Micromeritics ACCUPYC II 1345 Series User manual

OPERATOR MANUAL
134-42851-01
Not Released
(Rev -)
ACCUPYC®II 1345
GAS DISPLACEMENT PYCNOMETER
Pre-review Copy

TRADEMARKS
AccuPyc is a registered trademark of Micromeritics Instrument Corporation.
Micromeritics is a registered trademark of Micromeritics Instrument Corporation.
Microsoft and Windows are registered trademarks of Microsoft Corporation.
Windows is a registered trademark of Microsoft Corporation.
Copyright
The software described in this manual is furnished under a license agreement and may be used or
copied only in accordance with the terms of the agreement.
______________________________________________________________________________
Copyright © 2019. Micromeritics Instrument Corporation. All rights reserved.
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WARRANTY
MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment each instrument it
manufactures to be free from defects in material and workmanship impairing its usefulness under normal use and service
conditions except as noted herein.
Our liability under this warranty is limited to repair, servicing and adjustment, free of charge at our plant, of any instrument or
defective parts when returned prepaid to us and which our examination discloses to have been defective. The purchaser is
responsible for all transportation charges involving the shipment of materials for warranty repairs. Failure of any instrument
or product due to operator error, improper installation, unauthorized repair or alteration, failure of utilities, or environmental
contamination will not constitute a warranty claim. The materials of construction used in MICROMERITICS instruments and
other products were chosen after extensive testing and experience for their reliability and durability. However, these
materials cannot be totally guaranteed against wear and/or decomposition by chemical action (corrosion) as a result of
normal use.
Repair parts are warranted to be free from defects in material and workmanship for 90 days from the date of shipment.
No instrument or product shall be returned to MICROMERITICS prior to notification of alleged defect and authorization to
return the instrument or product. All repairs or replacements are made subject to factory inspection of returned parts.
MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications are made by
persons other than its own authorized service personnel unless such work is authorized in writing by MICROMERITICS.
The obligations of this warranty will be limited under the following conditions:
1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold under their respective
brand names or trade names. We, therefore, make no express or implied warranty as to such products. We shall use
our best efforts to obtain from the manufacturer, in accordance with his customary practice, the repair or replacement
of such of his products that may prove defective in workmanship or materials. Service charges made by such man-
ufacturer are the responsibility of the ultimate purchaser. This states our entire liability in respect to such products,
except as an authorized person of MICROMERITICS may otherwise agree to in writing.
2. If an instrument or product is found defective during the warranty period, replacement parts may, at the discretion of
MICROMERITICS, be sent to be installed by the purchaser, e.g., printed circuit boards, check valves, seals, etc.
3. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs (rotor) and stems,
seals and O-rings, ferrules, etc., are excluded from this warranty except for manufacturing defects. Such items which
perform satisfactorily during the first 45 days after the date of shipment are assumed to be free of manufacturing
defects.
Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought against
MICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard product or manufactures a
special product to the purchaser’s specifications.
MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its products
other than the liability stated above. This warranty is in lieu of all other warranties, express or implied, including but not
limited to, the implied warranties of merchantability or fitness for use.
Warranty
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Corporate Profile
CORPORATE PROFILE
Micromeritics Instrument Corporation is a leading global provider of solutions for material characterization with best-
in-class instrumentation and application expertise in five core areas: density; surface area and porosity; particle size
and shape; powder characterization; and catalyst characterization and process development. Founded in 1962, the
company is headquartered in Norcross, Georgia, USA and has more than 400 employees worldwide. With a fully
integrated operation that extends from a world class scientific knowledge base through to in-house manufacture,
Micromeritics delivers an extensive range of high-performance products for academic research and industrial
problem-solving. The implementation of tactical partnerships to incubate and deliver valuable new technologies
exemplifies the company’s holistic, customer-centric approach which extends to a cost-efficient contract testing
laboratory – the Particle Testing Authority (PTA). The strategic acquisitions of Freeman Technology Ltd and Process
Integral Development S.L. (PID Eng & Tech) reflect an ongoing commitment to optimized, integrated solutions in the
industrially vital areas of powders and catalysis.
