QbD Solid Fraction Analysis in Roller Compaction Operations AccuPyc 1340 Gas Pycnometer GeoPyc 1365 Envelope and T.A.P. Density THE IMPORTANCE OF SOLID FRACTION DATA IN ROLLER COMPACTION OPERATIONS Roller compaction is a continuous dry granulation process used to increase the bulk density and uniformity of powders into free flowing granules used in downstream manufacturing operations. It is a complex procedure due to the diversity of available powder blends and the control and adjustment parameters involved in the process. The character and homogeneity of the produced ribbon is controlled by a number of factors, such as the properties of the individual powders themselves, roll speed, roll gap/nip angle, and feed speed; all of which subsequently determine the character of the granules produced (size distribution, density and flow behavior). It is critical to produce uniform and specified ribbon densities throughout the process, as well as throughout the ribbon itself. This is important in order to achieve repeatable tensile strength and the desired particle size distribution in the milled material. Specified ribbon densities can be achieved by maintaining equivalent compaction pressure applied by the rolls on the ribbon for a specified gap distance and speed. In pharmaceutical operations, the roller compaction process has a significant effect on the homogeneity, compactability and compressibility of the API, additive/ excipient mix. These factors have a direct influence on particle size distribution, porosity, and flowability in downstream operations, which in turn influence dissolution profiles, disintegration time, and hardness of the produced solid dosage form. 2 Regulatory agencies worldwide are now emphasizing the employment of a QbD approach. Companies are being required to show a greater understanding of the way in which variability in raw materials, process design and operating conditions affect final product quality and use this knowledge to implement effective quality control strategies. To date, roller compaction operations have utilized mostly mathematical modeling and operator experience as the identified process controls . Solid Fraction Solid Fraction, determined through instrumental methods and quantifiable data is an excellent path to achieve roller compaction operations that incorporate a QbD policy. Solid Fraction can be used as an important Critical Process Parameter (CPP) and is determined using the following formula: SF= Pe Po SF= Solid Fraction (relative density) Pe = envelope density of the ribbon Po = true density of the granules Micromeritics AccuPyc gas pycnometers are used to determine the true density of a sample. These fully automated instruments can be placed at-line or within a supporting lab. operation for manufacturing process control. They offer precise and rapid determination of the sample’s true volume and automatic calculation of density using the associated sample mass. For envelope density Micromeritics automated GeoPyc employs a unique, non-destructive, fast displacement measurement technique that uses Dry Flo, a quasi-fluid composed of small, rigid spheres having a high degree of flow-ability. The sample is placed in a bed of Dry Flo which is agitated and gently consolidated about the sample. While true and envelope volume measurements are important in their own capacities, their combination permits the pharmaceutical scientist to also accurately calculate percent porosity and total pore volume. With this data a process engineer or quality assurance scientist can better understand and optimize the manufacturing process resulting in a consistent product from one batch to the next. Employed in tandem, these two instruments can achieve data driven, instrumental analysis enabling Solid Fraction to be employed as a CCP in pharmaceutical densification operations. 