QUANTACHROMEAUTOsORb-1 sERIEsSURFACE AREA, PORE SIZE AND CHEMISORPTION

®

uantachrome...

where research andengineering of new andimproved products isongoing. Manufacturersalso rely on particlecharacterization technology tomore precisely specify bulkmaterials, to control quality,and to isolate the source ofproduction problems withgreater efficiency...betterproducts through particlecharacterization—a forceevident in today’s industrialworld.

Quantachrome is alsorecognized as an excellentresource for authoritativeanalysis of your samplesin our fully equipped,state-of-the-art particlecharacterization laboratory.

Quantachrome Instruments…world leader in thedevelopment of instrumen-tation for the characteri-zation of powdered andporous materials.

renowned inno-vator of ideas for today’sparticle technology needs.For more than 35 years,Quantachrome’s scientistshave revolutionized mea-surement techniques anddesigned instrumentationto enable the accurate,precise, and reliable charac-terization of powdered andporous materials.

• Surface Area Measurement• Adsorption/Desorption

Isotherms• Pore Size Distribution• Chemisorption Studies• TPR/TPO/TPD• True Solid Density• Mercury Porosimetry• Water Vapor Sorption

Not only are Quantachromeproducts the instruments ofchoice in academia, but thetechnologies conceived anddeveloped by our scientificstaff are applied in industriallaboratories worldwide,

Quantachrome Instruments’corporate headquarters in Boynton Beach, Florida.

molecules quickly find theirway to the surface of everypore in the solid (the adsor-bent). These molecules caneither bounce off or stick tothe surface. Gas moleculesthat stick to the surface aresaid to be adsorbed. Thestrength with which adsorbedmolecules interact with thesurface determines if theadsorption process is to beconsidered physical (weak) orchemical (strong) in nature.

Physical adsorption(physisorption) is the mostcommon type of adsorption.Physisorbed molecules arefairly free to move around thesurface of the sample. As moregas molecules are introducedinto the system, the adsorbatemolecules tend to form a thinlayer that covers the entireadsorbent surface. Based onthe well-known Brunauer,Emmett and Teller (BET) the-ory, one can estimate the num-ber of molecules required tocover the adsorbent surfacewith a monolayer of adsorbed

Photomicrograph:Carbon black

Photomicrograph:Prickly gold

All matter is made up ofatoms. In gases, atoms andmolecules are free to moveabout in space. In contrast,atoms in solids are located infixed positions by electricalforces of attraction amongneighboring atoms. But theoutermost (or surface) atomsin the solid have fewer neigh-bors than the atoms beneaththem. To compensate for theirelectrical force imbalance,surface atoms seek to attractsurrounding gas molecules.The tendency of all solid sur-faces to attract surroundinggas molecules gives rise to aprocess called gas sorption.As illustrated by the ensuingexamples, monitoring the gassorption process provides awealth of useful informationabout the characteristicsof solids.

Before performing gas sorp-tion experiments, solidsurfaces must be freed fromcontaminants such as waterand oils. Surface cleaning(degassing) is most often car-ried out by placing a sampleof the solid in a glass celland heating it under vacuum.Figure 1 illustrates how a solidparticle containing cracks andorifices (pores) of differentsizes and shapes may lookafter its pretreatment.

Once clean, the sample isbrought to a constant tempera-ture by means of an externalbath. Then, small amounts of agas (the adsorbate) are admit-ted in steps into the evacuatedsample chamber. Adsorbate

Photomicrograph:Radiolaria

The structure and reactivity of with gas molecules. Quantif

isotherms permits the routineas surface area, size a

Quantachromehas fostered w

The Porous materials

characterization serves many industries

including:

AerospaceAgricultureAutomotive

AviationBuilding Materials

CeramicsChemicals

Communications EquipmentConstruction

Consumer GoodsCosmetics

Electrical & ElectronicsEnvironmental Services

FoodsFood Processing

ManufacturingMarine

Medical DevicesMetals

Mining & MineralsMunitions

Oil ExplorationOptics

Paints & CoatingsPaper & Packaging

PetrochemicalsPharmaceuticals

PlasticsRubberTextiles

Water Treatment

Industries Served

molecules, Nm (see Figure 2).Multiplying Nm by the cross-sectional area of an adsorbatemolecule yields the sample’ssurface area.

