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    The Science and Technology of Small Particles

    Surface Area and Porosity System

    TriStarII 3020

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    Analytical Versatility/High Throughput/Small Footprint

    TriStar II 3020 Surface Area and Porosity System

    Surface area and porosity are importantphysical properties that influence the qualityand utility of many materials and products.Therefore it is critically important that thesecharacteristics be accurately determinedand controlled. Likewise, knowledge ofsurface area and especially porosity oftenis an important key to understandingthe formation, structure, and potential

    application of many natural materials.

    High Sample Throughput/Analytical Versatility

    The TriStar II 3020 is a fully automated,three-station, surface area and porosityanalyzer that delivers high-quality data at anaffordable price. It is capable of increasingthe speed and efficiency of routine qualitycontrol analyses, yet has the accuracy,resolution, and data reduction capabilityto meet most research requirements. TheTriStar II also features a new KryptonOption, allowing measurements in the verylow surface area range. The instrument alsocombines versatility in analysis methodsand data reduction to allow the user to

    optimize analyses to specific applications.A Small Footprint/Packed withFeatures

    Three analysis ports operate simultane-ously and independently of one another.Three BET surface area measurements canbe performed in less than 20 minutes. Foradditional throughput, four TriStars can beoperated with one computer.

    Surface areas as low as 0.01 m2/g canbe measured with the standard nitrogensystem. The TriStar II also accommodatesthe use of argon, carbon dioxide, andother non-corrosive gases such as butane,methane, or other light hydrocarbons. AKrypton Option can extend surface areameasurements to as low as 0.001 m2/g.

    A dedicated POport is standard, allowing

    the measurement of saturation pressureon a continuous basis. Saturation pressurecan be entered manually, measured contin-uously, or collected over the sample. TheTriStar II provides the flexibility to controland fine-tune analysis speed and accuracy.

    Incremental or fixed dosing routinesprevent overshooting pressure pointswhile minimizing analysis time.

    Free space can be measured, calculatedor manually entered providing maximumflexibility in accommodating specialsample types and emphasizing speed whneeded.

    Enhanced product support featuresinclude: video clips; Ethernet communiction between the computer and TriStar; code reader capability; built-in electronitest points and diagnostic software;

    ability to perform remote diagnostics vithe internet; and the ability to read andcompare historical TriStar and Gemini dto TriStar II data.

    A 2.75-liter Dewar and extended lengthsample tubes allow complete adsorptionand desorption isotherms to be collectewithout operator intervention.

    The TriStar II can collect up to 1000 datpoints. Fine details of the isotherm canbe observed and recorded providing higresolution and revealing pore structuredetails.

    Intuitive and powerful Windows-basedsoftware allows more versatility in dataarchiving and networking. However, themost powerful features of this softwareare found in its expanded range of datareduction and reporting. SPC reports, nisotherm and thickness models, isosteriheat of adsorption, and integrated DFTmodels are all included.

    Optional sample preparation devices aravailable combining flowing gas and/or

    vacuum with heat to remove atmosphercontaminants, such as water vapor and

    adsorbed gas, from the surface and poreof the sample.

    An attractively designed cabinet combina small footprint with easy accessibility

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    Typical TriStar II ApplicationsPharmaceuticals Surface area andporosity play major roles in the purification,processing, blending, tableting, andpackaging of pharmaceutical products aswell as their useful shelf life, dissolutionrate, and bioavailability.

    Ceramics Surface area and porosity affectthe curing and bonding of greenware andinfluence strength, texture, appearance, anddensity of finished goods. The surface areaof glazes and glass frits affects shrinkage,

    crazing, and crawling.

    Adsorbents Knowledge of surface area,total pore volume, and pore size distributionis important for quality control of industrialadsorbents and in the development ofseparation processes. Surface area andporosity characteristics affect the selectivityof an adsorbent.

    Activated Carbons Surface area andporosity must be optimized within narrowranges to accomplish gasoline vaporrecovery in automobiles, solvent recovery in

    painting operations, or pollution controls inwastewater management.

    Carbon Black The wear lifetime, traction,and performance of tires are related to thesurface area of carbon blacks used in their

    production.

