HPVAII Series

High Pressure Volumetric Analyzer

Operator’s Manual
V1.0

P02-42806-01
March 2013
Excel and Windows are registered trademarks of Microsoft Corporation.
Alconox is a registered trademark of the Alconox Company.
Viton is a registered trademark of DuPont Dow Elastomers L.L.C.

© Particulate Systems 2013. 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 (770) 662-3696
Domestic Sales - (770) 662-3633
Domestic Repair Service - (770) 662-3666
International Sales - (770) 662-3660
Customer Service - (770) 662-3636
HPVAII Series Operator’s Manual Table of Contents

TABLE OF CONTENTS

1. GENERAL INFORMATION
Operator’s Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
Equipment Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5

2. USER INTERFACE
Controls and Connectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Upper Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Sample Compartment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Turning the Analyzer On and Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Main Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Starting and Exiting the HPVAII Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
File Names . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Hover Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6

3. EXPERIMENT PROCEDURES
Preparing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Cleaning the Sample Cylinder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Weighing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
Assembling the Sample Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5
Degassing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Attaching the Sample Holder to the Analysis Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-10
Purging the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12
Performing the Experiment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-17
Viewing Experiment Progression . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-20
Displaying the Isotherm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-20

4. MAIN MENU
Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Adsorption . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Experiment Definition New . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Step Isotherm: Define Run Window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4
Manual Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
Controlling Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
Setting the Sample Bath Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8
Change Data Directory. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9

Mar 2013 i
Table of Contents HPVAII Series Operator’s Manual

Configure Hardware . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-10

Instrument Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-10
Tasks Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-12
Analog Input Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-13
Analog Output Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-14
Instrument Options Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-15
Dosing Tab. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-17
Adsorption Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-19
Free Space Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-21
Help. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-22
Exit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-22

5. EXPERIMENT RESULTS
Running the Macro . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Parameters Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2
Gases Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
Read Me Tab. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Compile Error Message . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Displaying Experiment Data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
Isotherm Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
Free Space Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
Long Data Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12

6. TROUBLESHOOTING AND MAINTENANCE

Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1
Resetting the Pressure Limit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
Replacing Degas and Analysis Port O-Rings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
Connecting Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
Guidelines for Connecting Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
Disconnecting the Depleted Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
Connecting a Replacement Gas Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-5
Adjusting the Metering Valves. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-9

7. ORDERING INFORMATION

A. ERROR MESSAGES

B. CRYOGENIC ANALYSIS
Measuring Free Space. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-2
Performing a Blank Tube Experiment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-2
Displaying the Free Space . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-7

ii Mar 2013
HPVAII Series Operator’s Manual Table of Contents

Preparing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-8

Performing the Adsorption/Desorption Analysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-9
Viewing the Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-14

C. SOFTWARE INSTALLATION

INDEX

Mar 2013 iii

 1. GENERAL INFORMATION

This manual describes how to operate and maintain the HPVAII High-Pressure Volumetric
Analyzer, Models HPVAII-100 and HPVAII-200.

Operator’s Manual
The HPVAII operator’s manual is organized as follows:

Chapter 1 General Information

Provides a general description of the HPVAII system as well as its
specifications.

Chapter 2 USER INTERFACE

Provides basic hardware and software interface

Chapter 3 EXPERIMENT PROCEDURES

Provides step-by-step instructions for experiment procedures.

Chapter 4 MAIN MENU

Provides a description of the options on the HPVAII main menu.

Chapter 5 EXPERIMENT RESULTS

Provides a description of the Excel Macro which is used to view and
manipulate experiment results.

Chapter 6 TROUBLESHOOTING AND MAINTENANCE

Provides instructions for troubleshooting hardware problems and for
performing routine maintenance procedures

Chapter 7 ORDERING INFORMATION

Provides part numbers and descriptions of the HPVAII components and
accessories.

Appendix A ERROR MESSAGES

Lists the error messages that may be displayed in the analysis program;
includes a cause and action for each.

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Operator’s Manual HPVAII Series Operator’s Manual

Appendix B CRYOGENIC ANALYSIS

Provides instructions for using the Cryogenic options to perform cryogenic
analyses.

Appendix C SOFTWARE INSTALLATION

Provides instructions for installing the HPVAII software.

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.

Light Blue text Indicate a link to additional information about the subject matter.

1-2 Mar 2013

HPVAII Series Operator’s Manual Equipment Description

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 equilibrium points (volume adsorbed and equilibrium
pressure) is then plotted to provide an isotherm.

The HPVAII Series of analyzers includes two single-station models: the HPVAII-100, capable of
achieving pressures up to 100 bar and the HPVAII-200, capable of achieving pressures up to 200
bar.

The HPVAII Analyzers 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.

Mar 2013 1-3

Equipment Description HPVAII Series Operator’s Manual

As a safety measure, the HPVAII includes a hydrogen gas sensor to detect excessive levels of H2
gas should a leak in the system occur. If tripped, the safety circuit closes all valves and turns off the
HPVAII unit.

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
circulating temperature bath, and two stainless-steel sample holders with diaphragm shut-off
valves.

The following is a system schematic which can be viewed from within the application software
and can be used to manually control the valves if required.

1.000

1000.00

35.00

25.00

1-4 Mar 2013

HPVAII Series Operator’s Manual Specifications

Specifications

Characteristic Specification

Environment

Temperature: 10 to 30 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 (27.2 kg)
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: HPVAII-100: vacuum to 100 bar

HPVAII-200: vacuum to 200 bar
High Pressure  Pressure reading accuracy is + 0.04% full scale with a stability of 
transducer: + 0.1%
1000-Torr Pressure Pressure reading accuracy is + 0.15% of reading
transducer:

Mar 2013 1-5

Specifications HPVAII Series Operator’s Manual

Characteristic Specification

Computer

Minimum  Intel Core 2 Duo processor - 2.0 GHz or faster

requirements:
One DVD ROM drive

1 gigabyte of RAM

20-gigabyte hard disk space

SVGA Monitor

Windows® XP Professional or Windows 7 (32-bit); 

Microsoft® Excel 2002 or higher

Mouse

Printer that is IBM Graphics or Epson LQ compatible (optional)

UPS for computer (optional)

1-6 Mar 2013

 2. USER INTERFACE

Controls and Connectors

Upper Front Panel

Manifold temperature
and control

H2 Fault

Furnace temperature
and control

Manifold Temperature Displays the current manifold panel heater temperature in degrees
Control and Display Celsius. Use the up/down arrows on the display to increase or
decrease the set point temperature. You must hold down the *
(asterisk) button when using the arrows.

