Particulate Systems HPVA Series User manual

HPVA Series
High Pressure Volumetric Analyzer
Operator’s Manual
V4.0
P02-42801-01
March 2011

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Windows is a registered trademark of Microsoft Corporation.
© Particulate Systems 2011. All rights reserved. Printed in the U.S.A.
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.

WARRANTY
Particulate Systems, a brand operating under MICROMERITICS INSTRUMENT CORPORATION, warrants
for one year from the date of shipment each instrument it distributes 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 products distributed by MICROMERITICS under the Particulate Systems
brand 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 inspec-
tion 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 manufacturer 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 dis-
cretion 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 man-
ufactures 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.
4356 Communications Drive, Norcross, GA 30093
Fax [phone]
Domestic Sales - [phone]
Domestic Repair Service - [phone]
International Sales - [phone]
Customer Service - [phone]

Mar 2011 i
Table of Contents
1. Introduction
Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-1
Equipment Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-2
Controls and Connectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4
Upper Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4
Sample Compartment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-6
Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-7
Turning the Analyzer On and Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-8
Main Menu. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-9
Starting and Exiting the HPVA Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-10
File Names . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-10
Specifications. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-11
2. Performing an Experiment
Preparing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1
Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1
Cleaning the Sample Cylinder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-2
Weighing the Sample. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-4
Assembling the Sample Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-5
Degassing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-7
Attaching the Sample Holder to the Analysis Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-12
Purging the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-15
Running the Experiment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-20
Viewing the Experiment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-23
Displaying the Isotherm. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-23
Adjusting Flow Valves. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-26
Definitions of Fields in the System Windows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-27
Define New Experiment Window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-27
Define Run Window. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-29
3. Viewing Experiment Results
Running the Macro. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-1
Read Me Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-2
Gases Tab. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-2
Parameters Tab. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-3
Compile Error Message . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-5
Displaying Experiment Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-6
Read Long Data File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-6
Read Short Data File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-8
Read Helium Data File. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-13

Table of Contents HPVA Series Operator’s Manual
ii Mar 2011
4. Using the Manual Control Window
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Controlling Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Setting the Sample Bath Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3
5. Configuring the System
Calibrating the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Changing the Data Directory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Configuring the Hardware . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2
System Configuration Window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2
Instrument Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2
Tasks Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
Analog Input Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Analog Output Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
Instrument Options Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Dosing Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Adsorption Tab. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10
Free Space Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
6. Troubleshooting and Maintenance
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1
Resetting the Pressure Limit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
Entering the Slope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-5
Replacing Degas and Analysis Port O-Rings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
Connecting Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
Guidelines for Connecting Gases to the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
Required Items.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-7
Disconnecting the Depleted Bottle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-7
Connecting a Replacement Gas Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-8
Adjusting the Metering Valves. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-11
7. Ordering Information
A. Error Messages
B. Performing a Cryogenic Analysis
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1
Measuring Free Space. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-2
Performing a Blank Tube Experiment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-2
Displaying the Free Space . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-8
Preparing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-9

HPVA Series Operator’s Manual TableofContents
Mar 2011 iii
Conducting the Adsorption/Desorption Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-10
Analyzing the Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-16
INDEX

Table of Contents HPVA Series Operator’s Manual
iv Mar 2011

Mar 2011 1-1
1. Introduction
This manual describes how to operate and maintain the HPVA High Pressure Volumetric Analyzer,
Models HPVA-100 and HPVA-200.
Conventions

This manual uses the following conventions:

Indicates important information pertinent to the subject matter.


Provides information that helps you prevent actions that may damage
the instrument.

Provides information that helps you prevent actions that may cause
personal injury.
Blue words Indicate a link to additional information about the subject matter.

