ACCUPYC II

Accupyc II gas displacement pycnometry system

Accupyc II AppLIcATIONS Gas Displacement pycnometry System Gas pycnometry is recognized as one of the most reliable techniques for obtaining true, absolute, skeletal, and apparent volume and densi- Application Discussion Reference ty. This technique is non-destructive as it uses the gas displacement Results of many intermediate and final processing steps are controlled by or method to measure volume. Inert gases, such as helium or nitrogen, related to skeletal density of the metal. In addition, the performance of many are used as the displacement medium. Density calculations using the Powder sintered or cast metal structures may be predicted from the skeletal density of gas displacement method are much more accurate and reproducible Metallurgy the starting metal powder. than the traditional Archimedes water displacement method. The AccuPyc II 1340 Series Pycnometers are fast, fully automatic pycnometers that provide high-speed, high-precision volume True density is a useful value for: classification, detecting differences in chemi- measurements and true density calculations on a wide variety of cal composition between supposedly similar samples, indicating Refractory powders, solids, and slurries. The instrument completes most sample mineralogical phases or phase changes, calculating total porosity when the ASTM C604-02Materials analyses in less than three minutes without sacrificing bulk density is known, and for any other test method that requires this value accuracy. After analyses are started with a few keystrokes, data are for the calculation of results. collected, calculations are performed, and results displayed. A minimal amount of operator attention is required. The density of calcined petroleum coke directly influences the physical and Calcined chemical properties of the manufactured carbon and graphite artifacts for Petroleum which it is used. Density, therefore, is a major quality specification of calcined ASTM D2638-10 Coke petroleum coke and is used as a control in coke calcination. Benefits The specific gravity of soils that contain extraneous matter (such as cement, lime, etc.) or water-soluble material (such as salt) must be corrected because of the precipitate that forms on the specimen after drying. If the precipitate Soil ASTM D5550-06 has a specific gravity less than the parent soil grains, the uncorrected test Maintain product integrity with this Minimize cost and space requirements - result will be too low. If the precipitate has a higher specific gravity, then the non-destructive test low maintenance and small footprint uncorrected test value will be too high. Total solids content can be used to determine minimum coverage obtainable Powder with different coating blends. Mixtures of dry pigments can be monitored by Coatings comparing measured density with theoretical density based upon composition ASTM D5965-20 Adapt instrument configuration to Operate with either a keypad or of the mixture. ® meet your sample size needs Windows software Clear or Dried film density can be used in the determination of Volatile Organic Pigmented Compound (VOC) content of clear and pigmented coatings. VOC is required ASTM D6093-97 Coatings by government regulations. Maximize your results with superior speed of analysis, accuracy, Use a variety of gases Plastic foams exhibit different properties based upon the ratio of open and repeatability, and reproducibility Rigid Cellular closed cells. Insulation foams limit thermal conductivity through pockets of ASTM D6226-10 Plastics trapped gases contained within closed pores. Flotation devices owe buoyancy to closed air-filled pores that prohibit water entry. Eliminate error with programmable automatic repeat and data acquisition Increase efficiency and compliance Composition of active and excipient ingredients can be monitored and set to your tolerances to comply with with barcoding compatibility controlled through determination of product density. Polymorphic, hydrated, your SOPs Pharmaceuticals and amorphous forms of products, as well as purity, can be determined by USP 699 comparing measured density with theoretical and historical values. Eliminate procedural steps with direct input from an analytical balance 8g More instruments, in more countries, to more satisfied users