Furnace Temperature  Displays the current furnace temperature in degrees Celsius. Use
Control and Display the up/down arrows on the display to increase or decrease the set
point temperature. You must hold down the * (asterisk) button
when using the arrows.

H2 Fault Illuminates when instrument is turned on or if the hydrogen

sensor is triggered. Press the Alarm Reset button on the rear
panel to reset; the H2 Fault light will turn off.

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Controls and Connectors HPVAII Series Operator’s Manual

Sample Compartment

Thermocouple Connectors

Analysis Port Degas Port

Furnace

Temperature
Control Vessel

Temperature Control  Maintains the temperature of the sample during an experiment.

Vessel

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.

2-2 Mar 2013

HPVAII Series Operator’s Manual Controls and Connectors

Rear Panel

Alarm Reset
Bath Communication Vent

On/Off Power Cord Connector Vacuum Air Gas 1 Gas 2 Gas 3

Switch

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 Reset Resets the instrument to a ready state. It is used when the
instrument is turned on or if the H2 sensor is activated.

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.

Air Connects the nitrogen or compressed air supply for the pneumatic
valves to the instrument.

Mar 2013 2-3

Turning the Analyzer On and Off HPVAII Series Operator’s Manual

Gas1 Connects an analysis gas to the instrument.

Gas2 Connects another analysis gas to the instrument.

Gas3 Connects helium (backfill gas) to the instrument.

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 H2 Fault
LED on the front panel illuminates indicating that power is applied to the instrument.

2. Wait approximately 20 seconds, then press the ALARM RESET button on the back panel of
the analyzer.

3. The alarm indicator will turn off.

4. Allow 30 to 60 minutes for 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.

2-4 Mar 2013

HPVAII Series Operator’s Manual Main Menu

Main Menu
The Main Menu enables you to access all software functions of the HPVAII system. Refer to
MAIN MENU, page 4-1 for a detailed description of the options on the menu.

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 Directory Enables 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 HPVAII Series Operator’s Manual. Use the

Bookmarks and Table of Contents to locate the information you
need.

Exit Closes the HPVAII program.

Mar 2013 2-5

Starting and Exiting the HPVAII Software HPVAII Series Operator’s Manual

Starting and Exiting the HPVAII Software

Start the HPVAII software: Double-click the HPVAII icon on your desktop or select the
program using the appropriate function for the Windows operating system.

Close the software: Click the Exit button on the HPVAII M ain Menu.

File Names
The following table shows the file name extensions used by the HPVAII software.

File Type Extension

Data file - generated when Advanced Mode is activated. Primarily used to dat
troubleshoot the instrument; contains data for everything that occurred during the
analysis

Long data file - contains the manifold and sample pressures and temperatures HIlo
recorded over time

Short data file - contains data used for the isotherm calculations HIsh

Helium free space data file - contains data used to calculate free space in the HIHe
sample tube

Analysis parameters file - used to load previous analysis conditions prior to the HItm
experiment

Hover Menus
The fields of the experiment dialogs contain a hover menu. Simply hover at the field of interest
and a brief description is displayed. This example shows the hover menu for the Measure FS
option.

2-6 Mar 2013

 3. EXPERIMENT PROCEDURES

This chapter provides step-by step instructions for performing experiment procedures including:

• Preparing a sample
• Degassing a sample
• Entering experiment parameters
• Running an experiment
• Viewing experiment isotherm

Preparing the Sample

Requirements
The following items are required to prepare a sample and perform an experiment with the
HPVAII analyzer.

Supplied by User Supplied by Particulate Systems

• Ultrasonic bath • Sample holder assembly

• Long-stemmed pipette • 5/8-in wrench

• Drying oven • 3/4-in. wrench

• Dry, compressed nitrogen or air to dry  • Funnel

sample cylinder

• Isopropyl alcohol (IPA); acetone or

deionized water may be used if IPA is
unavailable

• Balance

• Detergent

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Preparing the Sample HPVAII Series Operator’s Manual

Cleaning the Sample Cylinder

1. Preheat the drying oven to 110 °C.

2. Clean the sample cylinder using a ratio of 5 grams of detergent (Alconox or a similar
product) per 500 mL of warm water. Fill the bowl of the ultrasonic unit with enough water
to cover the sample cylinder. Ensure that the detergent is dissolved before placing the
sample cylinder into the water.

3. Submerge the sample cylinder in the bath and fill a long-stemmed pipette with water. Pipe
the water into the cylinder to remove all air.

4. Turn on the ultrasonic bath and allow it to run for approximately 30 minutes.

5. Using latex gloves, remove the sample cylinder from the bowl. Fill a pipette with hot water
and then pipe the water into the cylinder to rinse it. Repeat this process several times.

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HPVAII Series Operator’s Manual Preparing the Sample

6. Rinse the cylinder with Isopropyl Alcohol.

7. Using dry, compressed nitrogen or air dry the interior of the sample tube.

8. Place the sample cylinder into a drying oven that has been preheated to 110 °C.

9. Bake for two hours. Using insulated gloves, remove the cylinder and allow it to cool.

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Preparing the Sample HPVAII Series Operator’s Manual

Weighing the Sample

1. Tare the balance and allow it to stabilize at zero.

2. Place the sample cylinder on the balance and record the weight as Weight of empty sample
cylinder.

3. Remove the sample cylinder from the balance and place a funnel in the sample cylinder.

4. Slowly add the sample material to the cylinder.

5. Tare the balance and allow it to stabilize at zero.

6. Place the sample cylinder, with sample, on the balance. Record the weight as Weight of
sample cylinder plus sample.

7. Subtract the Weight of sample cylinder (recorded earlier) from the Weight of sample
cylinder plus sample. The value obtained is Weight of sample, which you will enter when
starting the experiment.

