Gas Displacement Pycnometry System

AccuPyc™ II 1340

Highly Adaptable Density Determinations

The AccuPyc II 1340 Gas Displacement Pycnometry System

Gas pycnometry is a common analyticaltechnique that uses a gas displacementmethod to measure volume accurately. Inertgases, such as helium or nitrogen, are usedas the displacement medium. The sample issealed in the instrument compartment ofknown volume, the appropriate inert gas isadmitted, and then expanded into anotherprecision internal volume. The pressurebefore and after expansion is measured andused to compute the sample volume.Dividing this volume into the sample weightgives the gas displacement density.

The AccuPyc II 1340 Series Pycnometersare fast, fully automatic pycnometers that provide high-speed, high-precision volumemeasurements and density calculations on awide variety of powders, solids, and slurrieshaving volumes from 0.01 to 350 cm3. Theinstrument completes most sample analysesin less than three minutes with excellentaccuracy. After analyses are started with afew keystrokes, data are collected, calcula-tions are performed, and results displayedwithout further operator intervention.

Wide Variety of StandardFeatures

• Simple calibration process allows theuser to determine easily the volume ofthe instrument sample cell and expansionchambers using a traceable standard volume. After calibration, the cell andexpansion chamber volumes are stored automatically.

• A unique run precision feature increasesthe precision of analysis results byreporting data from five consecutivemeasurements that are within a user-specified tolerance. This feature allowsearly termination of analysis, therebydecreasing the number of cycles neededfor accurate results.

• Sample mass may be directly input from an analytical balance through an RS-232 port.

• USB ports on the rear panel of the controlmodule allow for connection to a printer(output of analysis and calibrationresults) and keyboard (alphanumericcharacter input). The USB port is alsoused for installing software upgrades.

• An Ethernet port on the rear panel of thecontrol module enables the user to e-mailreports, send data to a web browser forarchiving, or interface with the AccuPycII 1340 Windows® application.

• The AccuPyc may be operated in five different languages: English, French,German, Italian, or Spanish.

The AccuPyc II 1340 Pycnometer consists ofan integrated control and analysis module.For those who require high throughput,analysis modules are also available in a singleunit configuration, allowing you to attach upto five additional analysis modules to a singlecontrolling unit. Each module has its owngas connection. In addition, each modulecan contain a different size sample chamber(1 cm3, 10 cm3, 100 cm3, or 350 cm3) providingeven more versatility.

Wide Variety of Options

• Optional Windows interface providesexceptional reporting and archiving capability.

• Integrated control and analysis modulecan control up to five additional externalanalysis modules.

• Four standard sample chamber sizes areavailable - 1 cm3, 10 cm3, 100 cm3, and350 cm3.

• MultiVolume Option Kits allow analysesof a variety of sample sizes in one analytical module.

• Allows measuring of open- and closed-cell foam materials in accordance with ASTM method D 6226.

• Temperature-control version allowsanalysis at user-selectable temperatures.

• Glove box model separates the controland analysis modules, allowing analysisin controlled environments.

The AccuPyc II integrated control/analysis module with

an additional analysis module – up to five additional analysis

modules can be operated by a single control/analysis module.

Typical AccuPyc II 1340Applications

Pharmaceuticals – Composition of activeand excipient ingredients can be monitoredand controlled through determination ofproduct density. Polymorphic, hydrated, andamorphous forms of products, as well aspurity, can be determined by comparingmeasured density with theoretical and historical values.

Coatings – Dried film density can be usedin determination of Volatile OrganicCompound (VOC) content of clear and pig-mented coatings. VOC reporting is requiredby government regulations. In addition, totalsolids content can be used to determineminimum coverage obtainable with differentcoating blends. Mixtures of dry pigmentscan be monitored by comparing measureddensity with theoretical density based uponcomposition of the mixture.

Calcination – Many materials undergostructural rearrangement through pressureor temperature treatment, or both.Conversion level can be monitored throughdensity measurement during and at the endof processing. SPC reporting of results facilitates monitoring of product control.Applications include different crystal structures of carbon and ceramics.

Ceramics and powder metallurgy –Density measurements can be used to deter-mine closed porosity from casting, sintering,and forging operations where parts aremade from powdered samples. If the densityof the finished part is significantly less thanthat of the constituent powder, closed poreshave formed during the part processing.

Rigid cellular plastics – Closed-cell rigidplastics (foams) exhibit different propertiesbased upon the ratio of open and closedcells. Insulation foams limit thermal con-ductivity through pockets of trapped gasescontained within closed pores. Flotationdevices, likewise, owe buoyancy to closedair-filled pores that prohibit water entry.