DENSITy MEASuREMENT On an elementary level, the volume of a solid material can be calculated by measuring its length, width, and thickness. However, many materials have within their structure surface irregularities, small fractures, fissures, and pores. Some of these voids or pores Fertilizers are open to the surface or closed within the structure of the solid A single particle containing Knowledge of the bulk density is of material. Therefore, differences in the material volume depend on open and closed pores interest in package sizing, in calibrating the measurement technique, measurement method, and the volumetric feeders or applicators, and in conditions under which the measurements were performed. determining the storage capacity of bins and transport vehicles. Apparent density Assemblage of porous Interparticle void information can be used in segregation particles in a container studies and development of granulation particle Volume processes. True density measurements are important in process control and the design of process equipment. Mining cores Simple physical measurements of a circular core cylinder’s diameter and length allow the envelope volume to be calculated. A The envelope gas displacement pycnometer, with a larger sample chamber designed specifically to accept intact drill cores, provides a low-cost, Surface void time-saving, non-destructive technique for included within measuring the skeletal volume. Knowing the the envelope envelope and skeletal volumes allows the total pore volume and percent porosity of the core sample to be determined. Density Volumes Included in Definition Material Open-Pore Closed-Pore Inter particle External Density Type Definition Volume Volume Volume Volume Void Volume Addressed by The mass of a substance divided True by its volume, excluding open AccuPyc II (Absolute) and closed (or blind) pores The ratio of the mass of the solid cosmetics Skeletal material to the sum of the volume AccuPyc II The presence of air bubbles in cosmetic (Apparent) including closed (or blind) pores preparations, such as lipsticks and powder cakes, is undesirable for a The ratio of the mass of a number of reasons. Trapped air can substance to the envelope create pinholes and poor appearance in Envelope GeoPyc volume (imaginary boundary lipsticks and compromise the integrity surrounding the particle) of cakes. The effectiveness of different methods of air bubble removal can be Mass of the material divided evaluated by comparing the true density Bulk by the volume occupied that GeoPyc measurements of the material before includes interstitial space and after air bubble removal. Apparent powder density Tap obtained under stated GeoPyc with conditions of tapping T.A.P. function

GAS DISpLAcEMENT pycNOMETRy principle of Operation This technique uses the gas displacement method to Inert gas flows Equilibrium is reached measure volume accurately. Inert gases, such as helium or nitrogen, are used as the displacement medium. The sample 1 Into sample chamber 4 yet again is sealed in the instrument compartment of known volume, valve a opens then closes the appropriate inert gas is admitted, and then expanded into Volume divided into another precision internal volume. The pressures observed upon filling the sample chamber and then discharging it into Equilibrium is sample weight a second empty chamber allow computation of the sample 2 reached 5 solid phase volume. Helium molecules rapidly fill pores as determines density small as one angstrom in diameter; only the solid phase of the sample displaces the gas. Dividing this volume into the Gas flows into sample weight gives the gas displacement density. 3 second chamber Pressure ventedfor volume measurement 6 off to atmosphere valve b opens valve c opens 2 4 3 5 Density 1 sample 6 Every Eight Hours – A Technical Paper Citing a Micromeritics instrument is Accepted for Publication in a Scientific Journal

HIGHLy ADApTIVE SySTEM Direct sample mass input The AccuPyc II Pycnometer consists of an integrated control and Sample mass may be directly input from corepyc*** analysis module. For those who require high throughput, analysis an analytical balance modules are also available in a single configuration, allowing you to Specialized unit with attach up to five additional analysis modules to a single controlling 2000-cm3 sample chamber size unit. Each module has its own gas connection. A variety of sample chamber sizes can be selected to provide the best fit with your samples. The run precision mode allows you to achieve high repeat- ability. The instrument automatically purges water and volatiles from the sample and then repeats the analysis until successive measure- ments converge upon a consistent result. Integrated control and analysis module unique run Can control up to five additional external analysis modules precision Increases the precision of analysis results by reporting data from five consecutive measurements that are within a user-specified tolerance. This feature allows early termination of analysis, thereby decreasing the number of cycles needed for accurate results. Multilingual The AccuPyc may be operated in five languages: English, French, German, Italian, or Spanish Five standard Ethernet port sample chamber An Ethernet port on the rear panel of sizes the control module enables you to email 3 3 3 3 reports, send data to a web browser for 1 cm , 10 cm , 100 cm , 350 cm , and 3 archiving, or interface with the AccuPyc 2000 cm *** Windows application uSB ports Simple calibration Bayonet cap fitting Provides superior repeatable seal compared USB ports on the rear panel of the process to screw-type fitting control module allow for connection to a printer (output of analysis and Allows you to easily determine the volume of the calibration results in either ascii or excel instrument sample cell and expansion chambers formats) and keyboard (alphanumeric using a traceable standard volume. After character input). The USB port is also calibration, the cell and expansion chamber used for installing software upgrades volumes are stored automatically 2000 cm3 350 cm3 100 cm3 10 cm3 1 cm3

