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QbD Solid Fraction Analysis in Roller Compaction Operations AccuPyc 1340 Gas Pycnometer GeoPyc 1365 Envelope and T.A.P. Density

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Page 1: QbD Solid Fraction Analysis in Roller Compaction … 3 THE IMPORTANCE OF SOLID FRACTION DATA Solid Fraction IN ROLLER COMPACTION OPERATIONS Roller compaction is a continuous dry granulation

QbD Solid Fraction Analysis in Roller Compaction OperationsAccuPyc 1340 Gas Pycnometer GeoPyc 1365 Envelope and T.A.P. Density

Page 2: QbD Solid Fraction Analysis in Roller Compaction … 3 THE IMPORTANCE OF SOLID FRACTION DATA Solid Fraction IN ROLLER COMPACTION OPERATIONS Roller compaction is a continuous dry granulation

2 3

Solid FractionTHE 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.

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, 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= 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.

SF=Pe

Po

Page 3: QbD Solid Fraction Analysis in Roller Compaction … 3 THE IMPORTANCE OF SOLID FRACTION DATA Solid Fraction IN ROLLER COMPACTION OPERATIONS Roller compaction is a continuous dry granulation

4 5

GEOPYC 1365Envelope Density Analyzer

Highly accurate and reproducible results

Fast operation in a small bench-top instrument

Fully automated data acquisition and reporting

Nondestructive analysis maintains sample integrity

Intelligent touch panel for ease of operation and reporting

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.

T.A.P. Density Option

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.

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

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.

Technique

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.

Precision bore glass cylinder

Plunger

Dry solid medium Baseline: Solid Medium Only in Cell

A

A B

Measurement: Solid Medium and Object in Cell

h

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. Sample-

specific information can be entered into the analysis reports.

Available Reports: Envelope Density, Volume Calibration, Blank Report, Force Calibration, Instrument Log

Page 4: QbD Solid Fraction Analysis in Roller Compaction … 3 THE IMPORTANCE OF SOLID FRACTION DATA Solid Fraction IN ROLLER COMPACTION OPERATIONS Roller compaction is a continuous dry granulation

6 7

GeoPyc 1365 Specifications

ReproducibilityWhen sample volume is at least 25% of sample holder volume: Typically ± 1.1%

Sample Chamber12.7-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

PhysicalHeight 11 in. (27.9 cm)

Width 22 in. (55.9 cm)

Depth 15 in. (38.1 cm)

Weight 42 lbs (19 kg)

Electrical PowerElectrical Power 95 VA

Voltage 85 to 265 VAC

Frequency 47 to 63 Hz

EnvironmentTemperature 15 °C to 35 °C

Humidity 20% to 80% non-condensing

*Due to continuous improvements, specifications are subject to change without notice.

ACCUPYC IIGas Displacement Pycnometry System

Benefits

8g

Maximize your results with superior speed of analysis, accuracy, repeatability, and reproducibility

Adapt instrument configuration to meet your sample size needs

Operate with either a keypad or Windows® software

Use a variety of gases

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

Increase efficiency and compliance with barcoding compatibility

Eliminate procedural steps with direct input from an analytical balance

Minimize cost and space requirements; low maintenance and small footprint

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.

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.

Page 5: QbD Solid Fraction Analysis in Roller Compaction … 3 THE IMPORTANCE OF SOLID FRACTION DATA Solid Fraction IN ROLLER COMPACTION OPERATIONS Roller compaction is a continuous dry granulation

8 9

Density Type Definition Material

VolumeOpen-Pore Volume

Closed-Pore Volume

Inter Particle Volume

External Void Volume Addressed by

True (Absolute)

The mass of a substance divided by its volume, excluding open and closed (or blind) pores

AccuPyc II

Skeletal (Apparent)

The ratio of the mass of the solid material to the sum of the volume including closed (or blind) pores

AccuPyc II

EnvelopeThe ratio of the mass of a substance to the envelope volume (imaginary boundary surrounding the particle)

GeoPyc

BulkMass 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

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 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.

Particle VolumeInterparticle void

Assemblage of porous particles in a container

A single particle containing open and closed pores

The envelope

Surface void included within the envelope

Gas Displacement Pycnometry

Principle of Operation

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.