Continued addition of gasmolecules beyond monolayerformation leads to the gradualstacking of multiple layers (ormultilayers) on top of eachother. The formation of multi-layers occurs in parallel tocapillary condensation (see

Figure 3). The latter process isadequately described by theKelvin equation, which quan-tifies the proportionalitybetween residual (or equilibri-um) gas pressure and the sizeof capillaries capable of con-densing gas within them.Computational methods suchas the one by Barrett, Joynerand Halenda (BJH) allow thecomputation of pore sizesfrom equilibrium gas pres-sures. One can therefore gen-erate experimental curves (orisotherms) linking adsorbedgas volumes with relative

solid materials determine the manner in which their surfaces interactfying gas–solid interactions through the generation of gas sorption evaluation of properties that control the performance of solids, suchand shape of pores, chemically active sites, and many others.

saturation pressures at equi-librium, and convert themto cumulative or differentialpore size distributions.

As the equilibrium adsorbatepressures approach satura-tion, the pores become com-pletely filled with adsorbate(see Figure 4). Knowing thedensity of the adsorbate, onecan calculate the volumeit occupies and, conse-quently, the total porevolume of the sample. Ifat this stage one reversesthe adsorption processby withdrawing knownamounts of gas from thesystem in steps, one canalso generate desorptionisotherms. Since adsorp-tion and desorptionmechanisms differ,adsorption and desorptionisotherms rarely overlayeach other. The resultinghysteresis leads to isothermshapes that can be mechanis-tically related to thoseexpected from particularpore shapes.

In contrast to physisorption,chemical adsorption(chemisorption) involves theformation of strong chemicalbonds between adsorbatemolecules and specificsurface locations known aschemically active sites.Chemisorption is thus usedprimarily to count thenumber of surface activesites which are likely topromote chemical andcatalytic reactions.

e’s pioneering development of gas sorption instrumentsworldwide R&D and quality control efforts for decades.

Gas Sorption Process

A section ofone greatly

enlargedparticle of

a solid.

1

The monolayer ofadsorbed molecules;approximately 15%saturation.

2

The multilayer/capillarycondensation stage;approximately 70%

saturation.

3

Total pore volume fill-ing; approximately100% saturation.

4

Photomicrograph:Coal ash

Photomicrograph:Natural zeolite

Applications forQuality Controland Research

The list of materials andproducts employing Quantachrome’sparticle characterization technologyis as diverse as industry itself:

Carbon for rubber, adsorbents (gasseparation and water purification),gas masks, inks, laser printersand copiers

Catalysts for the automotive,fertilizer and petrochemical industries

Organic materials for adhesives,chromatography, cosmetics, detergents,foodstuffs, explosives, ion exchangeresins, pharmaceuticals and plastics

Minerals such as alumina,clays, hydroxyapatite, pigments,phosphates, silicas, zirconia, etc.,used for abrasives, adsorbents,biomaterials, ceramics, cements,desiccants, fillers, papers and paints

Powdered metals and ferrites forbatteries, pressure formed/ sinteredproducts, electronics, magnets andmagnetic tape

Other applications related to bone,composite materials, fibers, rigidfoams, soil, sludge, slurries,suspensions and well cores

AUTOSORB-1 Series Product Overview

Quantachrome’s AUTOSORB-1Series offers a full line of highquality, high performance SurfaceArea and Pore Size Analyzers withthree fully automatic models tomeet the needs of any research orquality assurance laboratory.The AUTOSORB-1 for stan-dard applications using avariety of adsorbates

• Fully automated analyzer for sur-face area and pore size measure-ments.

• Simultaneous analysis and sam-ple preparation.

• System supplied complete andready for operation.

• Low maintenance, vacuum volu-metric system with stainlesssteel manifold construction.

• Speed and precision ensured byMAXIDOSE™, a proprietaryoperating algorithm.

• DoseWizard™ learn mode andInitialFill™ for analysis time sav-ings up to 60%.

• High sensitivity ensured by mul-tiple pressure transducers, mini-mum void volume and accuratecoolant level control.