MODEL SELEcTION HARDWARE Sample Sample Available Temp Catalog Chamber Chamber MultiVolume Control Number Capacity Dimensions Insert Kits Type VERSATILITy AccuPyc II 1 cm3 1-cm ID x 1.1-cm D 0.1 cm3 134/00001/00 MultiVolume Kits 10 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 N/A 134/00000/00 A MultiVolume option allowing you to analyze smaller-sized samples with your current AccuPyc model is available for 100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 134/00002/00 configurations listed below; Each kit includes appropriate insert(s), reference standard(s), and AccuPyc II 1340 Remote Analysis Instruments sample cup(s). Bundle includes Control module and 2-ft cable connected to Analysis modules. 2000-cm3 nominal cell volume 650- and 1300-cm3 cups 1 cm3 1-cm ID x 1.1-cm D 0.1 cm3 134/00031/00 AccuPyc II Bundle 10 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 134/00030/00 100-cm3 nominal cell volume 3 100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 N/A 134/00032/00 10- and 35-cm cups 350 cm3 5.84-cm ID x 13.94-cm D NA 134/00033/00 10-cm3 nominal cell volume 2000 cm3 9.7-cm ID x 26.00-cm D 650 and 1300 cm3 134/00034/00 1- and 3.5-cm3 cups Remote analysis modules only. Remote analysis units require connection to a control module 1-cm3 nominal cell volume or AccuPyc II 1340 0.1-cm3 cup Remote Analysis Module Only 1 cm3 1-cm ID x 1.1-cm D 0.1 cm3 134/00041/00 10 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 134/00040/00 100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 N/A 134/00042/00 SOFTWARE VERSATILITy 350 cm3 5.84-cm ID x 13.94-cm D NA 134/00043/00 Data presentation 2000 cm3 9.7-cm ID x 26.00-cm D 650 and 1300 cm3 134/00046/00 Density vs Cycle # The AccuPyc II can be operated with a keypad or an optional Average: 3.8691 g/cm³ Standard Deviation: 0.0123 g/cm³Density vs Cycle # Windows® interface that provides exceptional reporting and 3.895 Control Module Only archiving capability. Both versions include direct sample mass input Control module only. Up to 5 analysis modules can be connected to a single control module. 3.890from a balance and cycle-based displacement volume reporting. With the Windows interface, features such as time-based pressure 3.885 N/A N/A N/A N/A 134/00005/00 equilibration reporting and additional calculations such as percent 3.880 solids content and total pore volume are included. Operational status can also be continually monitored in a status window on the 3.875 AccuPyc II 1340 Temperature - Controlled Instruments monitor screen. Equilibration Repo3.8r7t0 10 cm3 1.80-cm ID x 3.93-cm D 3 • Combined Report P2 (Expansion Pressure) shown every 1 second(s) 1.0 and 3.5 cm Use with External 134/00010/00 Cycle #1 Cycle #2 Cycle #3 Cycle #4 3.865 Cycle #5 Cycle #6AccuPyc II TC Cycle #7 Cycle #8 3 Recirculating Bath100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm 134/00020/00 • Summary Report 18 3.860 AccuPyc II TEC 15-50 ˚C 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5V.0 o5.l5. v6.0s6 .C5 y7.0cl7.e5 #8.0 8.5 9.0 9.5 10.0 17 Cycle Number • User-Defined Tabular Reports Average: 6.3725 cm³ Standard Deviation: 0.0004 cm³ Vol. vs Cycle # Reference 10 cm3 1.80-cm ID x 3.93-cm D 3 Sigma+/- 1.0 and 3.5 cm Integral Thermo- 134/00050/00 16 6.378 Min/Max• Volume vs. Cycle # Electric Cooling, 15 100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 15-36 ˚C, ± 0.1 ˚C* 134/00051/00 6.376• Density vs. Time 14 6.374 • Total Pore Volume vs. Temperature 13 6.372 • Density vs. Cycle # 12 10 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 Use with External 134/00044/00 11 6.370 4.62-cm ID x 6.17-cm D 3 Recirculating Bath 134/00045/00 • Options Report 0 2 4 6 8 10 12 14 16 18 20 22 24 26100 cm3 10 and 35 cm Time (seconds)15-50 ˚C 6.368 • Equilibration Report FPO Research grade helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or 6.366 argon may be used. A multigas option for up to four gases on one analysis unit is available. 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0• Sample Log Cycle Number *Subject to environmental operating conditions P2 (Expansion Pressure) (psig) Density (g/cm³) Volume (cm³)