3 GEOPYC 1365 Technique Envelope Density Analyzer Highly accurate and reproducible results ast operation in a small F bench-top instrument Fully automated data acquisition and reporting Nondestructive analysis maintains sample integrity The GeoPyc employs a unique displacement measurement technique that uses Dry Flo, a quasi-fluid composed of small, rigid spheres having a high degree of flow-ability. The sample is placed in a bed of Dry Flo which is agitated and gently consolidated about the sample. The GeoPyc collects the displacement data, performs the calculations, and displays or prints the results. The unit also reports percentage porosity and specific pore volume when absolute density information (density excluding pore and small cavity volume obtained from a Micromeritics AccuPyc II pycnometer) is entered. The GeoPyc automatically determines the envelope volume and density of a solid object by displacement of Dry Flo, a solid medium. The medium is a narrow distribution of small, rigid spheres that have a high degree of flow ability and achieve close packing around the object under investigation. The particles are sufficiently small that during consolidation they conform closely to the surface of the object, yet do not invade pore space. Repeatability and reproducibility are achieved by a controlled method of compaction. The sample cell in which the Dry Flo is placed is a precision cylinder. A plunger compresses the powder as the cell is oscillated; the force of compression is selectable and, therefore repeatable from test to test. A preliminary compaction with only the displacement medium in the cell establishes a zero-volume baseline. The sample is then placed in the cylinder with the Dry Flo and the compaction process is repeated. The difference in the distance ht the piston penetrates the cylinder Precision bore glass cylinder I ntelligent touch panel for ease of operation and reporting A Plunger Dry solid medium T.A.P. Density Option Baseline: Solid Medium Only in Cell A The GeoPyc T.A.P. density option obtains precise results comparable to conventional T.A.P. density analyzers, only it does it faster, quieter, and with a higher degree of reproducibility. When equipped with the T.A.P. Density option, the GeoPyc measures the packed volume and calculates the bulk density of granular and powdered samples, including pharmaceutical and electrochemical materials, under a wide range of compaction conditions. To determine T.A.P. density, the sample chamber is rotated and agitated while a user specified force is precisely applied to the sample. A force transducer measures the consolidation force in Newtons and the distance over which the piston travels is precisely monitored and recorded. The user specifies the force applied and the number of consolidations per analysis. The GeoPyc averages the measurements from each consolidation and automatically calculates volume and density, and reports the results in cm3 and g/cm3. h B during the test and the distance h0 it penetrates during the baseline procedure (h = h0– ht ) is used to calculate the volume of Dry Flo displaced using the formula for the volume of a cylinder of height h, V =π r2h The GeoPyc is operated from an intelligent touch screen. Data acquisition and reporting are fully automated for convenient incorporation in LIMS or other data collection systems. A variety of sample chambers is available to accommodate a wide range of sample sizes. After the analysis, a light shaking or dusting completely removes the Dry Flo so the samples can be reused or retested. The GeoPyc has multiple operating modes including full blank, computed blank, and reference solid calibration with variance, which allows you to optimize speed and accuracy for your individual needs. During analysis, indications of progress and preliminary results make it possible to track the progress of the experiment. Measurement: Solid Medium and Object in Cell Software The GeoPyc has multiple operational modes that are accessed through the instruments smart touch screen. Operating modes including full blank, computed blank, and reference solid calibration with variance, which allows you to optimize speed and accuracy for your specific application. During