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HPVAII Series Operator’s Manual Preparing the Sample

Assembling the Sample Holder

1. Place the gasket on the sample cylinder as shown below.

Gasket

Two types of gaskets are available. One is filtered, the other one is not. It
is best to use a filtered gasket for fine powders. The non-filtered gasket is
sufficient for other types of materials.

Note that the gasket can be used only once. Reusing the gasket may
cause leaks at the sample holder connection.

2. Place the upper portion of the sample holder on the cylinder and hand-tighten the connector
nut.

Connector
Nut

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Degassing the Sample HPVAII Series Operator’s Manual

3. Use the 5/8- and 3/4-in. wrenches to tighten the connector an additional 1/8 turn.

Degassing the Sample

1. Insert the furnace thermocouple cables into the thermocouple connectors inside the sample
compartment.

2. Plug the furnace power cord into the power connector inside the sample compartment.
Thermocouple Connectors

Power Connector

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HPVAII Series Operator’s Manual Degassing the Sample

3. Tilt the furnace, then insert the sample holder assembly into the furnace.

4. Ensure that the O-ring is in place, then attach the sample holder to the degas port; hand-
tighten the connector nut.

O-ring

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Degassing the Sample HPVAII Series Operator’s Manual

5. Using the 3/4-in. and 5/8-in. wrenches to tighten the nut just until snug.

Do not over-tighten the connector nut, doing so could damage the port
fitting.

6. Use the Manual Control screen to open Valve 10 to begin evacuation.

1.000

1000.00

35.00

25.00

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HPVAII Series Operator’s Manual Degassing the Sample

7. Slowly open the isolation valve on the sample holder by turning it completely
counterclockwise.

Turn isolation valve

counterclockwise

8. Use the Manual Control screen to monitor the vacuum gauge to ensure the vacuum is
reached.

9. Hold down the * (asterisk) button and use the up or down button to set the desired furnace
temperature. Allow the sample to degas for an appropriate amount of time.

Asterisk Up
Down

10. Turn the isolation valve completely clockwise to end the degas procedure.

11. Use the Manual Control screen to close valve 10.

12. Set the furnace to 0 °C and allow the sample to cool to room temperature.

13. After the sample has cooled to room temperature, use the 3/4-in. and 5/8-in. wrenches to
loosen the connector nut and remove the sample holder from the degas port.

14. Ensure that the O-ring remains in place in the degas port, then place a cap on the port.

15. Tilt the furnace and remove the sample holder assembly from the furnace.

Mar 2013 3-9

Attaching the Sample Holder to the Analysis Port HPVAII Series Operator’s Manual

Attaching the Sample Holder to the Analysis Port

1. Attach the supply (bottom) and return (top) hoses from the temperature control vessel to
the ports inside the sample compartment. Make sure the hoses are connected to the
appropriate input and output ports from the circulating bath.

Return

Supply

The port assignment above reflects the supply coming from the top port and the return
exiting through the lower one. Either port can be used for input/output as long as the hoses
from the vessel match the port assignment. The vessel should always fill at the bottom to
ensure efficient temperature control.

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HPVAII Series Operator’s Manual Attaching the Sample Holder to the Analysis Port

2. Tilt the temperature control vessel and insert the sample holder into the vessel.

3. Ensure that the O-ring is in place, then attach the sample holder to the analysis port and
hand-tighten the connector nut.

O-ring

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Purging the System HPVAII Series Operator’s Manual

4. Using the 3/4 in and 5/8 in. wrenches, tighten the nut just until snug.

Do not over-tighten the connector nut, doing so could damage the port
fitting.

Purging the System

1. Click Manual Control from the Main Menu to display the Manual Control screen.

1.000

1000.00

35.00

25.00

To open and close a valve, select the desired valve and double-click the left mouse button or
press the spacebar. Yellow indicates a closed valve and green indicates an open valve.

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HPVAII Series Operator’s Manual Purging the System

2. Open valves 1 and 3. Observe the High Pressure Transducer pressure displayed on the
screen. There should be no pressure on the manifold (reading should be 1 bar or less).

1.000

1000.00

.
35.00

25.00

3. Double-click on the Vac Servo valve and set the valve to 0.30 bar; wait until the set pressure
is attained.

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Purging the System HPVAII Series Operator’s Manual

4. Open valve 5. Leave the valves (1, 3, and 5) open until the internal Vacuum Gauge reads
the minimum value specific for the vacuum pump.

0.000

1000.00

35.00

25.00

5. Close valve 5 and turn off the Vac Servo valve.

6. Open valve 8. Pressurize the instrument until the reading for the High Pressure
Transducer is 5 bar, or the maximum pressure available from the helium cylinder and
regulator; use whichever is less..

5.000

1000.00

35.00

25.00

Close valve 8.

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HPVAII Series Operator’s Manual Purging the System

7. Open valve 2. Double-click on the Vent servo valve and to set the system pressure to 2 bar
or lower.

8. Open Valve 4.

9. When the pressure reaches 1 bar or less, close Valves 2 and 4.

10. Repeat steps 2 through 8 two times, then proceed to step 11.

11. Double-click on the Vac servo valve and set the pressure 0.3 bar; wait until pressure level is
attained.

12. Open valve 5 to perform the unrestricted evacuation.

13. When the system reaches full vacuum, open the isolation valve on the sample holder by
turning it completely counterclockwise.

Isolation valve

14. Plug the temperature probe cable into the connector on the instrument.

15. Insert the temperature probe into the temperature control vessel.

Connector

Temperature
Probe

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Purging the System HPVAII Series Operator’s Manual

16. Add the appropriate liquid to the temperature control vessel until the level reaches about ½
inch from the top.

17. Double-click the Bath icon and set the circulating bath controller to the desired
temperature.

If the circulating bath is not interfaced with the HPVAII software, manually
set the desired temperature on the bath controller.

18. Close all valves.

19. You are now ready to run the experiment.

3-16 Mar 2013

HPVAII Series Operator’s Manual Performing the Experiment

Performing the Experiment

The Adsorption option on the Main Menu is used to define and perform experiments. This func-
tion involves the following windows:

• Experiment Definition: enables you to enter a sample ID and sample information.