Freeman Technology (Tewkesbury, UK) brings market-leading powder characterization technology to
Micromeritics’ existing portfolio of particle characterization techniques. The result is a suite of products that directly
supports efforts to understand and engineer particle properties to meet powder performance targets. With over 15
years of experience in powder testing, Freeman Technology specializes in systems for measuring the flow
properties of powders. In combination with detailed application know-how these systems deliver unrivalled insight
into powder behavior supporting development, formulation, scale-up, processing and manufacture across a wide
range of industrial sectors.
PID Eng & Tech (Madrid, Spain) complements Micromeritics’ renowned offering for catalyst characterization with
technology for the measurement and optimization of catalytic activity, with a product range that extends to both
standard and bespoke pilot scale equipment. Launched in 2003, PID Eng & Tech is a leading provider of
automated, modular microreactor systems for the detailed investigation of reaction kinetics and yield. These
products are supported by a highly skilled multidisciplinary team of engineers with in-depth expertise in the design,
construction and operation of laboratory units and process scale-up.
The Particle Testing Authority (PTA) provides material characterization services for fine powders and solid materials
using Micromeritics’ instrumentation alongside complementary solutions from other vendors. With the certification
and expertise to operate across a wide range of industries the PTA offering runs from single sample analysis to
complex method development, method validation, new product assessment, and the analytical support required for
large scale manufacturing projects. An experienced, highly trained team of scientists, engineers, and lab
technicians works closely with every client to ensure that all analytical requirements are rapidly and responsively
addressed.
Micromeritics has a strong global network with offices across the Americas, Asia, and Europe complemented by a
dedicated team of distributors in additional locations. This ensures that local, knowledgeable support is available
for every customer, in academia or industry. Micromeritics works across a truly diverse range of industries from oil
processing, petrochemicals and catalysts, to food and pharmaceuticals, and at the forefront of characterization
technology for next generation materials such as graphene, metal-organic-frameworks, nanocatalysts, and zeolites.
Engineering solutions that work optimally for every user is a defining characteristic of the company.
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CONTACT US
Micromeritics Instrument Corporation
4356 Communications Drive
Norcross, GA / USA / 30093-2901
Phone: [phone]
Fax: [phone]
www.Micromeritics.com
Instrument Service or Repair
Phone: [phone]
International — contact your local distributor or call 1-770-662-3666
[e-mail]
Micromeritics Learning Center
Phone: [phone]
www.Micro.edu
Contact Us
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About this Manual
ABOUT THIS MANUAL
Log in to your customer portal to access the following:
lCalculations
lError Messages
Parts and accessories can be found online at www.Micromeritics.com.
The following symbols indicate safety precautions and supplemental information and may appear in
this manual:
NOTE— Notes contain important information applicable to the topic.
CAUTION — Cautions contain information to help prevent actions that may damage the
analyzer or components.
WARNING — Warnings contain information to help prevent actions that may cause
personal injury.
KEYPAD FUNCTION- - The keypad icon indicates the section is applicable only when
using the keypad.
NOTE— Notes that apply to 21CFR11 environments only (Confirm applications).