analysis, indications of progress and preliminary results make it possible to track experiment progress. Samplespecific information can be entered into the analysis reports. Available Reports: Envelope Density, Volume Calibration, Blank Report, Force Calibration, Instrument Log 4 5 GeoPyc 1365 Specifications ACCUPYC II Gas Displacement Pycnometry System Reproducibility When sample volume is at least 25% of sample holder volume: Typically ± 1.1% Gas pycnometry is recognized as one of the most reliable techniques for obtaining true, absolute, skeletal, and apparent volume and density. This technique is non-destructive as it uses the gas displacement method to measure volume. Inert gases, such as helium or nitrogen, are used as the displacement medium. Density calculations using the gas displacement method are much more accurate and reproducible than the traditional Archimedes water displacement method. Sample Chamber 12.7-mm (0.50 in.) ID Sample volumes between 0.3 cm³ and 0.8 cm³ 19.1-mm (0.75 in.) ID Sample volumes between 0.8 cm³ and 2.4 cm³ 25.4-mm (1.00 in.) ID Sample volumes between 2.4 cm³ and 5.3 cm³ 38.1-mm (1.50 in.) ID Sample volumes between 5.3 cm³ and 13 cm³ 50.8-mm (2.00 in.) ID Sample volumes between 13 cm³ and 25 cm³ Physical Height 11 in. (27.9 cm) Width 22 in. (55.9 cm) Depth 15 in. (38.1 cm) Weight 42 lbs (19 kg) Electrical Power The AccuPyc II 1340 Series Pycnometers are fast, fully automatic pycnometers that provide high-speed, high-precision volume measurements and true density calculations on a wide variety of powders, solids, and slurries. The instrument completes most sample analyses in less than three minutes without sacrificing accuracy. After analyses are started with a few keystrokes, data are collected, calculations are performed, and results displayed. A minimal amount of operator attention is required. Electrical Power 95 VA Voltage 85 to 265 VAC Frequency 47 to 63 Hz Environment Temperature 15 °C to 35 °C Humidity 20% to 80% non-condensing *Due to continuous improvements, specifications are subject to change without notice. Benefits 6 Maintain product integrity with this non-destructive test Eliminate error with programmable automatic repeat and data acquisition set to your tolerances to comply with your SOPs Use a variety of gases Adapt instrument configuration to meet your sample size needs Minimize cost and space requirements; low maintenance and small footprint Increase efficiency and compliance with barcoding compatibility Maximize your results with superior speed of analysis, accuracy, repeatability, and reproducibility Operate with either a keypad or Windows® software Eliminate procedural steps with direct input from an analytical balance 8g 7 Density Measurement Gas Displacement Pycnometry 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 are open to the surface or closed within the structure of the solid material. Therefore, differences in the material volume depend on the measurement technique, measurement method, and the conditions under which the measurements were performed. Principle of Operation A single particle containing open and closed pores This technique uses the gas displacement method to measure volume accurately. Inert gases, such as helium or nitrogen, are used as the displacement medium. The sample is sealed in the instrument compartment of known volume, the appropriate inert gas is admitted, and then expanded into another precision internal volume. The pressures observed upon filling the sample chamber and then discharging it into a second empty chamber allow computation of the sample solid phase volume. Helium molecules rapidly fill pores as small as one angstrom in diameter; only the solid phase of the sample displaces the gas. Dividing this volume into the sample weight gives the gas displacement density. Interparticle void Particle Volume Assemblage of porous particles in a container The envelope Surface void included within the envelope 2 1 Definition True (Absolute) The mass of a substance divided by its