• Step Isotherm Define Run: enables you to specify experiment parameters.
• Manual Control: enables you to perform manual operations as needed for the experiment.

The HPVAII software allows you to perform multiple experiments, or runs, in sequential order
for one sample. For example, if you have a sample you wish to analyze at different temperatures,
you can add multiple runs with the desired temperatures.You can edit the order of the runs using
the buttons to the right of the run list.

The software also enables you to save experiment parameters in a Template. Once a template is
created, you can use it for other experiments by just loading it into the System Definition win-
dow and entering a unique Experiment ID. You can modify the template as needed and save the
changes as another template if desired.

The following is a general procedure for entering experiment parameters, starting the experi-
ment, and viewing the isotherm. Refer to Experiment Definition New, page 4-2 for details about
the fields on this window.

1. Click Adsorption on the Main Menu to display the Experiment Definition New window.

The Manual Control Screen also displays with the Experiment Definition window. This
allows you to operate valves or set values while specifying experiment parameters.

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Performing the Experiment HPVAII Series Operator’s Manual

2. Choose one:

• Click Recall Template to copy the values of an existing template into the current file.
You can edit any parameter you wish.

• Proceed to the next step to define a new set of parameters

3. Enter a unique ID in the Expt ID field. You may use up to 12 characters.

4. Enter an Operator ID for the experiment.

5. Enter the weight of the prepared sample. If the sample chamber is empty (blank), enter 1.
The experiment will not begin if the weight is 0.

6. Enter the sample name and, optionally, the lot number and any pertinent notes.

7. Click Add to add run parameters to the experiment. The HPVAII Step Isotherm: Define
Run window is displayed.

8. Add the parameters for the run, then click OK. Refer to Step Isotherm: Define Run Window,
page 4-4 for a description of the fields on this screen.

9. Repeat steps 7 and 8 for each run you wish to add to the experiment.

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HPVAII Series Operator’s Manual Performing the Experiment

10. When you have finished entering information, click Run Experiment on the System
Definition Experiment window. The Save Experiment Template window prompting you to
save the template is displayed.

11. Enter a name for the template if you wish to save it, then click Save.

12. You can view the isotherm as the experiment progresses (described in the next topic).

Mar 2013 3-19

Viewing Experiment Progression HPVAII Series Operator’s Manual

Viewing Experiment Progression

Displaying the Isotherm

During an experiment, a screen similar to the example below is displayed. If you would like to
zoom into an area of the graph, hold the Ctrl key and drag, selecting an area with the left mouse
button. To return to the full graph, double-click in the graph.

Pressure The current pressure readings of the high-pressure and 1000-Torr

transducers.

Temperature The current temperature readings of the manifold and sample RTDs.

Graph Type Select the type of graph you wish to display, you may choose:

• Temp vs Time
• Pressure vs Time

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HPVAII Series Operator’s Manual Viewing Experiment Progression

View Parameters Displays the Modify Current Run Parameters window, enabling you to
change parameters for any step that has not completed.

View FS Data Enables you to view free-space data.

Ambient gives the free space at ambient temperature.

Analysis gives the free space at the analysis temperature.

Row 1 shows the values at ambient temperature

Row 2 shows the values at the analysis temperature.

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Viewing Experiment Progression HPVAII Series Operator’s Manual

View FS Data The column contents are as follows:

(continued)
Pm0 (1000T) Initial manifold pressure, 1000-torr transducer
Pm0 Initial manifold pressure, HP transducer
PmA (1000T) Manifold pressure before dosing, 1000-torr
transducer
PmA Manifold pressure before dosing, HP transducer
TmA Manifold temperature before dosing
PmB (1000T) Manifold pressure after dosing, 1000-torr
transducer
PmB Manifold pressure after dosing, HP transducer
TmB Manifold temperature after dosing
Ts Sample temperature after dosing
Vol Quantity dosed into sample chamber

3-22 Mar 2013

 4. MAIN MENU

This chapter describes the options on the Main Menu.

Calibration
Click Calibration to display the Calibration window.

Calibration requires the use of a known volume cylinder. This option should be used only by
authorized service personnel, or under their direction.

Mar 2013 4-1

Adsorption HPVAII Series Operator’s Manual

Adsorption
This option displays the windows required to specify experiment parameters and to run the
experiment.

Experiment Definition New

This windows displays when you click Adsorption on the Main Menu.

Exp ID Enter the experiment identifier. The data files created will use this
name. You may enter up to 12 characters.

Operator ID Enter the name or initials of the operator.

Sample Weight Enter the sample weight obtained during sample preparation.

Sample Name Enter the name you wish to assign to the sample.

Lot # If the sample has a designated identification number, enter it here.

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HPVAII Series Operator’s Manual Adsorption

Notes (1) and (2) Use these fields to enter additional information about the sample.

Add Displays the Step Isotherm Define Run window (see page 4-4)
enabling you to add a run to the experiment.

Edit Displays the Step Isotherm Define Run window (see page 4-4)
enabling you to edit the selected run.

Cut Use these buttons to rearrange the order of runs for the experiment.
Paste Above
Paste Below

Recall Template Enables you to load a saved template.

Save Template Allows you to save the current experiment definition as a template
to use for future experiments.

Run Experiment Starts the experiment.

Help Displays the HPVAII operator’s manual.

Close Closes the Experiment Definition New window and returns to the
Main Menu.

Mar 2013 4-3

Adsorption HPVAII Series Operator’s Manual

Step Isotherm: Define Run Window

Equilibration Criteria Enter the pressure fluctuation tolerance over a period of time for the
high-pressure and low-pressure transducers.

Enter the maximum equilibration time in minutes in the min

maximum field (last field)

This criteria specifies when the system has reached equilibrium after
each step in the adsorption/desorption procedure.

Temperature The options in this group box enable you to specify temperature
requirements.

Control Method Select Bath if a recirculation bath or cryostat is to be used.

Select External if the furnace or a Dewar is to be used.

4-4 Mar 2013

HPVAII Series Operator’s Manual Adsorption

Experiment Temp: Enter the temperature for the experiment in °C.