Equipment Description HPVA Series Operator’s Manual
1-2 Mar 2011
Equipment Description

The High Pressure Volumetric Analyzer (HPVA) from Particulate Systems is designed to obtain high-
pressure adsorption isotherms using gases such as hydrogen, methane, and carbon dioxide employing
the static volumetric method. The volumetric technique consists of introducing (dosing) a known
amount of gas (adsorptive) into the chamber containing the sample to be analyzed.When the sample
reaches equilibrium with the adsorbate gas, the final equilibrium pressure is recorded. These data are
then used to calculate the quantity of gas adsorbed by the sample. This process is repeated at given
pressure intervals until the maximum pre-selected pressure is reached. Each of the resulting equilib-
rium points (volume adsorbed and equilibrium pressure) is then plotted to provide an isotherm.
Excellent reproducibility and accuracy are obtained by using separate transducers for dosing the sam-
ple and for monitoring the pressure in the sample chamber.
The HPVA Series of analyzers includes two models: the HPVA-100, capable of achieving pressures up
to 100 bar and the HPVA-200, capable of achieving pressures up to 200 bar.
The HPVA Analyzer includes a separate degas port for drying the sample before testing. The furnace is
capable of temperatures up to 500 °C, controlled with a routine which includes ramp and soak
capabilities.

HPVA Series Operator’s Manual Equipment Description
Mar 2011 1-3
To protect the user, the HPVA includes a hydrogen gas sensor to detect excessive levels of H2 gas
should a leak in the system occur. If tripped, the safety circuit places the HPVA unit in a safe condition
by removing power to the unit and closing all valves.
Analysis results are displayed real-time on the computer screen during an experiment and details can
be viewed and printed via a Microsoft®Excel macro provided with the application software.
The standard system consists of a vacuum pump and gauge, a gas manifold maintained at a constant
temperature (40 °C typically) with two pressure transducers, a sample chamber, an outgassing furnace
with PID controller, a temperature control vessel that can be connected to a constant temperature bath,
and two stainless steel sample holders with diaphragm shut-off valves. The following is a schematic of
the HPVA system. A system schematic can be viewed from within the application software and can be
used to manually control the valves if required.

Controls and Connectors HPVA Series Operator’s Manual
1-4 Mar 2011
Controls and Connectors
Upper Front Panel
Pressure Display Manifold Temperature
System
Schematic
Valve Switches Vent Valve Vacuum Valve
Control Control
Control/Display
Furnace
Temp.
Control/
Display
Pressure Displays the manifold pressure when set to PM and the
sample pressure when set to PS. The display is useful as a
quick reference; a more accurate reading of the pressure
can be displayed on the software screen.
Manifold Temperature
Control and Display Displays the current manifold panel heater temperature in
degrees Celsius. Also enables you to increase or decrease
the set point temperature.
Furnace Temperature
Control and Display Displays the current furnace temperature in degrees
Celsius. Also enables you to increase or decrease the set
point temperature.

HPVA Series Operator’s Manual Controls and Connectors
Mar 2011 1-5
Vacuum Valve Control Enables you to control the flow rate through vacuum
valve 4.
Vent Valve Control Enables you to control the flow rate through the vent
valve.
Valve Switches Enable you to open and close valves. You can also open
and close valves 1 through 8 through the software, which
is the recommended method of manual control. 

Valve 9 can be controlled by the switch only.
System Schematic A schematic of the manifold, showing valve status. A
valve indicator turns on when the valve is open and turns
off when a valve is closed.
When the HPVA is performing an experiment or being operated in
manual control mode, the valve switches on the front panel should be
placed and remain in the closed (down) position.
If a switch is placed in the opened position during a software
operation, it will override the software and may damage the
instrument.

Controls and Connectors HPVA Series Operator’s Manual
1-6 Mar 2011
Sample Compartment
Thermocouple Connectors
Analysis Port Degas Port
Furnace
Temperature
Control Vessel
Temperature Control Vessel Maintains the temperature of the sample during an
experiment.
Analysis Port Port used to perform an experiment.
Thermocouple Connectors Connect the furnace thermocouples to the instrument.
Degas Port Port used to evacuate a sample (remove moisture and
contaminants) prior to performing an experiment.
Furnace Maintains the desired temperature during the preparation
process.

HPVA Series Operator’s Manual Controls and Connectors
Mar 2011 1-7
Rear Panel
Bath Communication Vacuum Vent Alarm Alarm Reset
On/Off Power Cord Air Gas1 Gas2 Gas3
Switch Connector
Bath Connects the recirculating bath to the instrument.
Communication Connects the computer to the instrument.
Vacuum Connects the vacuum pump to the instrument.
Vent Connects vent tubing to the instrument.
Alarm Turns on when power is applied to the instrument or when
the H2 sensor is triggered.
Alarm Reset Must be pressed after the instrument On/Off switch is
placed in the ON position and when the H2 sensor is
activated, which shuts off power.
On/Off Switch Turns power to the instrument on or off.
Power Cord Connector Connects the power cord from the power source to the
instrument.