volume, excluding open and closed (or blind) pores The ratio of the mass of the solid Skeletal material to the sum of the volume (Apparent) including closed (or blind) pores 8 Material Volume Open-Pore Volume 3 5 Density sample a Density Type 4 b c 6 Closed-Pore Inter Particle External Void Addressed by Volume Volume Volume AccuPyc II AccuPyc II Envelope The ratio of the mass of a substance to the envelope volume (imaginary boundary surrounding the particle) GeoPyc Bulk Mass of the material divided by the volume occupied that includes interstitial space GeoPyc Tap Apparent powder density obtained under statedconditions of tapping GeoPyc with T.A.P. function 1. Inert gas flows Into sample chamber. Valve a opens then closes. 2. E quilibrium is reached. 3.Gas flows into second chamber for volume measurement. Valve b opens. 4.Equilibrium is reached again. 5. V olume divided into sample weight determines density. 6. P ressure vented off to atmosphere. Valve c opens. 9 Highly Adaptive System The AccuPyc II Pycnometer consists of an integrated control and analysis module. For those who require high throughput, analysis modules are also available in a single configuration, allowing you to attach up to five additional analysis modules to a single controlling 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 repeatability. The instrument automatically purges water and volatiles from the sample and then repeats the analysis until successive measurements converge upon a consistent result. Direct sample mass input Sample mass may be directly input from an analytical balance CorePyc*** Specialized unit with 2000 cm3 sample chamber size Integrated control and analysis module Can control up to five additional external analysis modules Unique run 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 Ethernet port An Ethernet port on the rear panel of the control module enables you to email reports, send data to a web browser for archiving, or interface with the AccuPyc Windows application USB ports USB ports on the rear panel of the control module allow for connection to a printer (output of analysis and calibration results in either ascii or excel formats) and keyboard (alphanumeric character input). The USB port is also used for installing software upgrades 10 Five standard sample chamber sizes 1 cm3, 10 cm3, 100 cm3, 350 cm3, and 2000 cm3*** Simple calibration process Bayonet cap fitting Allows you to easily determine the volume of the instrument sample cell and expansion chambers using a traceable standard volume. After calibration, the cell and expansion chamber volumes are stored automatically Provides superior repeatable seal compared to screw-type fitting 2000 cm3 350 cm3 100 cm3 10 cm3 1 cm3 11 Model Selection Hardware Versatility Sample Sample Sample AccuPyc AccuPyc AccuPycIIIIII AccuPyc II AccuPyc II AccuPyc II AccuyPyc II Sample Chamber 3 cm 1 11cm 1 cm3 Chamber cm3 3 Capacity 1 cm3 Capacity 10 cm3 33 10cm cm3 10 cm3 10 101cm cm3 33 33 100 cm 1 cm 100 cm 100 3 cm3 100 cm 100 cm 10 cm3 10 cm3 100 cm3 AccuPyc 100 cmII3 1340 AccuPyc II Bundle AccuPyc II Bundle AccuyPyc II Bundle Remote Analysis Remote RemoteAnalysis Analysis Remote Analysis Module Only Module ModuleOnly Only Module Only Remote Analysis Remote Analysis Module Only Module Only Remote Analysis Control Module Only Control Module Only Control Module Only Control Module Only Module Only Control Module Only Control Module Only Sample Chamber 1-cm 1.1-cm 1-cm IDID 1-cm IDxxx1.1-cm 1.1-cm D 1-cm ID x Chamber 1.1-cm D DD 1-cmDimensions ID x 1.1-cm D Dimensions 1.80-cm 3.93-cmDD 1.80-cm IDIDxx3.93-cm Available Available Available Temp Temp Temp Catalog Catalog Catalog Available Temp MultiVolume Control MultiVolume MultiVolume Control MultiVolumeTemp Control Control Catalog Number Number Catalog Number Number MultiVolume Control Insert Kits Type Insert Type InsertKits Kits Type Type Number Insert Kits Available Temp Insert Kits Type Available MultiVolume 3 0.1 cm 0.1 0.1 cm3MultiVolume N/A 0.1cm cm3 3 Insert 0.1 cm3Kits Insert Kits 3 