Hold: Enter the number of minutes the system should wait after the
sample RTD reaches the experiment temperature. A hold time of at
least 60 minutes is recommended if a liquid nitrogen bath is used.

Ambient Temp: Enter the temperature of the air in the laboratory in °C.

Hold: Enter the number of minutes the system should wait after the
sample RTD reaches the ambient temperature.

Evacuation Time Enter the number of minutes you wish to evacuate the sample after
running the free-space routine.

Adsorbate Name: Enter the name of the gas to be used for the experiment. This
gas should match the one in the Adsorbate column on the Gases tab
of the Excel macro spreadsheet.

Gas Port: Select the port (6 or 7) to which the adsorbate gas tank is
attached to the instrument. If the adsorbate is a gas mixture, check
Mixture.

Data Logging Interval Enables you to specify how often data points are collected either by
time or by pressure.

Enter a number of minutes in the min field or a pressure in the bar

field.

This is typically set to every 2 minutes or whenever the system

pressure changes by 0.005 bar.

Pressure Steps This group box enables you to specify pressures the sample holder
will reach during the experiment when the standard dosing mode is
used.

Enter a pressure (in bars) in the Pressure field, then click Add to
add a step.

Highlight a step in the table and click Delete to remove a pressure

step.

The first three steps entered in the table are automaticxally used as
the dosing pressures. Select Use as dose pressure to set each
pressure step as the dosing pressures.

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Adsorption HPVAII Series Operator’s Manual

Port 1 This group box enables you to specify free-space criteria.

Measure FS Click this option if you wish to have a free-space analysis conducted
prior to the isotherm experiment.

Ambient FS Enabled when Measure FS option is deselected, allowing you to

enter the ambient free-space volume of the sample tube.

Exper FS Enabled when Measure FS option is deselected, allowing you to

enter the experiment free-space volume of the sample tube.

OK Saves all run parameters and returns to the Experiment Definition

window.

Cancel Discards your entries and returns to the Experiment Definition

window.

Help Displays the HPVAII operator’s manual.

4-6 Mar 2013

HPVAII Series Operator’s Manual Manual Control

Manual Control
The Manual Control option shows a schematic of the HPVAII System. It can be used to:

• manually open and close valves

• set the sample temperature when a temperature control bath or cryostat is used.

High-pressure transducer 1.000

Low-pressure transducer 1000.00

Manifold temperature 35.00

Sample temperature 25.00

Anglysis station Degas station

The manifold and sample pressures and temperatures are displayed in real-time and are con-
stantly updated.

Controlling Valves

There are 12 valves on the schematic; 10 numbered pneumatic valves and two servo valves.:

Valve Description
1 Analysis port valve
2 Vent valve
3 Manifold valve
4 Full vent valve
5 Full vacuum valve
6 Adsorptive gas 1 valve
7 Adsorptive gas 2 valve
8 Helium gas valve
9 1000-torr isolation valve
10 Degas port valve

Mar 2013 4-7

Manual Control HPVAII Series Operator’s Manual

You can open and close a valve by double-clicking the left mouse button on the valve icon or by
clicking the valve icon then pressing the space bar. Yellow indicates a closed valve and green
indicates an open one.

Do not open the vacuum valve (Valve 5) when there is high pressure
(pressure greater than 1.5 bar) in the manifold. The software cannot
control the pressure in the manifold when the valves are manually
operated.

The Vac and Vent servo valves are opened and closed in the same manner as explained above.
When you open either servo valve; a dialog prompting you to enter a target pressure is displayed.

Enter or select the desired pressure, click OK, and the servo opens. The servo valves are indi-
cated closed when black, and open when green.

Setting the Sample Bath Temperature

If a temperature control bath or cryostat is configured with the instrument, you can set the bath
temperature using the Manual Control screen as follows:

1. Double-click the left mouse button on the Bath icon; the Bath Temperature dialog is
displayed.

Bath icon

2. Enter the temperature, then click OK.

4-8 Mar 2013

HPVAII Series Operator’s Manual Change Data Directory

Change Data Directory

This command is used to create a directory, or to select a different directory in which the files
produced by the system are placed.

Click Change Data Directory from the Main Menu; the following window is displayed.

Click here to create new folder.

Select the desired folder, or click the New Folder icon and name the folder. Then click Done.

Mar 2013 4-9

Configure Hardware HPVAII Series Operator’s Manual

Configure Hardware
Configure Hardware displays the System Configuration window, which contains 8 tabs of
parameters that are either entered at installation or are default values. You should not edit these
values unless directed by your service representative.

Instrument Tab

Serial number The instrument’s serial number. If an incorrect serial number

is entered, the software will not be able to locate the
instrument’s calibration data.

Pressure limit The highest pressure the manifold will be allowed to reach.
For a HPVAII-100, the maximum should be set no higher than
120 bar and for a HPVAII-200, the maximum should be set no
higher than 202 bar.

Low pressure limit The highest pressure the system will allow the 1000-torr
transducer to reach. This value should be set lower than the
maximum of the transducer range (1.3 bar).

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HPVAII Series Operator’s Manual Configure Hardware

Low pressure match During low-pressure dosing, the high-pressure transducer is

offset-calibrated to match the current low-pressure transducer
reading. The value shown here is the threshold above which
the calibration is not performed.

Unrestricted evac  When the system vacuums down the manifold, the Vac servo is
pressure used until this pressure is reached. When reached, the system will
open Valve 5, allowing a strong vacuum to be applied to the
system.

Default ambient temp The air temperature of the lab.

Data directory Click the ellipsis (…) button next to the Data directory field to
change the directory in which data files are written (this is more
conveniently done using the Change Data Directory option on the
Main Menu).

Advanced mode This option allows you to operate the instrument in Advanced
Mode and should only be used under the direction of a
Micromeritics/Particulate Systems service representative.

Mar 2013 4-11

Configure Hardware HPVAII Series Operator’s Manual

Tasks Tab

The tasks listed in this dialog are all configured with the NIMAX software during soft-
ware installation.

Analog Input Tasks The tasks used to read data from the instrument.

Analog Output Tasks The tasks used to send analog signals from the instrument.

Digital Output Tasks The tasks used to control the instrument valves.

