Center) One Micromeritics Drive No. 31 Zi Zhu Yuan Road, Hai Dian District Micromeritics N.V./S.A. Norcross, GA 30093-1877 Beijing 100089, P.R., CHINA Eugene Plaskylaan 140B 1030 Brussels, BELGIUM [email protected] Tel: (+86) (0)10-6848-9371 Fax: (+86) (0)10-6848-9371 Tel: (+32) 2-743-39-74 Fax: (+32) 2-743-39-79 Include your title, return address and Micromeritics Shanghai China phone number. Contributions cannot Room 15M, J Building, Ladoll International Micromeritics SRL be returned, but each will be acknowl- No. 831 XinZha Road, JingAn District, Via W. Tobagi n. 26/7 edged. Shanghai 200041, CHINA 20068 Peschiera Borromeo Milano, ITALY Micromeritics France S.A. Tel: (+39) (0)2 553 02833 Parc Alata Fax: (+39) (0)2 553 02843 Rue Antoine Laurent Lavoisier 60550 - Verneuil en Halatte, FRANCE Tel: (+33) (0)33-3-44-64-6080 Fax: (+33) (0)33-3-44-64-6089 e h t microReport The Science and Technology of Small Particles™ Micromeritics The microReport newsletter is One Micromeritics Drive published by Micromeritics Norcross, GA 30093-1877, U.S.A. Instrument Corporation. Editor: James Kerce, (770) 662-3654

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