pOROSITy SOLuTION FOAM SOLuTION Total pore Volume/percent porosity Bundle Foampyc Bundle – Density Measurements for pharmaceutical Applications Open- and closed-cell Foams While skeletal and envelope volume measurements are each The AccuPyc II unit can be ordered initially with the FoamPyc important on their own merit, their combination also allows you to application installed. If you have a standard AccuPyc, you can accurately calculate percent porosity and total pore volume of a upgrade with a software enhancement. A FoamPyc option for body. measuring open- and closed-cell foam materials is available in the following configurations for the standard and temperature-controlled pycnometers: • 10-cm3 nominal cell volume (for conformance to ASTM and ISO methods) • 100-cm3 nominal cell volume WEIGHING SOLuTION Analytical Balance Bundle The AccuPyc weighing solution bundle provides one-touch transfer of mass data from the analytical balance directly to the AccuPyc’s Tablet press pharmaceutical Ribbons Windows software. Direct transfer eliminates user error associated Pharmaceutical scientists realize that many of the physical, me- With the skeletal density measured by the AccuPyc included in the with manual entry of mass data. Optional Peltier temperature con- chanical, and pharmacokinetics properties of tablets are influenced setup parameters for the envelope density, the GeoPyc will calcu- trol eliminates environmental temperature variation and facilitates by the basic settings of a tablet press. Using the AccuPyc coupled late and report the percent porosity and total pore volume of the the handling of “hot” samples. with the GeoPyc, scientists are now able to determine quickly and ribbon. This information has proven to be useful in controlling the • Optional Peltier thermoelectric control easily the skeletal density, envelope density, total pore volume, mechanical properties of the material, compression force settings (15 to 36 oC) provides ambient temperature percent porosity, and closed-cell pore volume of tablets produced on the roller compactor, and subsequent tablet press settings. stability with varying press settings. • Seamless device compatibility Geopyc Accupyc/Geopyc* • One-touch mass data transfer to Envelope Density Analyzer AccuPyc for automatic calculation of density The GeoPyc utilizes a quasi-fluid displacement medium composed of non-hazardous microspheres having a high degree of flowability • Includes 120 X 0.01 mg electronic that do not wet the sample or fill its pores. analytical balance with calibration weight • Determines envelope volume and density of monolithic samples as well as bulk volume and density of powdered materials • A variety of sample chambers is available to accommodate a wide range of sample sizes • T.A.P. Density option – measures the packing volume and calculates the *included in porosity bundle bulk density of granular and powdered samples Superior Worldwide Support Assures You Consistent Instrument Performance for Years to Come