    Catalyst The active surface area and porestructure of catalysts influence productionrates. Limiting the pore size allows onlymolecules of desired sizes to enter andexit, creating a selective catalyst that will

    produce primarily the desired product.

    Paints and Coatings The surface areaof a pigment or filler influences the gloss,

    texture, color, color saturation, brightness,solids content, and film adhesion properties.The porosity of a print media coating isimportant in offset printing where it affectsblistering, ink receptivity, and ink holdout.

    Projectile Propellant The burn rate ofpropellants is a function of surface area.Too high a rate can be dangerous; too low arate can cause malfunction and inaccuracy.

    Medical Implants Controlling theporosity of artificial bone allows it toimitate real bone that the body will acceptand allow tissue to be grown around it.

    Electronics By selecting high surfacearea material with carefully designed

    pore networks, manufacturers of super-capacitors can minimize the use of costlyraw materials while providing moreexposed surface area for storage of charge.

    Cosmetics Surface area is often used bycosmetic manufacturers as a predictor of

    particle size when agglomeration tendenciesof the fine powders make analysis with a

    particle-sizing instrument difficult.

    Aerospace Surface area and porosity ofheat shields and insulating materials affectweight and function.

    Geoscience Porosity is important ingroundwater hydrology and petroleumexploration because it relates to thequantity of fluid that a structure can containas well as how much effort will be requiredto extract it.

    Nanotubes Nanotube surface area andmicroporosity are used to predict thecapacity of a material to store hydrogen.

    Fuel Cells Fuel cell electrodes requirehigh surface area with controlled porosityto produce optimum power density.

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    Superior Data Presentation Capability

    Operating SoftwareThe TriStar II 3020 Windows interface

    provides a familiar environment for theuser. It is easy to collect, organize, archiveand reduce raw data, and store standardizedsample information for later use. Thereports may be generated to screen, paper,or data transfer channels. Cut-and-pastegraphics, scalable-and-editable graphs, andcustomized reports are easily generated.

    In addition to controlling instrument operation,the Windows software also reduces the raw

    data collected during analysis. The reduceddata can be reviewed or printed in a variety ofeasy-to-interpret tabular and graphical reports.These include:

    Single- and multipoint BET surface area

    Total pore volume

    Langmuir surface area and isotherm reports

    t-Plot

    - Harkins and Jura Thickness Equation

    - Halsey Thickness Equation

    - Carbon STSA

    - Broekhoff-de Boer

    - Kruk-Jaroniec-Sayari

    This BET plot of 200 m2/

    silica alumina (red), 50

    silica gel (green), and 20

    m2/g titania (blue) demo

    strates the versatility of

    TriStar II. Three differen

    materials may be analyz

    simultaneously and then

    overlaid for comparison.

    An example of an analysis in progress the TriStar II features an embedde

    microprocessor that controls the unit operation and sample analysis. This u

    friendly Windows software allows the user to control the instrument from a

    workstation, monitor the progress of the analysis, and view the results of

    the experiment.

    BJH adsorption and desorption - Standard

    - Kruk-Jaroniec-Sayari correction

    Dollimore-Heal adsorption and desorption

    Mesopore and Macropore

    - Volume and area distributions by pore size

    MP-Method

    DFT pore size

    DFT surface energy

    Summary report SPC reports

    Validation reports

    For applications that fall under the FDAs21 CFR 11 rule, Micromeritics optionalconfirm software option provides thesecurity features and audit trails requiredthis regulation.

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    Pore volume and pore size distri-

    butions are easily determined

    using the full-featured TriStar II

    report system.

    Pore volume and pore size

    distributions for several samples

    may be overlaid to emphasize

    the difference between variousmaterials.

    TriStar II Reference Materials

    Silica-aluminaThe silica-alumina is a typical poroushigh surface area reference material.The surface area of silica-aluminatypically exceeds 200 m2/g and the poresize is a nominal 100 . This materialis recommended for users that analyzeamorphous materials with surface arearanging from 10 to greater than 300 m2/gand for both non-porous and porousmaterials in the 40-3000 range.Silica-alumina is suitable for use withBET, t-plot, and BJH pore size reports.

    Carbon BlackStandard Reference Blacks are availablefrom 20 to greater than 100 m2/g. Theseare stable and very well characterizedmaterials. They are recommended for allusers but may be especially suited forresearchers in the carbon, tire, and fillerindustries. The carbon black referencematerials are suitable for use with theBET and STSA reports.