1.0 and 3.5 cm3 3 1.80-cm ID3.93-cm x 3.93-cmDD 33.5cm 1.0 1.0and and3.5 cm3 N/A 1.80-cm ID xID 1.0 and 3.5 cm 1.80-cm 3.93-cm 1.0 and 1-cm ID xx1.1-cm D D 0.13.5 cm3cm 3 3 4.62-cm 6.17-cm 1-cm IDID xID D DD and 35 cm 4.62-cm xxx6.17-cm 0.1 4.62-cm ID1.1-cm 6.17-cm D 1010 35 10and and3cm 35cm cm333 4.62-cm ID x 6.17-cm D 4.62-cm ID x 6.17-cm D 10 and 35 cm N/A 10 and 35 cm 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 Remote Analysis Instruments 4.62-cm ID x 6.17-cm D 10 and 35 cm3 Catalog Temp Control Catalog 134/00001/00 Number 134/00001/00 134/00001/00 134/00001/00 Control Type 134/00001/00 Number Type N/A N/A N/A N/A N/A N/A AccuPyc IIIIII 1340 1340 Remote Remote Analysis Analysis Instruments Instruments AccuPyc AccuPyc 1340 Remote Analysis Instruments Bundle includes Control module and 2-ft cable connected to Analysis modules. Bundle includes Control module andand 2-ft 2-ft cable connected to Analysis modules.modules. Bundle includes Control module connected to Bundle includes Control module and 2-ftcable cable connected toAnalysis Analysis modules. Bundle includes Control module and 2-ft cable connected to Analysis modules. AccuPyc II 1340 Remote Analysis Instruments 1 cm 1-cm ID xRemote 1.1-cm D DD 0.1 cm N/A 1-cm 1.1-cm cm 0.1 cm AccuPyc Instruments 1-cm IDID 1 11cm 0.1 1-cm IDxxx1.1-cm 1.1-cm D Analysis cm II 1340 0.1cm cm 134/00000/00 134/00000/00 134/00000/00 134/00000/00 134/00000/00 134/00001/00 134/00002/00 134/00001/00 134/00002/00 134/00002/00 134/00002/00 134/00002/00 134/00000/00 134/00000/00 134/00002/00 134/00002/00 134/00031/00 134/00031/00 134/00031/00 134/00031/00 134/00031/00 134/00030/00 134/00030/00 134/00030/00 10 cm 1.80-cm ID xID3.93-cm 1.0 and 3.5 cm3.5 cm3 N/A 134/00030/00 134/00030/00 1.80-cm x 3.93-cmD D 10 cm33 1.0 and 3 3 33 33 4.62-cm 6.17-cm 134/00032/00 N/A 10 and 35 cm 100 cm 1-cm ID xxxx1.1-cm D DD 134/00031/00 0.135 cmcm 4.62-cm IDID 6.17-cm 134/00032/00 N/A 10 and 100 4.62-cm ID 6.17-cm D 134/00032/00 N/A 10 and 35 cm 1001cm cm 3 33 3 4.62-cm x 6.17-cm 1-cm ID ID x 1.1-cm D D 134/00032/00 N/A 10 and 35 cm 3 100 cm 3 134/00031/00 1 cm 0.1 3cm 100 cm3 350 4.62-cm ID x 6.17-cm D 10 and 35 cm N/A 134/00032/00 NA 134/00033/00 3 134/00030/00 1.80-cmIDID IDxxxx13.94-cm 3.93-cmDDD 5.84-cm 13.94-cm 10cm cm 1.0 andNA 3.5 cm 350 134/00033/00 NA 134/00033/00 5.84-cm 5.84-cm ID 13.94-cm D 350 cm3 NA cm3 134/00033/00 134/00030/00 1.80-cm 10 cm 1.0 and 3.5 5.84-cmID IDxx3.93-cm 13.94-cmDD 350 cm3 33 3 33 3 4.62-cm ID x 6.17-cm D 134/00034/00 9.7-cm ID xx26.00-cm 26.00-cm D 134/00032/00 N/A 10and 35 cm 100cm cm 2000 650 and 1300 cm 134/00034/00 9.7-cm cm 134/00034/00 9.7-cm ID 26.00-cmDD D N/A 650 2000 cm3 650 and1300 1300 cm3 350 cm32000 5.84-cm IDID xxx13.94-cm 134/00033/00 4.62-cm ID x26.00-cm 6.17-cm DD 134/00032/00 N/A 10 and cm3cm3 N/A 100 cm 134/00034/00 9.7-cm ID 2000 cm3 33 650 and35 1300 NA 134/00033/00 ID x 13.94-cm D 350 cm modules5.84-cm Remote analysis only. Remote analysis units require connection to control module Remote analysis modules only. Remote analysis units require to 3 Remote analysis modules only. Remote analysis units require connection toaa acontrol controlmodule module NAcmconnection 134/00033/00 5.84-cm ID x 13.94-cm D 3 3 350 cm 2000 cm 9.7-cm ID x 26.00-cm D 650 and 1300 N/A 134/00034/00 Remote analysis analysis units650 require connection to a control module 3 modules only. 134/00034/00 9.7-cm Remote ID x 26.00-cm D or AccuPyc 1340 2000IIII and 1300 cm3 or 1340 orAccuPyc AccuPyc IIcm 1340 3 134/00034/00 9.7-cm ID x 26.00-cm D 2000 cm 650 and 1300 cm3 or AccuPyc II 1340 Remote only. Remote analysis units require connection to a control or AccuPyc II 1340 3 modules 33 connection Remoteanalysis analysis modules only. Remote tomodule a control module 1-cm 1.1-cm cm 134/00041/00 0.1 cm 1-cm xxx1.1-cm 1 11cm 1-cmIDID ID 1.1-cmDD Danalysis units require cm333 modules 134/00041/00 0.1 134/00041/00 0.1cm cm3connection Remote analysis only. Remote analysis units require to a control module 3 1-cm ID x 1.1-cm D 1 cm 134/00041/00 