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HPVAII Series Operator’s Manual Configure Hardware

Analog Input Tab

This dialog shows the slope and intercept for linear calibrations.

Manifold High  Linear calibration of the high-pressure manifold transducer.

Pressure The slope values for the HPVA II systems are:

HPVAII-100 = 13.7895
HPVAII-200 = 20.6843

Manifold Low  Linear calibration of the 1000-torr transducer

Pressure

Manifold Temp Linear calibration of the manifold RTD.

Sample Temp Linear calibration of the sample RTD.

Vacuum Gauge Linear portion of the vacuum gauge.

Mar 2013 4-13

Configure Hardware HPVAII Series Operator’s Manual

Analog Output Tab

Calibration The values used for the temperature calibration of the

temperature control bath.

Limits These are the limits for the bath temperature and voltage when
Bath is selected on the System Step Isotherm window.

Min bath temp

The minimum analysis temperature allowed.

Max bath temp

The maximum analysis temperature allowed.

Min volts out 

The minimum voltage the system is allowed to output to the
bath.

Max volts out 

The maximum voltage the system is allowed to output to the
bath.

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HPVAII Series Operator’s Manual Configure Hardware

Instrument Options Tab

Digital Output Tasks Displays the NIMAX tasks associated with the Vacuum and Vent
servo valves.

Multiplier Enables you to increase the speed for the Vacuum and Vent servo
valve. Decrease the value(s) to improve the servo precision.

Constants Fixed values used for the servo algorithm; they cannot be
changed.

Delay after pulse Lapse between each pulse when using the servo valves.

Pulse minimum Minimum amount of time the servo valve is to remain open
during a pulse.

Gas multipliers The values used to control the servo valve based on the gas in the
system.

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Configure Hardware HPVAII Series Operator’s Manual

Cryostat configured Selected when using a cryostat during analysis; the fields are
enabled.

Port
Lists the serial port used to connect the cryostat controller to
the computer.

Bit rate
The speed of the connection between the cryostat controller
and the computer (default 9600 bits/sec).

Control
The type of control used by the cryostat to maintain
temperature (PID or PID Table); refer to the cryostat manual
for more information.

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HPVAII Series Operator’s Manual Configure Hardware

Dosing Tab

Dosing Mode Select one of three dosing modes from the drop-down list:

Standard
The sample is dosed to the pressure points listed in the Step
Isotherm Define window without evacuating the sample tube
between points.

Cycle
The manifold is dosed to the pressure points listed in the Step
Isotherm Define window and vents the sample after each
pressure point.

Selective Adsorption
The manifold is dosed to the pressure points listed in the System
Step Isotherm window and evacuates the sample tube between
points and triggers an external device to collect said evacuated
gas for composition analysis.

Vent/Vacuum  Enter a Threshold pressure at which the system is to use the Vent
servo valve to reach specified pressures. The system uses the
Vacuum servo for any pressures attained below the specified
pressure.

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Configure Hardware HPVAII Series Operator’s Manual

Vent Line Flush Flush if below

If any dose pressure in the isotherm analysis is below the value you
enter here, the vent line is flushed with the analysis gas before
pressurizing the manifold to the dose pressure. This prevents
contamination of the manifold during venting at near-ambient
pressures.

Fill time
The amount of time the system is to fill the manifold with the
analysis gas before the vent line flush.

Vent time
The amount of time to flush the analysis gas through the vent line.

Cycle Mode The option in this group box is enabled when you choose Cycle
dosing.

The length of time the vent should remain open after each
pressure step.

Selective Adsorption Evac time

Mode The length of time the sample tube is to be evacuated between
pressure points.

Sampling pressure
Enter the pressure to which the manifold is to be vented after
equilibration before triggering the external device to collect data.

Trigger
Enter the length of time the trigger signal is to be sent to the
external device and the voltage at which it is to be transmitted.

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HPVAII Series Operator’s Manual Configure Hardware

Adsorption Tab

Pressure Tolerance The options in this group box allow you to specify pressure
tolerance details.

Threshold
Enter a pressure for the threshold. The pressure at which the dose
pressure tolerance below (this value) is different from the pressure
tolerance above (this value).

Above threshold
The manifold dose pressure must be within + of the value you enter
here for the system to continue during dosing.

Below threshold
The manifold dose pressure must be within + of the value enter
here for the system to continue during dosing.

Temperature Enter a value for the temperature tolerance. The sample

temperature must be within + of this value to be considered at the
target temperature.

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Configure Hardware HPVAII Series Operator’s Manual

Helium Flush The system cycles helium through the manifold and sample tube
five times after the last experiment to allow safe removal of the
sample.

Vent pressure
After pressurization with helium, the sample tube and manifold are
vented to this pressure.

He fill pressure
The pressure at which the helium is dosed to the manifold prior to
venting.

Vent time
The length of time for the vent remain open after the fifth helium
fill/vent cycle.

Vent Expand Vent pressure

During the adsorption experiment, the system is considered vented
if at or below the pressure you specify in this field.

Expand time
The amount of time for the system to wait after dosing from the
manifold to the sample before monitoring pressure equilibration.

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HPVAII Series Operator’s Manual Configure Hardware

Free Space Tab

Dose Allows you to specify dosing options for the free space.

Pressure
This is the pressure at which the manifold is dosed to before the
free-space analysis. The recommended value is 0.8 bar.

Tolerance
Enter a tolerance for the dosing pressure. The dosing pressure for
the free-space analysis must be within + of the value you enter
here.

Max equil var

The system is considered at equilibrium if the pressure does not
vary (during a one-minute period) by more than the value you enter
here.

Max equil time

Enter the maximum length of time to allow for equilibration during
the free-space analysis.

Temperature Enter a tolerance for the ambient and analysis temperatures during
the free-space analysis ( + this value).

Mar 2013 4-21

Help HPVAII Series Operator’s Manual

Evac Expand Enter the length of time for the sample tube to evacuate before the
free-space analysis.

Evac time
The amount of time the system will evacuate the sample tube prior
to the free space analysis.

Expand time
The amount of time for the system to wait after dosing from the
manifold to the sample before monitoring pressure equilibration.