• Operates with any non-corrosiveadsorbate and a wide variety ofcoolants, including slurries.

AUTOSORB-1-MP for low sur-face area and microporemeasurement

• Allows adsorption data acquisi-tion at relative pressures below1 x 10–7 utilizing 1 torr transduc-ers.

• Patented oil-free turbomolecularvacuum system eliminates anyrisk of oil backstreaming.

• Enhanced 22 bit A/D converter and micropore dosingalgorithm allow precisedata acquisition of up to 200data points, sub-ångström resolu-tion and automatic correction forlow pressure thermaltranspiration.

• Ideal for detailed micropore sizemeasurements of zeolites, car-bons, molecular sieves, etc.

• Many modern data reductionmodels and dosing algorithmsfor maximum flexibility.

• Well suited for low surface areaanalysis with krypton gas.

AUTOSORB-1-C for totalprecise, chemisorption/physisorption measurement

• Unattended chemisorption meas-urement with automatic transferfrom in-situ sample preparationto analysis.

• Patented oil-free turbomolecularvacuum system eliminates anyrisk of oil backstreaming.

• Sample preparation with flow,vacuum or static conditionsunder programmable heatingrates at temperatures up to1,100°C. Prep gas flows throughpowder bed for thorough reduc-tion.

• Built-in, five port gas inputmanifold with automatic gasswitching.

• Applications includecharacterization of metaldispersion, acid site distribution,crystallite size, heats of adsorp-tion and much more.

• Compatible with broadrange of gases and vaporsincluding hydrogen, carbonmonoxide, ammonia, and cyclo-hexane (optional seals available).

• Options: interface for mass specor GC and/or built-in TCD.

VAPOR SORPTION option forAUTOSORB -1-C andAUTOSORB-1-MP

• Thermostatted dosing manifold toreduce vapor condensation.

• Built-in, heated vapor generator.• Specially designed vapor dosing

software for precise vaporisotherms.

Vapor generation controls.(Vapor source visible through transparent cover)

AUTOSOP R E C I S E • R E L I A B L E • F A S T

A variety of sample cells are available for all applications.

Front panel LEDs displaycontinuous system status

information

Optional Mass Spectrometer

Sample and P0 station

Coolant level controller

60 hour dewar flaskand elevator

Vacuum cold trap totrap degas by-products

• Active metal area, degree ofmetal dispersion and aver-age crystallite size.

• Heats of adsorption.• Fractal dimension.

Sample preparation

Sample surface contaminantsare removed by heating undervacuum. Two automateddegassing stations may operateconcurrently with the analysisstation. PASS/FAIL degas testwith digital display of degaspressure permits user to setand monitor sample prepara-tion more precisely.

The AUTOSORB-1 analyzer ismicroprocessor controlled, andcommunicates with a Windows98, 2000, NT, XP-based PC withQuantachrome’s state-of-the-art,data acquisition and data reduc-tion software (ASWinTM).Comprehensive softwareto meet modern needsWhether a laboratory’s need isfor wide ranging physisorptionstudies or complete automationof the catalyst treatment andmultiple pass chemisorptionprocess, the AUTOSORB soft-ware serves admirably. It alsoserves two or more analyzers...and two or more users connect-ed via a network. And, afterthe accumulation of many datafiles, a built-in database enginequickly locates desired files bysearching for a specific ID,description, operator, commentor range of dates.The user-friendly software

guides you through samplepreparation, preprogrammedparameter recall or making set-tings for operations, datareduction, graphs and reportprintouts.During operation one can viewthe accumulated data, theisotherm and all associatedgraphs and analytical results upto that point.After a run, reports and graphsare printed automatically or theoperator can use the softwareto determine the best fittingmethod, to compare data byoverlaying curves or to adjustgraph, size, scaling, titles, plotmarkers and line colors forbest print out.

Data presentationA comprehensive range ofsurface area and pore sizemethods is available:• Adsorption and desorption

isotherms.• Multi and single point BET

surface area (including Cconstant and correlationcoefficient).

• Langmuir surface area• Mesopore volume and area

distribution (BJH and DHmethods).

