QbD Solid Fraction Analysis in Roller Compaction Operations

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
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Module Only
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AccuPyc IIIIII 1340
1340 Remote
Remote Analysis
Analysis Instruments
Instruments
AccuPyc
AccuPyc
1340
Remote
Analysis
Instruments
Bundle
includes
Control
module
and
2-ft
cable
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Analysis
modules.
Bundle includes
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module
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cable
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Bundle
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Bundle
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Bundle includes Control module and 2-ft cable connected to Analysis modules.
AccuPyc
II
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Remote
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N/A
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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.
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