    GlassA 5 m2/g glass reference material isrecommended for industries and usersthat characterize materials in the 1through 50 m2/g range. Glass referencematerial is suitable for use with the BETsurface area report.

    AluminaLow surface area alpha alumina (lessthan 1 m2/g) is available for use withkrypton. Alpha alumina is recommendedfor researchers in the pharmaceutical,

    abrasives, soil, and other areas thatrequire the characterization of materialswith surface areas less than 1 m2/g.

    Alpha alumina reference material isrecommended for use with krypton andthe BET surface area report.

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    Innovative Design

    The TriStar II TechniqueMicromeritics TriStar II utilizes the staticadsorption technique. The instrumentfeatures a thermally stable dosing manifold(M), a three-port sample manifold, adedicated tube for measuring saturation

    pressure (PO), and a rapid response servo

    valve (S). The main manifold features a1000-torr transducer and is coupled to therapid response servo valve. The servo valveis used for rate-controlled evacuationsof the sample, and used throughout theanalysis to rapidly and accurately dose the

    manifold. The servo-controlled evacuationrate may be set by the user to minimizethe risk of fluidizing powder samples. For

    pellets, spheres, extrudates, or other formedsamples, the evacuation rate may be set

    very high to rapidly evacuate the sampletube.

    The TriStar II also features four gasinlets for probe molecules (J). A typicalconfiguration will feature nitrogen as theanalysis gas and helium for determining the

    void volume of the sample tube. However,two additional gases may be connected foradditional flexibility. For example, carbondioxide is often used for difficult-to-analyzemicroporous materials, and krypton maybe preferred for low surface area samples(requires additional hardware for kryptonanalysis option-K).

    During a typical analysis, the manifold,sample tubes, and the POtube are

    evacuated. After a sufficient vacuum hasbeen achieved, the manifold is filled withhelium and then sample port 1 valve isopened to determine the warm free spaceof sample 1. This sequence is repeated forsamples 2 and 3 to determine the free spaceat room temperature. The elevator is raisedand the samples are cooled to nearly 77 K.This allows the free space to be determinedat the analysis temperature. Once the freespace analysis is finished, the saturation

    pressure of the adsorptive is determinedusing the POtube. Typically nitrogen isdosed into the tube above atmospheric

    pressure. The nitrogen is allowed tocondense and the vapor pressure of thenitrogen is easily monitored by a transducerthroughout the analysis.

    The adsorption isotherm is rapidly collecby using the servo valve to dose nitrogeninto the manifold. The pressure andtemperature of the nitrogen are recordeda sample port is opened, and the nitrogenis allowed to adsorb onto the sample.The quantity of nitrogen removed fromthe manifold is recorded as the quantitydosed. The sample valve is then closedand the adsorption is allowed to proceedto equilibrium. The quantity adsorbed canbe calculated from the quantity dosedminus any residual nitrogen in the sampletube. This process is repeated for all thresamples. The analysis is a parallel operatso that while one sample is equilibratinga different sample can be dosed withnitrogen.

    The order of sample analysis is based onthe material, not sequential operation.Samples that adsorb nitrogen rapidly canbe analyzed in parallel with materials thaare tortuous and require additional timeto adsorb nitrogen. This allows the userto characterize three unique materialssimultaneously providing rapid, reliable,

    repeatable results.

    K

    J

    S PO

    M

    ContinuousP

    OMonitoring

    Sliding Shield

    Three Parallel

    Sample Analyses

    Large Capacity

    Dewar

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    SmartPrep 065

    VacPrep 061

    Accessories

    Sample Preparation DevicesMicromeritics sample preparation devicesprepare batches of samples for surface areaand pore volume analysis. They combineflowing gas and/or vacuum with heat toremove atmospheric contaminants, suchas water vapor and adsorbed gas, from thesurface and pores of the sample. The qualityof the data produced by surface area andpore volume analyses depends greatly onthe cleanliness of the sample surface. AllMicromeritics sample preparation devicesaccept helium, nitrogen, argon, and other

    non-corrosive gases.