1

2 34 5

6a b c

sample

Density

1. Inert gas flows Into sample chamber. Valve a opens then closes.

2. Equilibrium is reached.

3. Gas flows into second chamber for volume measurement. Valve b opens.

4. Equilibrium is reached again.

5. Volume divided into sample weight determines density.

6. Pressure vented off to atmosphere. Valve c opens.

Page 6: QbD Solid Fraction Analysis in Roller Compaction … 3 THE IMPORTANCE OF SOLID FRACTION DATA Solid Fraction IN ROLLER COMPACTION OPERATIONS Roller compaction is a continuous dry granulation

10 11

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.

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

Simple calibration process

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.

Unique run precision

Can control up to five additional external analysis modules

Integrated control and analysis module

1 cm3, 10 cm3, 100 cm3, 350 cm3, and 2000 cm3***

Five standard sample chamber sizes

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

USB ports

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

Ethernet port

Specialized unit with 2000 cm3 sample chamber size

CorePyc***Sample mass may be directly input from an analytical balance

Direct sample mass input

Provides superior repeatable seal compared to screw-type fitting

Bayonet cap fitting

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

Multilingual

1 cm310 cm3100 cm3350 cm32000 cm3

Page 7: QbD Solid Fraction Analysis in Roller Compaction … 3 THE IMPORTANCE OF SOLID FRACTION DATA Solid Fraction IN ROLLER COMPACTION OPERATIONS Roller compaction is a continuous dry granulation

12 13

Model Selection

AccuPyc II Bundle

AccuPyc II

Remote Analysis Module Only

Control Module Only

Sample ChamberCapacity

Sample Chamber

Dimensions

AvailableMultiVolume

Insert Kits

Temp Control

Type

CatalogNumber

AccuPyc II TEC

AccuPyc II TC

Research grade helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or argon may be used. A multigas option for up to four gases on one analysis unit is available.

Bundle includes Control module and 2-ft cable connected to Analysis modules.

Remote analysis modules only. Remote analysis units require connection to a control module or AccuPyc II 1340

AccuPyc II 1340 Remote Analysis Instruments

AccuPyc II 1340 Temperature - Controlled Instruments

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

100 cm3

1 cm3

10 cm3

4.62-cm ID x 6.17-cm D

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

10 and 35 cm3

0.1 cm3

1.0 and 3.5 cm3

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

Use with External Recirculating Bath15-50 ˚C

Integral Thermo-Electric Cooling,15-36 ˚C, ± 0.1 ˚C*

Use with External Recirculating Bath15-50 ˚C

10 cm3

100 cm3

10 cm3

100 cm3

10 cm3

100 cm3

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.0 and 3.5 cm3

*Subject to environmental operating conditions

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

134/00000/00

134/00001/00

134/00002/00

134/00032/00

134/00033/00

134/00034/00

134/00041/00

134/00040/00

134/00042/00

134/00046/00

134/00031/00

134/00030/00

134/00043/00

134/00005/00

134/00010/00

134/00020/00

134/00050/00

134/00051/00

134/00044/00

134/00045/00

N/AN/A N/A N/A

Control module only. Up to 5 analysis modules can be connected to a single control module.

N/A

N/A

N/A

Hardware Versatility

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).

1-cm3 nominal cell volume 0.1-cm3 cup

MultiVolume Kits

10-cm3 nominal cell volume 1- and 3.5-cm3 cups

100-cm3 nominal cell volume 10- and 35-cm3 cups

2000-cm3 nominal cell volume 650- and 1300-cm3 cups

Sample Chamber Capacity

Sample Chamber Dimensions

MultiVolume Insert Kits

Temp Control Type

Catalog Number

1 cm3 1-cm ID x 1.1-cm D 0.1 cm3 N/A 134/00001/00

10 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 N/A 134/00000/00

100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 N/A 134/00002/00

AccuPyc II 1340 Remote Analysis Instruments

Bundle includes Control module and 2-ft cable connected to Analysis modules.

1 cm3 1-cm ID x 1.1-cm D 0.1 cm3 N/A 134/00031/00

10 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 N/A 134/00030/00

100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 N/A 134/00032/00

350 cm3 5.84-cm ID x 13.94-cm D N/A N/A 134/00033/00

2000 cm3 9.7-cm ID x 26.00-cm D 650 and 1300 cm3 N/A 134/00034/00

Remote analysis modules only. Remote analysis units require connection to a control module or AccuPyc II 1340

1 cm3 1-cm ID x 1.1-cm D 0.1 cm3 N/A 134/00041/00

10 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 N/A 134/00040/00

100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 N/A 134/00042/00

350 cm3 5.84-cm ID x 13.94-cm D N/A N/A 134/00043/00

2000 cm3 9.7-cm ID x 26.00-cm D 650 and 1300 cm3 N/A 134/00046/00

Control module only. Up to 5 analysis modules can be connected to a single control module.