• Standard micropore size dis-tribution (MP method) and t-method by deBoer, Halsey orcarbon black (STSA).

• Total pore volume,average pore size andsample density.

• Dubinin-Radushkevichmicropore surface area

• Horvath-Kawazoe, Dubinin-Astakhov and Saito-Foleymicropore distribution.

• Full Density FunctionalTheory library for unifiedmicro- and mesopore analy-sis using N2, Ar and CO2 onmaterials such as zeolites,MCM-41, carbons and silicas.

• Monte Carlo based pore sizemodel.

For chemisorption analysis,standard calculations include:• Combined, strong and weak,

(reversible and irreversible)isotherms.

• Monolayer coverage byextrapolation or bracketingof isotherm data and Temkinor Freundlich plots.

Functional Capability by Model

Surface area analysis

Mesopore size distribution

Standard micropore methods

Advanced, low pressure micropore analysis

Chemisorption methods

AUTOSORB-1

AUTOSORB-1-MP

AUTOSORB-1-C

–– –

Analysis parameters in Autosorb software

Mutiple graphs to view isotherm and related plots

Windows® based performance

ORB-1 Series®

• V E R S A T I L E • E C O N O M I C A L

AUTOSORB-1 Series BenefitsSuperior engineering deliversyears of trouble-free operation. Allprocess control features are self-contained, enabling the instrumentto function independently withoutoperator intervention or externalcomputer support.

Designed for operatorconvenience and ease of use

With minimal operator training,the AUTOSORB-1 produces theresults you need.

• Store a limitless number ofuser-defined analyses for fastand simple measurementinitialization.

• Automatic error checkingensures reliable data.

• Front panel LED displayof valve and dewar statusprovides “at-a-glance”confirmation of systemoperation.

• Easy-fill dewar flasks offer safeand simple handling of cryo-genic liquids.

• Benchtop and floor standingunits satisfy any laboratoryspace requirement.

• Excellent graphical interfaceoffers manual control of allinstrument functions. It alsoaids in maintenance and systemdiagnostics.

Meets the most rigoroustechnical demands

• Separate sample cell transduc-ers monitor equilibration in thesmallest possible volume. Thisgives maximum sensitivitywhile a sample cell is isolatedfrom the dosing manifold.

• Dedicated Po transducerupdates each data point formaximum accuracy of surfacearea and pore sizemeasurements.

• Sample preparation underhigh vacuum of turbo-molecular pump offers a morecomplete degassing.

• Welded, stainless steel dosingmanifold ensures compati-bility with a wide range ofgases and contamination-freeoperation.

• Thermistor sensor coolantlevel control withTempComp™ for improvedvoid volume accuracy andsensitivity.

• Built-in, automated calibrationmaintains optimum perform-ance consistent with ISO 9000requirements.

• Onboard computer contin-uously monitors the dosingmanifold temperature andautomatically compensates forenvironmental temperaturechanges.

Feature-rich, extra touchesdefine quality

• Oil-free turbomolecular dragpump eliminates oil backstream-ing ( -MP and -C models).

• Cold trap eliminates degasbyproducts.

• Tandem manifolds for lowmaintenance, high efficiencysingle vacuum system.

Comprehensive, advancedchemisorption capabilities

• Fully integrated chemisorptionoption with small bench-spacerequirements.

• PC programmable temperaturecontroller with auto-tuningfunctions offers limitlessnumber of preparation routineswith guaranteed temperatureaccuracy.

• Automatic repeat measurementof isotherm following evacua-tion provides complete weakand strong chemisorption datawithout operator intervention.

• Multiple, sequential unattendedmeasurements at operatorselected temperatures.

The AUTOSORB-1-C has auto-matic valves for active andtreatment gas selection, built-ingas flow meter and temperatureprogrammer.