0.1 cm 3 or AccuPyc II 1340 3 33 1.80-cm 3.93-cm cm 134/00040/00 1.0 and 3.5 cm 1.80-cm IDID DD 1010 1.80-cm IDxxx3.93-cm 3.93-cm D 10cm cm 134/00040/00 3 134/00040/00 1.0and and3.5 3.5cm cm333 N/A or1 cm AccuPyc 1340 3 1-cm 1.80-cm ID x 1.1-cm D 0.1 cm3 1.0 134/00041/00 ID x 3.93-cm D 10IIcm 134/00040/00 1.0 and 3.5 cm 33 3 3 134/00042/00 4.62-cm ID x 6.17-cm D 33 100 cm N/A 10 and 35 cm 134/00042/00 4.62-cm ID x 6.17-cm D 100 3 134/00042/00 4.62-cm ID x 6.17-cm D 1001cm cm33 N/A 10 and 35 cm N/A 10 and 1-cm ID x 1.1-cm D 134/00041/00 0.1 35 cmcm3 134/00042/00 4.62-cm ID x 6.17-cm D 100 cm3 N/A 10 and 35 3 3 cm 1-cm ID x 1.1-cm D 1 cm 134/00041/00 0.1 cm 3 10 cm3 350 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm N/A 134/00040/00 3 3 134/00043/00 NA 5.84-cm 13.94-cm 350 1.80-cmIDID 3.93-cmDDD 10cm cm 3 134/00043/00 NA 5.84-cm xxx13.94-cm 134/00040/00 1.0 and 3.5 cm 134/00043/00 NA 5.84-cm ID 13.94-cm D 350 134/00043/00 NA cm3 3 5.84-cmID IDxx3.93-cm 13.94-cmDD 1.80-cm 350 cm3333 10 cm 134/00040/00 1.0 and 3.5 3 3 9.7-cm 26.00-cm 2000 cm 134/00042/00 4.62-cm ID x 6.17-cm DDD 100cm 650 and 1300 cm 9.7-cm IDID xxx26.00-cm 134/00046/00 N/A 10 35 cm 9.7-cm ID 26.00-cm D 2000 cm 650 and cm 32000 31300 134/00046/00 650 and 1300 cm333 N/A 134/00046/00 33 100 cm 2000 4.62-cm ID x 6.17-cm D 10 and 35 cm 134/00042/00 3 9.7-cm ID x 26.00-cm D 134/00042/00 4.62-cm ID x 6.17-cm D cm 100 cm 650 and 1300 cm N/A 10 and 35 cm 134/00046/00 134/00043/00 NA 5.84-cm ID x 13.94-cm D 350 cm3 134/00043/00 NA 5.84-cm IDx x13.94-cm 13.94-cm DD N/A cm3 3 350 cm3 350 5.84-cm ID N/A 134/00043/00 3 ID x 26.00-cm D 2000 cm only. Up to9.7-cm 650 and 1300 cmto 134/00046/00 Control module analysis modules can be connected single control module. Control 55 modules can connected Controlmodule module only.Up Upto to 5analysis analysis modules canbe be connected toaa asingle singlecontrol controlmodule. module. 9.7-cm ID x 26.00-cm D cm3 only. 650 and 1300 cm3to 134/00046/00 Control 2000 module only. Up to 5 analysis modules can be connected to a single control module. 3 3 2000 cm N/A 9.7-cm ID x 26.00-cm D 650 and 1300N/A cm N/A 134/00046/00 134/00005/00 N/A N/A 134/00005/00 N/A N/A N/A N/A 134/00005/00 N/A N/A N/A N/A 134/00005/00 N/A N/A N/A N/A Control module only. Up to 5 analysis modules can be connected to a single control module. Control module module only. 5 analysis modules can be connected to a single Control only.Up Uptoto 5 analysis modules can be connected to acontrol singlemodule. control module. 134/00005/00 N/A N/A N/A N/A 134/00005/00 N/A N/A N/A N/A N/A N/A N/A N/A 134/00005/00 3 AccuPyc Bundle AccuPyc AccuPycIIIIIIBundle Bundle AccuPyc II Bundle Sample Sample Sample Sample Sample Chamber Chamber Sample Chamber Sample Chamber Chamber Chamber Chamber Chamber Chamber Chamber Capacity Dimensions Capacity Dimensions Capacity Dimensions Capacity Dimensions Sample Sample Capacity Dimensions 3 33 3 AccuPyc II TC and AccuPyc II TEC Title for this instrument? 12 A MultiVolume option allowing you to analyze smaller-sized samples with your current AccuPyc model is available for configurations listed below. Each kit includes appropriate insert(s), reference standard(s), and sample cup(s). 3 33 3 Bundle includes 2-ft modules. 1-cm ID and x 1.1-cm D cable connected 1 cm33 Control module 0.1to cmAnalysis 3 1.80-cm ID 3.93-cm cm 1.0 and 3.5 cm Bundle3 includes and 2-ft cable connected to3.5 Analysis modules. 