TEMpERATuRE-cONTROL SOLuTION HIGH-pRESSuRE SOLuTION Accupyc II Hp – Density Determinations in a High-pressure Environment Accupyc II TEc - Density Testing for Semi-Solid Bituminous Materials This pycnometer can provide high-speed, high-precision volume measurements and density determinations in an elevated pressure This AccuPyc solution can be closely correlated (< 0.15% difference) environment (i.e. intact or crushed shale core samples). to results obtained with ASTM Test Method D70-09. The ASTM method is burdensome and time consuming. Our approach offers an • Operates at a higher pressure of 500 psi to provide a better expedited, more robust, operator-independent method, with results diffusion of the gas into the rock in minutes. • Stainless-steel sample chamber with a volume of 100 cm3 • Reproducible results in minutes, virtually eliminates • Sample chamber can accommodate a 48-mm (1.85 in.) operator error diameter core of up to 60 mm (2.40 in.) in length • Integral solution with software for bituminous material testing includes results for specific gravity, volume, and density • Peltier thermoelectric control (15 to 36 °C) provides excellent temperature control/stability and sample handling • Disposable sample cups limit cross-contamination and minimize cleaning of sample chamber between analyses LARGE VOLuME SOLuTION Asphalt Analysis core pyc – Density of Intact core Samples Average Density %Relative Stan- ASTM Method %Difference With a large-volume sample chamber, this pycnometer has been Asphalt Sample AccuPyc II TEC dard Deviation Solution D70-9 Density Between Methods designed to address the specific needs of operations that require (n=11) (g/cc) pore volume knowledge of intact drilling cores. This instrument (n=11) (g/cc) improves sampling statistics by eliminating the need to break a core into many smaller pieces and run multiple analyses to obtain volume Sample A 1.01906 0.03 1.01758 0.1453 results. The CorePyc eliminates the need to run multiple analyses on large cores. Sample B 1.02543 0.03 1.02536 0.0067 • Large sample chamber with a volume of Sample C 1.01821 0.07 1.01848 0.0263 approximately 2000 cm3 Sample D 1.02563 0.09 1.02576 0.0125 • Sample chamber can accommodate a 95-mm (3.74 in.) diameter core of up to Samples varied in composition and viscosity 278 mm (10.9 inches) in length If your research work requires an analytical device, technique, or CUSTOM configuration that is not commercially available, talk to us about modifications to our standard instrument designs. There are no charges associated with the initial consultation and our research ENGINEERED into the feasibility of your project. PRODUCTS Call us here: 770.662.3698 Focused on your Solution

Height: 17.9 cm (7.0 in.), analysis modules for 1-, 10-, and 100-cm3 units, and control module 25.9 cm (10.2 in.), 350-cm3 analysis module 43.0 cm (17.0 in.), 2000-cm3 analysis module Width: 27.3 cm (10.7 in.), control module 27.3 cm (10.7 in.), control module 27.0 cm (10.6 in.), 2000-cm3 analysis module Depth: 36.2 cm (14.3 in.) Weight: 9.3 kg (20.5 lbs), control/analysis unit (1-, 10-, and 100-cm3 units) 7.9 kg (17.4 lbs), analysis module (1-, 10-, and 100-cm3 units) Micromeritics Instrument 10.5 kg (23.2 lbs), analysis module (350-cm3 unit) corporation 3.6 kg (8.0 lbs), control module 26.0 kg (57.0 lbs), 2000-cm3 analysis module 4356 Communications Drive Norcross, GA 30093 U.S.A. Electrical: To request a quote or additional product information, Voltage - 90 to 264 VAC Power - 30 VA visit Micromeritics website at: Frequency - 50 to 60 Hz www.micromeritics.com Contact your local Micromeritics sales representative, or Precision: our Customer Service Department at: Reproducibility typically to within ± 0.01% of the nominal 770.662.3636 full-scale sample cell chamber volume. Reproducibility guaranteed to within ± 0.02% of the nominal full-scale volume on clean, dry, thermally equilibrated samples using helium in the 15 to 35 ºC range. The Micromeritics Accuracy: Accurate to within 0.03% of reading, plus 0.03% of sample customer Experience... capacity. “ Micromeritics Instruments are easy to © All Rights Reserved 2014. Micromeritics Instrument Corporation. Norcross, GA 30093. 770.662.3636. Printed in U.S.A. use and yield powerful results. The tech and applications support professionals are responsive and knowledgeable” -Brenda Fisher, Lab Manager, Cornell University TechValidate Research Study, Nov 2014 134/42701/00