Multifunction temperature/pressure meter displays:• manifold pressure• manifold and degas

temperatures• station pressure• saturated vapor pressure

Vacuum pump for analysis anddegassing stations (inside cabinet)

• Oil-free turbomolecular vacuumpump ( -MP and -C models)

Heating mantle digitaltemperature controls

AUTOSORB-1-MP and -Cmodels provide sample prepa-ration in an oil-free vacuum atthe same high vacuum asrequired for analysis. The spe-cial needs of chemisorptionpreparation are achieved withmultiple gas inputs featuringautomatic switching. Flowrates for preparation are userselectable for each gas usingthe built-in flow meter. A pro-grammable temperature con-troller provides linear heatingrates for the furnace

Vapor Sorption option w/ heatedmanifold and vapor generator

Sample preparation stations(four with Degas Doubler)

Gas inlet portslocated on rear panel

Functional Capability by Model

Number of pressure transducersVery low surface area analysis with kryptonSample preparation by high vacuumAutomatic gas switching (5 ports)Sample preparation/activation by gas flowAvailable vapor sorption option

AUTOSORB-1

AUTOSORB-1-MP

AUTOSORB-1-C

3–––––

5

––

5

Pressure Transducers (per manufacturer’s specifications)0 to 1,000 torr yes yes

Accuracy: ±0.11% full scaleMinimum resolvable pressure: 2.5 x10-4 torrMinimum resolvable relative pressure (P/Po): 3 x 10-7 (nitrogen)

0 to 10 torr [Optional 0 -1 torr] no yes [yes]Accuracy: ±0.15 % readingMinimum resolvable pressure: 2.5 x 10-6 torr [2.5 x 10-7 torr]MInimum resolvable relative pressure (P/Po): 3 x 10-9 [3 x 10-10] (nitrogen), 7.6 x 10-5 (krypton)

Ultimate Vacuum (per manufacturer’s specifications)Vacuum Pump: 1.1 x 10-3 torr yes yesTurbo Molecular Pump: <5 x 10-9 torr no yes

AdsorbatesNon-corrosive gas (N2, Ar, CO2, C4H10, etc.) yes yesKrypton gas no yesCorrosive vapors (NH3, cyclohexane, etc.) no optionalProgrammable 5-gas switching no no

Temperature CapabilitiesDegas Heating Mantles (2 stations) yes yes

Heating up to 400°C in steps of 1°CAccuracy within 5°C of set pointOptional quartz mantles for higher temperatures

Analysis Heating Furnace no noHeating to 1,100°C with automatic calibrationProgrammed ramp rates from 1 to 50°C/min.Unlimited number of heating/cooling programs

Auto-Leveling Cooling Bath yes yesTwo liter standard (60 hours)

One liter, wide mouth (optional)

SPECIFICATIONS AUTOSORB-1General Physisorption

Measurement

AUTOSORB-1-MPDetailed Micropore

Characterization

Physical

Operating Temperature10°C to 38°C, non-condensing

Electrical100 to 240 V, 50/60 Hz750 VA without furnace1200 VA with furnace

DimensionsWidth : 25.5 in. (63.5 cm)Depth: 29.0 in. (72.2 cm)Height: 40.0 in. (99.6 cm)

WeightInstalled: 335 lbs. (161 kg)Includes internal vacuum pump(s)

Steel ConstructionCabinet and optional rolling cart

Performance

Surface Area AnalysisNitrogen range:

From 0.05 m2/g tono known upper limit

Krypton range:From 0.0005 m2/g tono known upper limit

Pore AnalysisDetectable volume limit:

<0.0001 cc/gPore diameter range:

3.5 to 5000 ångströmswith nitrogen

Analysis StationComponents

1 Sample cell with dedicatedpressure transducer(s)

1 Saturated vapor pressure(Po) cell with dedicatedtransducer

1 Dewar bath level sensorfor liquid coolant or slurries

Sample Cell VolumesStem OD

6 mm 9 mm 12 mmSmallPellet 1.40 cm3 1.80 cm3 2.40 cm3

LargePellet 5.50 cm3 5.50 cm3 5.50 cm3

Micro-Powder 0.34 cm3

Macro 18.50 cm3

Special cells available upon request.

yes

yes [yes]

yesyes

yesyesyesyes

yes

yes

yes

AUTOSORB-1-CChemisorption and

Physisorption Capability

System Requirements

Computer, Recommended:Pentium, 16Mb RAM, mouse,color printer

Operating System:MS Windows 98 or higher

• AUTOSORB® 6B & 3B for automated, inde-pendent multiple sample sorption measurements.