N/A N/A N/A N/A 134/00005/00

AccuPyc II 1340 Temperature-Controlled Instruments

10 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 Use with External Recirculating Bath 15–50 ˚C

134/00010/00

100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 134/00020/00

10 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 Integral Thermo-Electric Cooling, 15-36 ˚C, ±0.1 ˚C*

134/00050/00

100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 134/00051/00

10 cm3 1.80-cm ID x 3.93-cm D 1.0 and 3.5 cm3 Use with External Recirculating Bath 15–50 ˚C

134/00044/00

100 cm3 4.62-cm ID x 6.17-cm D 10 and 35 cm3 134/00045/00

Research grade helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or argon may be used. A multigas option for up to four gases on one analysis unit is available.

AccuPyc II Bundle

AccuPyc II

Remote Analysis Module Only

Control Module Only

Sample ChamberCapacity

Sample Chamber

Dimensions

AvailableMultiVolume

Insert Kits

Temp Control

Type

CatalogNumber

AccuPyc II TEC

AccuPyc II TC

Research grade helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or argon may be used. A multigas option for up to four gases on one analysis unit is available.

Bundle includes Control module and 2-ft cable connected to Analysis modules.

Remote analysis modules only. Remote analysis units require connection to a control module or AccuPyc II 1340

AccuPyc II 1340 Remote Analysis Instruments

AccuPyc II 1340 Temperature - Controlled Instruments

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

100 cm3

1 cm3

10 cm3

4.62-cm ID x 6.17-cm D

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

10 and 35 cm3

0.1 cm3

1.0 and 3.5 cm3

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

Use with External Recirculating Bath15-50 ˚C

Integral Thermo-Electric Cooling,15-36 ˚C, ± 0.1 ˚C*

Use with External Recirculating Bath15-50 ˚C

10 cm3

100 cm3

10 cm3

100 cm3

10 cm3

100 cm3

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.0 and 3.5 cm3

*Subject to environmental operating conditions

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

134/00000/00

134/00001/00

134/00002/00

134/00032/00

134/00033/00

134/00034/00

134/00041/00

134/00040/00

134/00042/00

134/00046/00

134/00031/00

134/00030/00

134/00043/00

134/00005/00

134/00010/00

134/00020/00

134/00050/00

134/00051/00

134/00044/00

134/00045/00

N/AN/A N/A N/A

Control module only. Up to 5 analysis modules can be connected to a single control module.

N/A

N/A

N/A

AccuPyc II Bundle

AccuPyc II

Remote Analysis Module Only

Control Module Only

Sample ChamberCapacity

Sample Chamber

Dimensions

AvailableMultiVolume

Insert Kits

Temp Control

Type

CatalogNumber

AccuPyc II TEC

AccuPyc II TC

Research grade helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or argon may be used. A multigas option for up to four gases on one analysis unit is available.

Bundle includes Control module and 2-ft cable connected to Analysis modules.

Remote analysis modules only. Remote analysis units require connection to a control module or AccuPyc II 1340

AccuPyc II 1340 Remote Analysis Instruments

AccuPyc II 1340 Temperature - Controlled Instruments

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

100 cm3

1 cm3

10 cm3

4.62-cm ID x 6.17-cm D

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

10 and 35 cm3

0.1 cm3

1.0 and 3.5 cm3

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

Use with External Recirculating Bath15-50 ˚C

Integral Thermo-Electric Cooling,15-36 ˚C, ± 0.1 ˚C*

Use with External Recirculating Bath15-50 ˚C

10 cm3

100 cm3

10 cm3

100 cm3

10 cm3

100 cm3

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.0 and 3.5 cm3

*Subject to environmental operating conditions

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

134/00000/00

134/00001/00

134/00002/00

134/00032/00

134/00033/00

134/00034/00

134/00041/00

134/00040/00

134/00042/00

134/00046/00

134/00031/00

134/00030/00

134/00043/00

134/00005/00

134/00010/00

134/00020/00

134/00050/00

134/00051/00

134/00044/00

134/00045/00

N/AN/A N/A N/A

Control module only. Up to 5 analysis modules can be connected to a single control module.