1.80-cm DD 1010 1.0 1.80-cmID IDxxx3.93-cm 3.93-cm D 10cm cm3 3 Control module 1.0and and 3.5 cm3 3 3 cm AccuPyc IIIIII 1340 1340 Temperature Temperature---Controlled Controlled Instruments Instruments AccuPyc AccuPyc 1340 Temperature Controlled Instruments Control Module Only 1.80-cm 3.93-cm 134/00010/00 cm 1.0 and 3.5 cm 1.80-cm 1.80-cmIDID IDxxx3.93-cm 3.93-cmDD D 134/00010/00 1010 1.0 134/00010/00 10cm cm 1.0and and3.5 3.5cm cm Use with External Use Usewith withExternal External AccuPyc TC 1.80-cm ID x 3.93-cm D AccuPyc 134/00010/00 10IIcm 1.0 and 3.5 cm AccuPycIIIIIITC TC AccuPyc II 1340 Temperature Controlled Instruments AccuPyc 1340 Temperature-Controlled Instruments Use with External Recirculating Bath AccuPyc II TC Recirculating Bath Recirculating Bath AccuPyc II 1340 Temperature Controlled Instruments 134/00020/00 4.62-cmIDIDxx6.17-cm 6.17-cmDD 10 and 35 cm 100 cm 134/00020/00 4.62-cm AccuPyc TEC AccuPyc AccuPycIIIIIITEC TEC AccuPyc AccuPycII IITEC TC AccuPyc II TC AccuPyc II TEC AccuPyc II TEC MultiVolume Kits 3 33 3 3 33 3 3 3 1010and 134/00020/00 4.62-cm ID x 6.17-cm D 100 and35 35cm cm333 Recirculating Bath 100cm cm333 15-50 15-50 15-50˚C˚C ˚C 134/00020/00 4.62-cm ID x 6.17-cm D 3 cm 3 10 and 35 3 100 cm 1.80-cm ID x 3.93-cm D 134/00010/00 10 cm 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3.5 cm Use with15-50 134/00010/00 10 cm 1.0 and External ˚C Use with External 1.80-cm ID x 3.93-cm D 134/00010/00 10 cm3 1.0 and 3.5 cm3 Recirculating Bath Use with External Recirculating Bath 3 3 134/00020/00 4.62-cm ID6.17-cm x3.93-cm 6.17-cmD 10and 35cm cm 3 33 134/00050/00 1.80-cm 3 33 Integral Thermo15–50 ˚CRecirculating 1.0 and 3.5 cm 134/00050/00 1.80-cm xxx3.93-cm DD cm Bath 134/00020/00 Integral Thermo100 cm3 100 4.62-cm IDID xID 10 and 35 cm 134/00050/00 1.80-cm ID 3.93-cm D 1.0 Integral Thermo1010 cm 1.0 and33.5 3.5 cm 10cm cm 15-50 ˚C 3 3 134/00020/00 4.62-cm 10 10010 134/00050/00 1.80-cm ID ID xx 6.17-cm 3.93-cmDD Integral Thermo1.0and and35 3.5cm cm3 cm3 Electric Cooling, 15-50 ˚CCooling, Electric Electric Cooling, Electric Cooling, 3 3 134/00051/00 4.62-cm 6.17-cm and 35 cm 4.62-cm ˚C* 15-36 ˚C, 100 cm 134/00051/00 4.62-cmIDID IDxxx6.17-cm 6.17-cmDD D 1010 15-36 100 10and and35 35cm cm3333 ±0.10.1 0.1˚C* ˚C* 134/00051/00 15-36˚C, ˚C,±± 100cm cm3333 4.62-cm 134/00050/00 1.80-cm ID x 6.17-cm 3.93-cmDD Integral 10 ± 0.1 ˚C* 134/00051/00 15-36 ˚C,Thermo1.0and and35 3.5cm cm 100 10cm cm 3 3 134/00050/00 1.80-cm ID x 3.93-cm D Integral 1.0 and 3.5 cm 10 cm ElectricThermoCooling, 134/00050/00 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 10 cm3 IntegralElectric ThermoCooling, 3 3 4.62-cm ID x 6.17-cm D 10 and 35 cm 15-36 ˚C, ± 0.1 ˚C* 134/00051/00 100 cm Electric Cooling, 4.62-cm ID x 6.17-cm D 10 and 35 cm3 15-36 ˚C, ± 0.1 ˚C* 134/00051/00 100 cm3 3 3 15-36 ˚C, ±0.1 ˚C* 100 cm 4.62-cm ID x 6.17-cm D 10 and 35 cm 134/00051/00 3 3 1.80-cm 3.93-cm 1.0 and 3.5 cm 1.80-cm 134/00044/00 cm 1.80-cmIDID IDxxx3.93-cm 3.93-cmDD D 1.0 134/00044/00 1010 1.0and and3.5 3.5cm cm333 Use with External 134/00044/00 10cm cm333 Use with External Use with External 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm 134/00044/00 10 cm Use with External Recirculating Bath Recirculating Bath 3 Recirculating Bath 134/00045/00 3 134/00045/00 4.62-cm 6.17-cm and 35 cm 4.62-cm 100 cm 134/00045/00 4.62-cmIDID IDxxx6.17-cm 6.17-cmDD D 1010 100 10and and35 35cm cm333 100cm cm333 Recirculating Bath 15-50 15-50 134/00045/00 4.62-cm ID xx 6.17-cm DD 15-50˚C˚C ˚C 10 and 35 cm 3 100 cm 3 1.80-cm ID 3.93-cm 1.0 and 3.5 cm 134/00044/00 10 cm 15-50 ˚C Use with External 3 3 1.80-cm 3.93-cm DD 134/00044/00 10 cm3 10 grade 1.80-cm IDIDxx3.93-cm 1.0 and1.0 3.5 cm and 3.5 cm 134/00044/00 cm3 Use with External Use with External Research helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or Research helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, Recirculating Bath Researchgrade grade helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air,or or 3 134/00045/00 4.62-cm ID xis 6.17-cm D Recirculating Bath 10 and 35 cm 100 cm3 used. Research grade helium or nitrogen strongly recommended. High purity Carbon dioxide, dry air, or Recirculating Bath argon may be A multigas option for up to four gases on one analysis unit is available. 3 15-50 ˚C 3 used. argon may be AAmultigas option for up to four gases on one analysis unit is available. 134/00045/00 4.62-cm ID x 6.17-cm D argon may be used. multigas option for up to four gases one analysis unit is available. 