• CHEMBET™-3000 TPR/TPD for chemisorptionstudies and catalyst characterization.

• NOVA® Series for simultaneous gas sorptionanalysis of 1, 2, 3 or 4 samples

• MONOSORB® for automated single point B.E.T.surface area determinations.

• HYDROSORB™ for water vapor sorption analysis.

• THERMOFLOWTM degassing instruments.

• FLOW CONTROLLER for gas mixing.

• POREMASTER® Series Mercury porosimeters(60,000 psi and 33,000 psi) for a full range ofpore size distribution.

• ULTRAPYCNOMETERTM 1000 & MICRO-ULTRAPYCNOMETERTM, PENTAPYCNOMETERTM, & ULTRAFOAMTM

PYCNOMETER for automatic volume and truedensity measurements.

• MULTI & STEREOPYCNOMETERSTM

for manual volume and true density measurements.

• AUTOTAPTM & DUAL AUTOTAPTM for tapdensity, Hausner/Carr's, and geometric density.

• SIEVING & ROTARY MICRO RIFFLERSTM

for accurate representative sampling of powders.

• REFERENCE MATERIALS for surface area,metal dispersion, pore volume and pore size.

Exclusive International RepresentativesQuantachrome Sales Offices & US Representatives

Other Fine Products from QuantachromeQuantachrome manufactures a full range of particle technology characterization instruments, including:

Global Network of DistributorsWith more than 50 offices worldwide, Quantachrome’s distribution network delivers products and supporton a global basis...truly a single source for all your particle characterization instruments.

You can depend on our staff for on-site installationand service, prompt factory repairs, and telephonetroubleshooting support.

The purchase of a Quantachrome product signifies thebeginning of a long term relationship, with a goal toensure the maximum return on your investment.

Prompt, Dependable Service… WorldwideAt Quantachrome, reliability means more than product performance...it means responsiveness.

Serving Porous Materials and PowderCharacterizationNeeds Since 1968

www.quantachrome.comTrademarks and registered trademarks arethe property of their respective owners.

Our policy of continuous development may cause the information and specifications contained herein to change without notice or liability.

WORLDWIDE SaLES anD SERvIcE

For more than 38 years, Quantachrome’s scientists and engineers have revolutionized measurement techniques and designed instrumentation to enable the accurate, precise, and reliable characterization of powdered and porous materials:

• Adsorption/Desorption Isotherms• Surface Area Measurement• Pore Size Distribution• Chemisorption Studies• Water Sorption Behavior• Mercury Porosimetry• True Solid Density• Tapped Density

Not only are Quantachrome products the instruments of choice in academia, but the technology conceived and developed by our expert staff is applied in industrial laboratories worldwide, where research and engineering of new and improved porous materials is ongoing.

Manufacturers also rely on porous materials characterization technology to more precisely specify bulk materials, to control quality, and to isolate the source of production problems with greater efficiency.

Quantachrome is also recognized as an excellent resource for authoritative analysis of your samples in our fully equipped, state-of-the-art powder characterization laboratory.

Quantachrome Instruments’ corporate headquarters in Boynton Beach, Florida.

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Quantachrome® Renowned innovator of ideas for today’s porous materials community.

CORPORATE HEADQUARTERSQuantachrome Instruments 1900 Corporate DriveBoynton Beach, FL 33426 USAPhone: +1 (561) 731-4999Fax: +1 (561) 732-9888E-mail: qc.sales@quantachrome.com

CHINAQuantachrome Representative Office Rm. 1701B, Everbright BuildingNo. 6 Fuxing Men Wai StreetBeijing 100045 ChinaPhone: 010-68561530; 010-68560808-172Fax: 010-68561530; 010-68029962

EUROPEQuantachrome UK Limited Pale Lane Farm, Pale LaneHartley Wintney Hook RG27 8BA, UKPhone: +44 (0) 1252819719Fax: +44 (0) 1252819901

EUROPEQuantachrome GmbH & Co. KG Rudolf-Diesel Str. 1285235 Odelzhausen, GermanyPhone: +49 (0) 8134/93240Fax: +49 (0) 8134/932425

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