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Table of Contents
Warranty i
Corporate Profile ii
Contact Us iii
About this Manual iv
1 About the AccuPyc II 1 - 1
About the TEC Module 1 - 2
Asphalt Density Application 1 - 3
About the FoamPyc Module 1 - 3
Instrument Components 1 - 5
Equipment Options and Upgrades 1 - 7
Configuration Options 1 - 8
Specifications for AccuPyc II 1 - 10
2 Data Entry with Keypad 2 - 1
About the Display 2 - 2
About the Keypad 2 - 3
Cancel an Analysis 2 - 6
Manual Mode 2 - 7
Transmit 2 - 8
Analysis Parameters 2 - 8
Review Data 2 - 11
View Data Results 2 - 13
Print a File 2 - 13
3 About the Software 3 - 1
Menu Structure 3 - 1
Common Fields and Buttons 3 - 2
Option Presentation 3 - 5
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Option Presentation for 21CFR11 Environments 3 - 7
File Status, Description, Extension, and Location 3 - 9
Keyboard Shortcuts 3 - 10
Default Methods 3 - 11
Analyzer Status 3 - 12
Show Instrument Log 3 - 12
Show Instrument Schematic 3 - 13
Show Status 3 - 14
Export Files 3 - 15
List Files 3 - 15
Open a Sample File 3 - 16
About the Software in 21CFR11 Environments 3 - 17
Software Uninstall 3 - 20
Software Updates 3 - 20
4 Create Sample Files 4 - 1
Sample Files 4 - 1
Sample Cup 4 - 5
Material Parameters 4 - 6
5 Parameter Files 5 - 1
Analysis Conditions 5 - 2
Report Options 5 - 5
6 Perform an Analysis 6 - 1
Prepare and Load a Sample 6 - 1
Perform an Analysis using the Software 6 - 3
QuickStart Analysis 6 - 7
Sequence Analysis 6 - 8
Review Analysis 6 - 9
7 About Reports 7 - 1
Open and Close Reports 7 - 1
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Start Reports 7 - 1
SPC Report 7 - 2
Report Features and Shortcuts 7 - 7
Graph Features and Shortcuts 7 - 11
Graph and Sample Overlays 7 - 16
Generate Multiple Graph Overlays 7 - 16
Generate Multiple Sample Overlays 7 - 18
Report Examples 7 - 20
Combined Report 7 - 20
Summary Report 7 - 21
Tabular Report 7 - 22
Graph Report 7 - 23
Overlay Report 7 - 24
Equilibration Report 7 - 25
Sample Log Report 7 - 26
8 Selected Reports 8 - 1
Combined Report 8 - 1
Density and Volume Table 8 - 2
Volume vs Cycle Number Trend Plot 8 - 3
Density vs Time Trend Plot 8 - 5
Equilibration Report 8 - 6
Options Report 8 - 8
Pressure and Volume Table 8 - 8
Sample Log Report 8 - 9
Summary Report 8 - 9
Total Pore Volume vs Temperature 8 - 10
Volume vs Cycle Number Trend Plot 8 - 10
9 Diagnostics using the Software 9 - 1
10 About Calibration 10 - 1
Calibrate using the Software 10 - 1
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Calibrate Pressure Scale 10 - 1
Calibration Report 10 - 2
Calibrate Temperature Offset 10 - 3
Calibrate Zero Cell Volume 10 - 4
Calibrate Zero Pressure 10 - 5
Reset Pressure Calibration 10 - 6
Calibrate Volume Scale 10 - 7
Verify Operation 10 - 12
Load Calibration from File 10 - 13
Save Calibration to File 10 - 13
Calibrate using the Keypad 10 - 14
Calibrate Function 10 - 14
Calibration Data 10 - 15
Calibrate Volume 10 - 16
Reset Pressure Calibration 10 - 17
Review Calibration 10 - 18
Temperature 10 - 20
Zero the Pressure Transducer & Chamber Volume 10 - 20
Load Calibration Data from a USBStick 10 - 21
Copy Calibration Data to a USBStick 10 - 21
11 Hardware 11 - 1
Add Analysis Module to Control Module 11 - 1
Analytical Balance 11 - 3
Brightness Control 11 - 4
Handling System Components 11 - 5
12 Maintenance and Troubleshooting 12 - 1
Chamber Cap O-Ring 12 - 3
Check the Cell and Expansion Chambers for Leaks 12 - 5
Clean the Dust Filter 12 - 7
Clean the Pycnometer 12 - 8
Guidelines for Connecting Gases 12 - 9
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Replace a Gas Cylinder 12 - 10
Regulator Pressure 12 - 12
Recover From a Power Failure 12 - 14
Reset the Pycnometer 12 - 14
Power Instrument On and Off 12 - 15
Service Test Mode 12 - 16
A Advanced Reports - Python Module A - 1
Advanced Report Options A - 2