Plastic films – Plastic films are producedthrough extrusion of plastic beads. Filmquality is related to the amount of encapsu-lated air in the starting beads. Density can beused to determine the quantity of entrappedair. In addition, the degree of crystallinity of the final film can be determined usingdensity. Brittleness of the film increaseswith crystallinity, while strength decreases.

Slurries – With knowledge of the dry powder and suspending liquid densities, the quantity of liquid in a slurry mixture can be calculated by measuring the densityof the slurry. Generally it is expensive to shipexcess liquid in slurries, and then to removesuspending liquid before casting operations.On the other hand, too little suspendingfluid can lead to difficulty in transportingthe slurry due to unfavorable rheologicalproperties of the slurry when the solids con-tent is too high. These rheological proper-ties can be monitored by measuring the den-sity of the slurry.

Organic chemicals and polymers –Polymerization and organic reformingprocesses are used to produce desired com-pounds from raw materials. Conversion andpurity can be monitored by comparingmeasured density to theoretical density ofthe desired product.

Blending of materials – Many powderproducts are shipped and used as blends ofprimary ingredients. The accuracy andreproducibility of the blend can be monitoredby comparing the measured densities to theexpected density based upon the targetrecipe of primary ingredients. The highdegree of accuracy and precision of theAccuPyc helps ensure that the blends produced at a given plant match the desiredrecipe, the previous lots of materials, andthose from other locations, regardless of theindustry where these blends are used.

Hardware and Software Versatility

Configurations

To ensure best fit with your sample, theAccuPyc is available in multiple configura-tions. Best fit means your sample nearly fillsthe sample chamber and, therefore, optimizesthe precision of your results. • 1-cm3 sample chamber

• 10-cm3 sample chamber

• 100-cm3 sample chamber

• 350-cm3 sample chamber

Temperature Control Option

The temperature-control unit is specificallydesigned for temperature-sensitive materials.This unit permits collection of volume/densitydata at a user-specified temperature. A temperature-control unit to which an externalbath is connected is available in the followingconfigurations:• 10-cm3 sample chamber

• 100-cm3 sample chamber

Glove Box Option

This unit consists of two separate modules.The controller is placed outside the glovebox, while the analysis module is placedinside the glove box. If you have an existingAccuPyc II 1340, you can order the glove boxanalysis unit containing the desired samplechamber and simply connect it to the connec-tor provided on the rear panel of the existingAccuPyc II. A glove box unit for analysis ofsamples in which a controlled environment is required is available in the following configurations:• 1-cm3 sample chamber

• 10-cm3 sample chamber

• 100-cm3 sample chamber

• 350-cm3 sample chamber

FoamPyc Option

The AccuPyc II 1340 unit can be orderedwith the FoamPyc application installed. Ifyou have a standard AccuPyc II 1340, you canupgrade with a software enhancement. AFoamPyc option for measuring open- andclosed-cell foam materials is available in thefollowing configurations for the standard andtemperature-control pycnometers:• 10-cm3 nominal cell volume

• 100-cm3 nominal cell volume (for confor-mance to ASTM and ISO methods)

MultiVolume Option

A MultiVolume option allowing you to analyzesmaller-sized samples with your currentAccuPyc model is available for the followingconfigurations:• 1-cm3 nominal cell volume, contains

a 0.1-cm3 cup

• 10-cm3 nominal cell volume, contains 1- and 3.5-cm3 cups

• 100-cm3 nominal cell volume, contains 10- and 35-cm3 cups

Analysis module

Glove Box controller

Software and Data Presentation

The AccuPyc II 1340 can be operated with akeypad or an optional Windows interfacethat provides exceptional reporting andarchiving capability. Both versions includedirect sample mass input from an analyticalbalance and cycle-based displacement vol-ume reporting. With the Windows interface, features such as time-based pressure equili-bration reporting and additional calculationssuch as percent solids content and totalpore volume are included. Operational statuscan also be continually monitored in a statuswindow on the monitor screen.

To request a quote or additional product information,

visit Micromeritics’ web site at www.micromeritics.com,

contact your local Micromeritics sales representative,

or our Customer Service Department at (770) 662-3636.

User-selected reports include:• Summary Report

• User-Defined Tabular Reports

• Volume vs. Cycle #

• Density vs. Temperature

• Total Pore Volume vs. Time

• Density vs. Cycle #

• Options Report

• Equilibration Report

• Sample Log

• Combined Report

Density versus analysis cycle number for a polymer sample initially

containing volatiles. Pressure equilibration versus time plot for eight analysis cycles for glass

sample illustrating the rate at which pressure equilibrates during analysis.

Integrated control and analysis module

Density and Volume Report for analysis of garnet powder.Control chart for analyses of glass samples showing mean value and control

limits at ± 3 �.

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