Help
This option displays the HPVAII operator’s manual. Use the Bookmarks, Table of Contents, and
Index to locate the information you need. The experiment dialogs also contain a Help button
from which you can access the operator’s manual.

Exit
Closes the HPVAII program.

4-22 Mar 2013

 5. EXPERIMENT RESULTS

Experiment data are viewed using the Microsoft Excel Macro that was installed during installa-
tion of the HPVAII. The macro is used to:

• Calculate free-space data for both the ambient volume and the analysis temperature vol-
ume

• Calculate the volume of gas adsorbed during an experiment

• Display data isotherms

• Calculate BET surface area, Langmuir surface area, and total pore volume (low pressure)
using the volume of gas adsorbed during an experiment

• Display the raw data collected by the HPVAII program during an experiment

• Copy and paste data into other programs such as Microsoft Word or to save data in a vari-
ety of formats using Excel features

Running the Macro

The following features must be selected in Excel to use the Macro:

• When prompted by Excel, select Enable Macros.

• Make sure the Macro Security (Excel Options window) is set to Medium or lower.

The Macro worksheet contains three tabs across the bottom and defaults to the contents of the
Parameters tab:

• Parameters
• Gases
• ReadMe

Mar 2013 5-1

Running the Macro HPVAII Series Operator’s Manual

Parameters Tab

The Parameters tab displays the parameters used in calculations.

You can adjust the parameters if required. The settings are described in the following table.

Isotherm Report Calculates the volume of gas adsorbed during an analysis and
generates a spreadsheet with the data. Automatically plots isotherms
and weight percentage uptake plots as well as other calculations
selected from the “parameters” page.

Free Space Report Calculates the free-space data for both the ambient volume and the
analysis temperature volume, and generates a spreadsheet with the
data used for the calculations.

Long Data Report Lists raw temperature and pressure data collected throughout an
experiment and automatically plots these data versus time.

Surface Area Options Psat

Enter the saturation pressure of the adsorbate at the analysis
temperature in millibar.

5-2 Mar 2013

HPVAII Series Operator’s Manual Running the Macro

Surface Area Options BET Surface Area Report

Calculates the BET surface area of the sample from the data listed
(continued) within the entered relative pressure range (typically 0.05 to 0.30 P/
Po).

Langmuir Surface Area Report

Calculates the Langmuir surface area of the sample from the data
listed within the entered relative pressure range.

Total Pore Volume Report

Calculates the total pore volume of the sample at the relative
pressure from the analysis that is closest to, but not greater than, the
entered value.

Hardware Options Selective Adsorption

Select this option if the analysis was conducted using the Selective
Adsorption dosing routine. This accounts for the evacuation of the
sample cell after each adsorption/desorption point during the
selective adsorption routine when performing calculations.

Cryostat Temperature Correction

Select this option if a ColdEdge cryostat was used for temperature
control of the analysis. When the ColdEdge cryostat is used, the
instrument reads the sample temperature from the control box of the
cryostat. The control box reads the temperature from a temperature
probe within the sample well of the cryostat. The reading of this
temperature probe is approximately 1 °C less than the true
temperature within the sample cell. This correction adds 1 °C to all
sample temperature readings prior to all calculations.

High Pressure Options This group box allows you to specify high-pressure options.

Set Baseline Use this option if you wish to subtract “blank” error from the sample
analysis using one of two methods. When selected and an Isotherm
Report is generated, you are prompted to:

• Select the analysis sample file

• Enter the dry mass of the sample
• Select the blank tube analysis sample file

Mar 2013 5-3

Running the Macro HPVAII Series Operator’s Manual

Point by Point Use this option only when the blank analysis was performed at the
same analysis temperature, with the same analysis gas, and used the
same number of pressure steps as the sample analysis. When
calculating the sample isotherm, the blank error at each point is
subtracted from the original volume adsorbed value. Recommended
for CO2 analyses.

Linear The slopes and intercepts of the lines of best fit for both the
Approximation adsorption and desorption data from the blank analysis are
calculated. The system corrects the sample analysis file by
subtracting the error at each pressure calculated from the slope and
intercept. This correction should only be used if the blank sample
tube analysis was performed at the same temperature, in the same
pressure range, and with the same analysis gas as the sample
analysis.

Fit Langmuir The shape of most high-pressure isotherms typically resemble Type
Equation 1 isotherms. The Langmuir equation can be used to model Type 1
isotherms. Select this option to generate a report that provides the
Langmuir coefficients used to model the data.

Free Space The options in this group box allow you to specify free-space criteria
for isotherm reports.

Measured The free space is calculated using the values collected during the
experiment.

Entered The entered Ambient and Analysis free-space values are used for
calculating adsorption data.

Density Correction The system uses the free-space values entered prior to the
experiment in the analysis set-up for isotherm calculations. When the
isotherm report is generated, you are prompted to enter the density of
the sample after you enter the dry mass for the sample. This
information is used to calculate the physical volume of the sample
and subtract it from the entered free-space values. Recommended for
cryogenic analyses of microporous materials (refer to CRYOGENIC
ANALYSIS, page B-1).

Equations of State Allows you to select the desired equation of state for each adsorbate
used to generate the compressibility factors of the high-pressure
gases. More information on the equations of state can be found in the
accompanying NIST REFPROP software

5-4 Mar 2013

HPVAII Series Operator’s Manual Running the Macro

Gases Tab

The Gases Tab displays the gas properties used in calculations. Use the side scroll bar to view all
gases.

Adsorbate The name of the adsorbate and its symbol are listed so the macro will
recognize the adsorbate, whether its name or its symbol was entered
in the Step Isotherm Define Run window prior to the experiment.

Pc(bar) The critical pressure expressed in bar.

Tc(K) The critical temperature expressed in Kelvin.

X Sec Area (nm2) The cross-sectional area of the adsorbate molecules in square
nanometers.

NistName The National Institute of Standards name of the adsorbate. This is the
name the REFPROP software recognizes when called for
compressibility data.

Molecular Weight The molecular weight of the adsorbate.

Density Conversion  Factor used to calculate total pore volume at a relative pressure of
Factor 0.95 or greater.