Scripts A - 4
Python Reports A - 6
Acquire Overlay Sample Data A - 9
Enable the Use of Overlay Data A - 11
MicModule Python Calls A - 12
B Multigas Option B - 1
C MultiVolume Insert Option C - 1
D RS232 Pin Assignment D - 1
E Sample Volume Equation Derivation E - 1
F TEC Module F - 1
Set the TECTemperature F - 1
Operate the TEC Module F - 2
Volume Change with Temperature for the 10 cm3 AccuPyc F - 2
Volume Change with Temperature for the 100 cm3 AccuPyc F - 3
Asphalt Density Measurement F - 4
G Temperature Controlled AccuPyc G - 1
Attach a Circulating Bath G - 1
Add Analysis Modules to a Temperature Controlled Module G - 2
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H Transmitted Data H - 1
I Exported Data Example I - 1
Index Index - 1
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1 ABOUT THE ACCUPYC II
The AccuPyc II is an easy to use, fully automatic gas displacement pycnometer. It determines
density and volume by measuring the pressure change of helium within calibrated volumes. It also
reports the chamber temperature at the end of the requested cycles. The AccuPyc II can be
operated using the analysis program installed on an attached computer, or if no computer is attached
to the pycnometer, the keypad can be used to start and run analyses. If using the keypad, the
analyzer may be operated in English, French, German, Italian, or Spanish. The application is
available in English only.
The AccuPyc II consists of a control module and an analysis module. When ordering a single unit,
the control module is built into the same unit as the analysis module for convenience. The analysis
modules are also available in a standalone configuration, allowing multiple analysis modules to be
attached to a single controlling unit. A maximum of five analysis modules can be installed to one
controller (six total). Each module has its own gas connection. The pycnometer can be controlled by
either:
lWindows 10 interface. The operational status of the pycnometer can be continually monitored
in the application. If the Windows interface is used, the keypad is disabled.
lthe keypad if not running the Windows interface. A separate keyboard and printer can be
attached to the pycnometer using USBports.
1 About the AccuPyc II
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1 About the AccuPyc II
ABOUT THE TEC MODULE
See TEC Module on pageF - 1
Density measurements at specific temperatures are required for certain applications. The AccuPyc II
Thermo Electric Cooling (TEC) Module maintains an accurate temperature control during analysis
using the principle of Peltier cooling.
TEC Modules, also known as Peltier coolers, are solid-state heat pumps that utilize the Peltier effect
to move heat. By passing a current through the TEC Module, heat is transferred from one side of the
module to the other, typically producing a heat differential of approximately 40° C.
The transferred heat is then removed from the system through the combination of a heat sink and
fan, cooling the system to maintain a set temperature for accurate analysis.
TEC systems feature:
• fast dynamic response
• long-life
• no moving parts
• no use of refrigerants or circulated liquids / antifreeze
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ASPHALT DENSITY APPLICATION
The AccuPyc II TEC Module can measure asphalt density using disposable cups to limit cross-
contamination of samples.
This solution can be closely correlated (< 0.15% difference) to results obtained with ASTM Test
Method D70-09. The AccuPyc asphalt density measurement is completed much faster than the
ASTM method while virtually eliminating operator error. The Peltier thermoelectric cooling control
(15 to 36 °C) provides stability for handling of samples.
Performing an asphalt density measurement requires the AccuPyc II Asphalt application and
disposable sample cups.