    TheSmartPrep 065 is a flowing-gasdegassing unit which removes adsorbedcontaminants from the surface and poresof a sample in preparation for analysis.It contains six sample ports, each oneindependently temperature-controlled forgreater flexibility. It contains two serialports, one for connecting to the computerand the other available for connection ofan additional SmartPrep. The temperature,ramp rates, and soak times of each sampleare individually controlled by the computer.Up to five ramps and soaks are allowed.All degas information is integrated into thesample data file for future reference.

    The FlowPrep 060applies both heatand a stream of inert gas to the sample.The heat causes contaminants to desorbfrom the surface and the stream of inert gassweeps them out of the sample tube. It letsyou choose the temperature, gas, and flowrate best suited for your sample materialand application. Needle valves allow you tointroduce the flowing gas slowly to prevent

    fluidization of samples.

    TheVacPrep 061 offers two methodsfor removing contaminants. In addition toflowing gas, it provides vacuum to preparesamples by heating and evacuation. Thiscombination allows you to choose the

    preparation method that is best suited toyour material or application. The VacPrep

    features six degassing stations, and a choiceof vacuum or gas flow preparation on eachof the six stations. Needle valves are also

    provided allowing you to introduce theflowing gas or vacuum slowly to preventfluidization of samples.

    Model 021 LN2Transfer System

    The Model 021 LN2Transfer System allowsyou to transfer liquid nitrogen or liquidargon from a nonpressurized storage Dewarinto smaller containers used in laboratoryexperiments.

    The system was specifically developedfor conveniently filling Dewars for gasadsorption instruments but also can be usedfor other cryogen applications. The Model021 can discharge cryogens at adjustablerates up to 3 liters/min. The roller basemakes it easy to move the 021 System to thelocation where the cryogen is needed. Thespigot and insulated, flexible hose enableconvenient filling and refilling of analysisDewars. The system can hold liquid nitrogenor liquid argon up to 30 days allowing cost-efficient use of your cryogen.

    Additional accessories are available forspecial applications.

    To request a quote or additional produc

    information, visit Micromeritics web sit

    at www.micromeritics.com, contact your

    local Micromeritics sales representative

    or our Customer Service Department at

    (770) 662-3636.

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    Micromeritics Instrument Corporation

    4356 Communications Drive

    Norcross, GA 30093

    USA

    Telephones:

    U.S.Sales (770) 662-3633

    International Sales (770) 662-3660Fax (770) 662-3696

    Micromeritics China - Beijing Office

    Room 1202. No. 1 Building

    Shi-Hao Ming-Di (Ten-Mansion)

    No. 81 Zi Zhu Yuan Rd.

    Hai Dian District

    Beijing, P.R. CHINA

    Code: 100089

    Telephone (86)-10-68489371

    Fax (86)-10-68489372

    Micromeritics France S.A.

    Parc Alata

    Rue Antoine Laurent Lavoisier

    F-60550 Verneuil en Halatte

    FRANCE

    Telephone (+33) (0)3 44 64 60 80

    Fax (+33) (0)3 44 64 60 89

    Micromeritics GmbH

    Avantis Science Park

    Rutherford 108

    D-52072 Aachen

    Telephone (+49) (0) 241 189 446 0

    Fax (+49) (0) 241 189 446 11

    Micromeritics Ltd.

    Unit 2, Chestnut House

    178-182 High Street North

    Dunstable, Bedfordshire LU6 1AT

    ENGLAND

    Telephone (+44) (0)1582-475248

    Fax (+44) (0)1582-475252

    Micromeritics N.V./S.A.

    Eugene Plaskylaan 140B

    1030 Brussels

    BELGIUM

    Telephone (+32) (0)2-743-39-74

    Fax (+32) (0)2-743-39-79

    Micromeritics SRL

    Via W.Tobagi n.26/7

    20068 Peschiera Borromeo, Milano

    ITALY

    Telephone (+39) (0)2553

    02833

    Fax (+39) (0)2553 02843

    Micromeritics Japan, G.K.

    5F Tokatsu Techno Plaza

    501, 5-4-6 Kashiwanoha

    Kashiwa, Chiba 277-0882

    Japan

    Telephone (81)-0-4-7128-5051

    Fax

    (81)-0-4-7128-5054