Turning the Analyzer On and Off HPVA Series Operator’s Manual
1-8 Mar 2011
Turning the Analyzer On and Off

To turn on the analyzer:
1. Place the power switch on the rear panel of the analyzer in the ON ( | ) position. The alarm
indicator will light indicating that power is applied to the instrument.
2. Wait about 20 seconds, then press the ALARM RESET button on the back panel of the analyzer.
3. The alarm indicator will turn off.
4. Wait 30 to 60 minutes to allow the manifold temperature to stabilize.
To turn off the analyzer:
1. Ensure that the analyzer is vented to atmosphere.
2. Place the power switch on the rear panel of the analyzer in the OFF (O) position.
Air Connects the nitrogen or compressed air supply for the
pneumatic valves to the instrument.
Gas1 Connects an analysis gas to the instrument.
Gas2 Connects another analysis gas to the instrument.
Gas3 Connects helium (backfill gas) to the instrument.

HPVA Series Operator’s Manual Main Menu
Mar 2011 1-9
Main Menu

The Main Menu enables you to access all software functions of the HPVA system.
Calibration Used to calibrate the manifold volume. This function is
used by authorized service personnel only.
Adsorption Enables you to enter experiment conditions and to
perform an experiment.
Manual Control Enables you to manually control the system through a
schematic displayed on the screen.
Change Data DirectoryEnables you to change the directory in which experiment
data are stored.
Configure Hardware Enables you to change parameters that affect the
operation of the analyzer.
Help Displays the HPVA Series Operator’s Manual on the
screen. Use the Bookmarks and Table of Contents to find
the information you need.
Exit Closes the HPVA software.

Starting and Exiting the HPVA Software HPVA Series Operator’s Manual
1-10 Mar 2011
Starting and Exiting the HPVA Software

To start the HPVA software, click the HPVAicon on your desktop or select the software using the
appropriate Windows function.
To close the HPVA software, click the Exit button on the HPVA Main Menu.
File Names

The following table shows the file name extensions used by the HPVA software.
File Type Extension
Data file - generated only if Advanced Mode is activated;
primarily used to troubleshoot the instrument; contains data for
everything that occurred during the analysis
dat
Long data file - contains the manifold and sample pressures and
temperatures recorded over time
HIlo
Short data file - used for the isotherm calculations HIsh
Helium free space data file - used to calculate free space in the
sample tube
HIHe
Analysis parameters file -used to load previous analysis
conditions prior to the experiment
HItm

HPVA Series Operator’s Manual Specifications
Mar 2011 1-11
Specifications
Characteristic Specification
Environment
Temperature: 10 to ºC, operating; -10 to 55 ºC, storing or shipping
Humidity: 20 to 80% relative, non-condensing
Physical
Height 35 in. (88.9 cm)
Width: 20 in. (50.8 cm)
Depth: 20 in. (50.8 cm)
Weight: 60 lbs
Electrical
Voltage: 115/230
Power: 15 Amps
Frequency: 50 to 60 Hz
Gases
Handles typical adsorbates such as Nitrogen, Hydrogen, Methane, Argon, Oxygen, Carbon
Monoxide, and Carbon Dioxide.
Pressure
Pressure range HPVA-100: vacuum to 100 bar, HPVA-200: vacuum to 200 bar
Pressure transducer Pressure reading accuracy is +0.04% full scale with a stability 
of +0.1%
Computer
Minimum requirements: Intel Core 2 Duo processor - 2.0 GHz or faster
One DVD ROM drive
1 gigabyte of RAM
20-gigabyte hard disk space
SVGA Monitor
Windows®XP Professional or Windows 7; Microsoft®Excel
2002 or higher
PCI slot for National Instruments control board
One RS232 serial port for each attached instrument and acces-
sory requiring an RS232 connection
Mouse
Printer that is IBM Graphics or Epson LQ compatible (optional)
UPS for computer (optional)

Specifications HPVA Series Operator’s Manual
1-12 Mar 2011