10 and 35 cm 3100 cm 3 on 15–50 ˚C15-50 100 cmmay be used. A4.62-cm ID option x 6.17-cm andgases 35 cm on one analysis 134/00045/00 argon multigas forDup to10 four unit˚Cis available. *Subject environmental operating conditions *Subject toto operating conditions *Subject toenvironmental environmental operating conditions Research grade helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or *Subject to environmental operating conditions Research grade helium oror nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or dry air, or Research grade helium nitrogen is strongly recommended. High purity Carbon dioxide, argon may be used. A multigas option for up to four gases on one analysis unit is available. argon may may be option for up four on oneon analysis unit is available. argon be used. used.AAmultigas multigas option fortoup to gases four gases one analysis unit is available. *Subject to environmental operating conditions *Subject to to environmental operating conditions *Subject environmental operating conditions 2000-cm3 nominal cell volume 650- and 1300-cm3 cups 100-cm3 nominal cell volume 10- and 35-cm3 cups 10-cm3 nominal cell volume 1- and 3.5-cm3 cups 1-cm3 nominal cell volume 0.1-cm3 cup 3 13 Software Versatility AccuPyc II Specifications Data Presentation Precision Density vs Cycle # Average: 3.8691 g/cm³ Density vs Cycle # Accuracy 3.890 Accurate to within 0.03% of reading, plus 0.03% of sample capacity. 3.885 Physical 3.880 17.9 cm (7.0 in.), analysis modules for 1-, 10-, and 100-cm3 units, and control module Height 25.9 cm (10.2 in.), 350-cm3 analysis module 43.0 cm (17.0 in.), 2000-cm3 analysis module 3.875 3.870 27.3 cm (10.7 in.), control module Width 27.3 cm (10.7 in.), control module 27.0 cm (10.6 in.), 2000-cm3 analysis module 3.865 1.0 1.5 2.0 2.5 3.0 3.5 • Total Pore Volume vs. Temperature 4.5 5.0 5.5 7.0 7.5 8.0 8.5 9.0Report 9.5 10.0 Equilibration 6.0 6.5 Cycle Number P2 (Expansion Pressure) shown every 1 second(s) Cycle #2 Cycle #3 Cycle #4 Cycle #5 Cycle #8 Cycle #6 18 Depth 436.2 cm (14.3 in.) 17 P2 (Expansion Pressure) (psig) • Density vs. Time 4.0 Cycle #1 Cycle #7 • Summary Report • Volume vs. Cycle # 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) Weight 10.5 kg (23.2 lbs), analysis module (350-cm3 unit) 3.6 kg (8.0 lbs), control module 26.0 kg (57.0 lbs), 2000-cm3 analysis module 3.860 • Combined Report • User-Defined Tabular Reports Reproducibility typically to within ± 0.01% of the nominal 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. Standard Deviation: 0.0123 g/cm³ 3.895 Density (g/cm³) The AccuPyc II can be operated with a keypad or an optional Windows® interface that provides exceptional reporting and archiving capability. Both versions include direct sample mass input from a balance and cycle-based displacement volume reporting. With the Windows interface, features such as time-based pressure equilibration reporting and additional calculations such as percent solids content and total pore volume are included. Operational status can also be continually monitored in a status window on the monitor screen. Electrical Power 16 Electrical Power -30 VA 15 Voltage -90 to 264 VAC Frequency -50 to 60 Hz 14 *Due to continuous improvements, specifications are subject to change without notice. 13 • Density vs. Cycle # • Options Report • Equilibration Report 12 11 0 2 4 6 8 10 12 14 Time (seconds) 16 18 20 22 24 26 • Sample Log Vol. vs Cycle # Vol. vs Cycle # Reference Sigma+/Min/Max 6.378 Average: 6.3725 cm³ Standard Deviation: 0.0004 cm³ 6.376 Volume (cm³) 6.374 6.372 6.370 6.368 6.366 14 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 Cycle Number 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 15 Micromeritics Instrument Corporation 4356 Communications Drive, Norcross, GA 30093 USA To request a quote or additional product information, visit micromeritics.com Contact your local Micromeritics sales representative or our Customer Service Department at 770-662-3636 © All Rights Reserved 2016. Micromeritics Instrument Corporation. Norcross, Ga 30093. 770-662-3636. Printed in the USA. 000/00000/00
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