N/A

N/A

N/A

AccuPyc II Bundle

AccuPyc II

Remote Analysis Module Only

Control Module Only

Sample ChamberCapacity

Sample Chamber

Dimensions

AvailableMultiVolume

Insert Kits

Temp Control

Type

CatalogNumber

AccuPyc II TEC

AccuPyc II TC

Research grade helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or argon may be used. A multigas option for up to four gases on one analysis unit is available.

Bundle includes Control module and 2-ft cable connected to Analysis modules.

Remote analysis modules only. Remote analysis units require connection to a control module or AccuPyc II 1340

AccuPyc II 1340 Remote Analysis Instruments

AccuPyc II 1340 Temperature - Controlled Instruments

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

100 cm3

1 cm3

10 cm3

4.62-cm ID x 6.17-cm D

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

10 and 35 cm3

0.1 cm3

1.0 and 3.5 cm3

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

Use with External Recirculating Bath15-50 ˚C

Integral Thermo-Electric Cooling,15-36 ˚C, ± 0.1 ˚C*

Use with External Recirculating Bath15-50 ˚C

10 cm3

100 cm3

10 cm3

100 cm3

10 cm3

100 cm3

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.0 and 3.5 cm3

*Subject to environmental operating conditions

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

134/00000/00

134/00001/00

134/00002/00

134/00032/00

134/00033/00

134/00034/00

134/00041/00

134/00040/00

134/00042/00

134/00046/00

134/00031/00

134/00030/00

134/00043/00

134/00005/00

134/00010/00

134/00020/00

134/00050/00

134/00051/00

134/00044/00

134/00045/00

N/AN/A N/A N/A

Control module only. Up to 5 analysis modules can be connected to a single control module.

N/A

N/A

N/A

AccuPyc II Bundle

AccuPyc II

Remote Analysis Module Only

Control Module Only

Sample ChamberCapacity

Sample Chamber

Dimensions

AvailableMultiVolume

Insert Kits

Temp Control

Type

CatalogNumber

AccuPyc II TEC

AccuPyc II TC

Research grade helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or argon may be used. A multigas option for up to four gases on one analysis unit is available.

Bundle includes Control module and 2-ft cable connected to Analysis modules.

Remote analysis modules only. Remote analysis units require connection to a control module or AccuPyc II 1340

AccuPyc II 1340 Remote Analysis Instruments

AccuPyc II 1340 Temperature - Controlled Instruments

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

100 cm3

1 cm3

10 cm3

4.62-cm ID x 6.17-cm D

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

10 and 35 cm3

0.1 cm3

1.0 and 3.5 cm3

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

Use with External Recirculating Bath15-50 ˚C

Integral Thermo-Electric Cooling,15-36 ˚C, ± 0.1 ˚C*

Use with External Recirculating Bath15-50 ˚C

10 cm3

100 cm3

10 cm3

100 cm3

10 cm3

100 cm3

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.0 and 3.5 cm3

*Subject to environmental operating conditions

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

134/00000/00

134/00001/00

134/00002/00

134/00032/00

134/00033/00

134/00034/00

134/00041/00

134/00040/00

134/00042/00

134/00046/00

134/00031/00

134/00030/00

134/00043/00

134/00005/00

134/00010/00

134/00020/00

134/00050/00

134/00051/00

134/00044/00

134/00045/00

N/AN/A N/A N/A

Control module only. Up to 5 analysis modules can be connected to a single control module.

N/A

N/A

N/A

AccuPyc II Bundle

AccuPyc II

Remote Analysis Module Only

Control Module Only

Sample ChamberCapacity

Sample Chamber

Dimensions

AvailableMultiVolume

Insert Kits

Temp Control

Type

CatalogNumber

AccuPyc II TEC

AccuPyc II TC

Research grade helium or nitrogen is strongly recommended. High purity Carbon dioxide, dry air, or argon may be used. A multigas option for up to four gases on one analysis unit is available.

Bundle includes Control module and 2-ft cable connected to Analysis modules.