ABOUT THE FOAMPYC MODULE
AFoamPyc option for measuring open and closed cell foam materials is available for both standard
and temperature controlled pycnometers. This unit can be ordered initially with the FoamPyc
application installed, or can be upgraded from the standard AccuPyc with a software enhancement
via USBmedia. Configuration options are:
l100 cm3nominal cell volume (recommended)
l10 cm3nominal cell volume
The FoamPyc option performs analyses on materials such as polystyrene, urethane, and rubber
foams using five different methods:
lCorrection using cell dimensions. Measures the closed cell fraction and corrects for the cells
damaged while cutting the sample to the necessary size and shape. This is accomplished by
using either the average cell diameter or the cell chord length (as defined in ASTM method D-
6226-15) and the measurements of the sample to determine the volume of the cut cells. This
volume is deducted from the total volume of the open cells measured by the pycnometer.
lCorrection by recutting sample. Corrects for the cut cells by using two separate meas-
urements. For the 2nd measurement, the sample is recut to double the amount of cut surface.
The observed difference in cut open cell volume is applied as a correction to the initial measured
volume. This method offers the distinct advantage that no assumptions are needed about the rel-
ative amounts of open and closed cells.
lNo correction. Does not correct for cut cells. It is used for materials with predominantly open
cells where good accuracy can be achieved without correction. The accuracy level deteriorates as
the percentage of closed cells increases.
lCompressibility test. The fill pressure is increased incrementally over the sample with each
repeat of the P1,P21 ) cycle. The apparent variation of the measured sample volume with the
1 ) Where P1 is the initial pressure to which the sample is charged, and P2 the final pressure after
expansion.
Asphalt Density Application
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1 About the AccuPyc II
average pressure is determined. This test is an approximate indication. It is not intended to be an
exact measure of the volume compressibility.Where P1 is the initial pressure to which the sample
is charged, and P2 the final pressure after expansion.
lCell fracture test. A perfectly rigid foam is assumed. First, a P1,P2 cycle is performed at the
lower of two specified P1 pressures, and the results stored. A second cycle is performed at a
higher specified value of P1, then a third cycle identical to the first cycle is performed. The dif-
ference between the volume of the sample on the first measurement and on the third meas-
urement is reported as the volume of fractured cells. It is assumed that cells fracture by exposure
to the highest pressure (2nd cycle) so that when the third measurement is made, the measured
sample volume has decreased from the first cycle by the amount of the closed cell volume which
was fractured.
The 100 cm3AccuPyc II has been designed and tested to follow the procedure in ASTM Method D
6226 for FoamPyc analyses. The 10 cm3and 350 cm3units can be used for some types of foam
materials; however, analyses on these AccuPycs will not conform to the ASTM method. The 1 cm3
AccuPyc II cannot be used to perform FoamPyc analyses.
The FoamPyc software also provides the capability to perform analyses in the Standard mode of
operation. This is especially convenient for users who have upgraded to the FoamPyc method from
the standard method. For example, a 100 cm3AccuPyc on which FoamPyc analyses are performed
and a 1 cm3analysis module attached on which standard analyses are performed.
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INSTRUMENT COMPONENTS
FRONT COMPONENTS
The sample chamber, located on the top panel, is where the sample container is placed for analysis,
or the standard for calibration.
The sample chamber should remain capped except when inserting or removing a sample. When left
uncapped, water vapor adsorbs on the inner surface of the chamber or the chamber temperature
becomes unstable; either condition can affect analysis results. If water vapor accumulates in the
chamber, the pycnometer must be purged.
The standalone control module, often used for the Glove Box pycnometer, does not contain a
sample chamber.
Component Description
Active indicator A blue LED which illuminates when an operation is in progress. It is included
on all analysis modules. It is not included on standalone control modules.
Display window Displays Remote Operation when the Windows application is being used.
The AccuPyc can be operated in the keypad mode when the Windows applic-
ation is closed.
Keypad Not used with AccuPyc software application.
Power indicator A green LED which illuminates when the analyzer is powered on.
Front Components
Instrument Components
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1 About the AccuPyc II
BACK COMPONENTS
Component Description
Analysis module
connector
Used to connect up to five analysis modules to the initial control / analysis mod-
ule. Each module contains analysis module input and output connectors.
Brightness con-
trol
Used to adjust the brightness of the display. See Brightness Control on
page11 - 4.
Dust filter (not
shown)
(For 2000 cm3units and high pressure units only.) Traps sample dust to pro-
tect internal valves.
Ethernet port Provides for setting up for e-mailing reports, sending data to a web browser,
or interfacing with the AccuPyc Windows application.
Gas inlet port Use to connect the analysis gas; helium is recommended. If multiple analysis
modules are attached, each module contains a gas inlet port. Multiple gases
can be attached using the Multigas option. See Multigas Option on pageB
- 1.
ON/OFF switch For powering the analyzer on and off.
Power connector For connecting the power source to the instrument.
RS232 port Used to transmit data only when using the keypad function. Also used to con-
nect to the analytical balance.
USB connectors Use for connecting a keyboard, printer, or balance to the instrument.
Back Components
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EQUIPMENT OPTIONS AND UPGRADES
Parts and accessories can be found online at www.Micromeritics.com.
HIGH PRESSURE CORE PYCNOMETER
Gas pycnometry is recognized as one of the most reliable techniques for obtaining skeletal volume
and density. The fully automatic AccuPyc High Pressure pycnometer provides high speed, high
precision volume measurements and density determinations on intact or crushed shale core
samples.
The high pressure pycnometer:
lOperates at a pressure of up to 500 psi to provide a better diffusion of the gas into the rock.
lHas a stainless steel sample chamber with a volume of 100 cm3.
lHas a sample chamber that can accommodate a 48 mm (1.85 in.) diameter core of up to 60 mm
(2.40 in.) in length.
LARGE VOLUME CORE PYCNOMETER
The AccuPyc Large Volume pycnometer sample chamber addresses the specific needs of
operations that require pore volume knowledge of intact drilling cores. This instrument eliminates the
need to break core samples into smaller pieces prior to analysis.
The large volume pycnometer:
lHas a large sample chamber with a volume of approximately 2000 cm3.
lHas a sample chamber that can accommodate a 95 mm (3.74 in.) diameter core of up to 278 mm
(10.9 in.) in length.
MULTIVOLUME INSERTS
The MultiVolume option is used to analyze smaller sized samples. Options are:
l1 cm3nominal cell volume; contains a 0.1 cm3cup
l10 cm3nominal cell volume; contains 1 cm3and a 3.5 cm3cups
l100 cm3nominal cell volume; contains 10 cm3and 35 cm3cups
l2000 cm3nominal cell volume, contains 650 cm3and 1300 cm3cups
Each kit includes inserts, reference standards, and sample cups.
Equipment Options and Upgrades
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1 About the AccuPyc II
MULTIGAS OPTION
The Multigas Option allows connection of up to four gases to one analyzer. See Multigas Option
on pageB - 1.
CONFIGURATION OPTIONS
For best fit with a sample, the AccuPyc II is available in multiple configurations.
All sample chamber volumes are nominal unless otherwise specified.
l1 cm3sample chamber
l10 cm3sample chamber
l100 cm3sample chamber
l350 cm3sample chamber
l2000 cm3sample chamber
l100 cm3High Pressure sample chamber
Best fit means the sample nearly fills the sample chamber and, therefore, optimizes the precision of
the results.
GLOVE BOX
Provides for analysis of samples in which a controlled environment is required.
Options Description
Configuration l1 cm3sample chamber
l10 cm3sample chamber
l100 cm3sample chamber
l350 cm3sample chamber
l2000 cm3sample chamber
l100 cm3High Pressure sample chamber
This unit consists of two separate modules. The controller is placed outside the glove box, while the
analysis module is placed inside the glove box. Up to six analysis modules may be placed in the glove
box, all controlled by one external control module.
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