Remote analysis modules only. Remote analysis units require connection to a control module or AccuPyc II 1340

AccuPyc II 1340 Remote Analysis Instruments

AccuPyc II 1340 Temperature - Controlled Instruments

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

100 cm3

1 cm3

10 cm3

4.62-cm ID x 6.17-cm D

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

10 and 35 cm3

0.1 cm3

1.0 and 3.5 cm3

1 cm3

10 cm3

100 cm3

350 cm3

2000 cm3

0.1 cm3

1.0 and 3.5 cm3

10 and 35 cm3

NA

650 and 1300 cm3

1-cm ID x 1.1-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

5.84-cm ID x 13.94-cm D

9.7-cm ID x 26.00-cm D

Use with External Recirculating Bath15-50 ˚C

Integral Thermo-Electric Cooling,15-36 ˚C, ± 0.1 ˚C*

Use with External Recirculating Bath15-50 ˚C

10 cm3

100 cm3

10 cm3

100 cm3

10 cm3

100 cm3

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.80-cm ID x 3.93-cm D

4.62-cm ID x 6.17-cm D

1.0 and 3.5 cm3

*Subject to environmental operating conditions

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

1.0 and 3.5 cm3

10 and 35 cm3

134/00000/00

134/00001/00

134/00002/00

134/00032/00

134/00033/00

134/00034/00

134/00041/00

134/00040/00

134/00042/00

134/00046/00

134/00031/00

134/00030/00

134/00043/00

134/00005/00

134/00010/00

134/00020/00

134/00050/00

134/00051/00

134/00044/00

134/00045/00

N/AN/A N/A N/A

Control module only. Up to 5 analysis modules can be connected to a single control module.

N/A

N/A

N/A

AccuyPyc II

AccuyPyc II Bundle

Remote Analysis Module Only

Control Module Only

AccuPyc II TC andAccuPyc II TEC

Title for this instrument?

*Subject to environmental operating conditions

Page 8: QbD Solid Fraction Analysis in Roller Compaction … 3 THE IMPORTANCE OF SOLID FRACTION DATA Solid Fraction IN ROLLER COMPACTION OPERATIONS Roller compaction is a continuous dry granulation

14 15

Software Versatility

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.

• Combined Report

• Summary Report

• User-Defined Tabular Reports

• Volume vs. Cycle #

• Density vs. Time

• Total Pore Volume vs. Temperature

• Density vs. Cycle #

• Options Report

• Equilibration Report

• Sample Log

Data Presentation

Cycle Number1.01.0 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

Den

sity

(g/c

m³)

3.8603.860

3.865

3.870

3.875

3.880

3.885

3.890

3.895

Density vs Cycle #Average: 3.8691 g/cm³ Standard Deviation: 0.0123 g/cm³

Density vs Cycle #

Time (seconds)00 2 4 6 8 10 12 14 16 18 20 22 24 26

P2

(Exp

ansi

on P

ress

ure)

(psi

g)

1111

12

13

14

15

16

17

18

Equilibration ReportP2 (Expansion Pressure) shown every 1 second(s)

Cycle #1 Cycle #2 Cycle #3 Cycle #4 Cycle #5 Cycle #6Cycle #7 Cycle #8

Cycle Number1.01.0 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

Vol

ume

(cm

³)

6.3666.366

6.368

6.370

6.372

6.374

6.376

6.378

Vol. vs Cycle #Average: 6.3725 cm³ Standard Deviation: 0.0004 cm³

Vol. vs Cycle #ReferenceSigma+/-Min/Max

AccuPyc II Specifications

PrecisionReproducibility 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.

AccuracyAccurate to within 0.03% of reading, plus 0.03% of sample capacity.

Physical

Height17.9 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

Width27.3 cm (10.7 in.), control module 27.3 cm (10.7 in.), control module 27.0 cm (10.6 in.), 2000-cm3 analysis module

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) 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

Depth 436.2 cm (14.3 in.)

Electrical PowerElectrical Power -30 VA

Voltage -90 to 264 VAC

Frequency -50 to 60 Hz

*Due to continuous improvements, specifications are subject to change without notice.

Page 9: QbD Solid Fraction Analysis in Roller Compaction … 3 THE IMPORTANCE OF SOLID FRACTION DATA Solid Fraction IN ROLLER COMPACTION OPERATIONS Roller compaction is a continuous dry granulation

000/00000/00© All Rights Reserved 2016. Micromeritics Instrument Corporation. Norcross, Ga 30093. 770-662-3636. Printed in the USA.

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To request a quote or additional product information, visit

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770-662-3636