Mar 2013 5-5

Compile Error Message HPVAII Series Operator’s Manual

Read Me Tab

The ReadMe tab displays information about the HPVAII Macro. Use the scroll bars to view the
contents.

Compile Error Message

Occasionally, you may see the following message display when trying to open a file:

Compile Error: Can't find project or library.

If this occurs, perform the following steps to clear the error.

1. Open the Excel macro workbook.

2. Press Alt + F11 to open the Visual Basic Editor.

3. Click Tools > References to display the References dialog.

4. Clear the check box for the type library or object library marked as Missing - this should be
SOLVER.XLS

5-6 Mar 2013

HPVAII Series Operator’s Manual Displaying Experiment Data

Displaying Experiment Data

Experiment data are displayed in the following three formats:

• Isotherm Report
• Free Space Report
• Long Data Report

Isotherm Report

The Isotherm Report displays the Volume Adsorbed isotherm and Weight Percentage plot, as
well as information about the experiment and calculations. When the graphs are displayed, you
can use Excel charting functions to change curve colors, add symbols, modify the legend, etc.
You can also use Excel functions such as Cut, Copy, and Save As to transfer data to other pro-
grams. Refer to your Excel documentation for more information.

1. Select Isotherm Report from the Parameters tab; the Open dialog is displayed.

2. Navigate to your data directory and select the desired file (file extensions are HIsh), then
click Open; the Dry Weight dialog is displayed.

3. Enter the mass of the sample after analysis in grams, then click OK; a spreadsheet similar to
the following and a Save As dialog are displayed.

Mar 2013 5-7

Displaying Experiment Data HPVAII Series Operator’s Manual

This spreadsheet contains a list of the Experiment data, and the volume dosed and volume
adsorbed calculations. If you would like to save the data in an Excel spreadsheet, enter a file
name, then click Save. If you do not wish to save the data, click Cancel to close the dialog
and display the contents of the Run tab window. Use the scroll bars to view all data.

The columns in the calculation tables are described below.

Column Heading Description

Volume Dosed
ReqPm Requested pressure by the user
PmA Pressure of manifold before dosing
TmA Temperature of manifold before dosing
ZA Compressibility of adsorbate at PmA and TmA
Vol A Volume of adsorbate in manifold before dosing
PmB Pressure of manifold after dosing
TmB Temperature of manifold after dosing
ZB Compressibility of adsorbate at PmB and TmB
Vol B Volume of adsorbate in manifold after dosing
Vol Dosed Volume of adsorbate dosed to sample this step
Total Dosed Total volume of adsorbate dosed to sample

5-8 Mar 2013

HPVAII Series Operator’s Manual Displaying Experiment Data

Column Heading Description

Volume Adsorbed
Ps Pressure of sample after dosing
Ts Temperature of sample after dosing
ZS Compressibility of adsorbate at Ps and Ts
Vs NAds Volume of adsorbate in sample cylinder after dosing
ZXL Compressibility of adsorbate at Ps and ambient temperature
Vxl NAds Volume of adsorbate in lower stem after dosing
ZXU Compressibility of adsorbate at Ps and TmB
Vxu NAds Volume of adsorbate in upper stem after dosing
Vol NAds Total volume of adsorbate below value 1 after dosing
Vol Ads Volume adsorbed by sample
Vol Ads/g Volume adsorbed by sample/sample mass
wt% Percentage of sample weight that is adsorbate

4. Click the Isotherm tab to display an isotherm of the experiment data. An example is shown
below.

Mar 2013 5-9

Displaying Experiment Data HPVAII Series Operator’s Manual

5. Click the PCT tab to display a weight percentage plot of the experiment. An example is
shown below.

5-10 Mar 2013

HPVAII Series Operator’s Manual Displaying Experiment Data

Free Space Report

The Free Space Report displays information about the free space analysis and calculations. You
can also use Excel functions such as Cut, Copy, and Save As to transfer data to other programs.
Refer to your Excel documentation for more information.

1. Select Free Space Report from the Parameters tab; the Open dialog is displayed. Free
Space reports have the same name as the experiment file with an HIHe extension

2. Select the desired HIHe file and click Open. The free-space data for the experiment and a
Save As dialog are displayed.

3. Enter a file name if you wish to save the data as an Excel file, or click Cancel to close the
Save As dialog to view the free-space data.

The columns in the calculation tables are the same as those in the Isotherm report, refer to
page 5-8 for an explanation.

Mar 2013 5-11

Displaying Experiment Data HPVAII Series Operator’s Manual

Long Data Report

The Long Data report displays the raw data from the experiment.

1. Select Long Data Report from the Parameters tab; the Open dialog is displayed. Long Data
reports have the same name as the experiment file with an HIlo extension.

2. Select the desired HIlo file and click Open. The raw data for the experiment and a Save As
dialog are displayed.

3. Enter a file name if you wish to save the data as an Excel file, or click Cancel to close the
Save As dialog to view the raw data.

4. Sample statistics are displayed in the upper portion of the report, followed by a table of the
collected data. The data are also plotted in subsequent tabs of the generated spreadsheet.

Column Heading Description

Elap Time min Elapsed time in the experiment
HP bar High-pressure transducer reading
LP bar Low-pressure (1000 torr) transducer reading
Tm deg C Manifold temperature
Ts deg C Sample temperature
Vac mbar Vacuum reading

5-12 Mar 2013

 6. TROUBLESHOOTING AND MAINTENANCE

The HPVAII system has been designed to provide efficient and continuous service. However, cer-
tain maintenance procedures should be followed to obtain the best results over the longest period
of time. This chapter includes troubleshooting and maintenance procedures.

Troubleshooting
Most operational problems are caused by:

• Leaks (commonly around the sample tube O-ring at the analysis port)
• Sample weighing errors
• Impure gas supply

Always check the items listed below first when expected experiment results are not obtained.
Some common operational problems, which are not indicated on the video monitor screen, and
their respective causes and solutions are provided in the following table.

What Happened Why What To Do

Vacuum error, such as Vacuum pump hose leaking The vacuum pump hose uses
vacuum gauge cannot around an O-ring. two O-rings:
reach lower limit
• One on the hose/instrument
connection on the rear panel
of the instrument

• One on the hose/vacuum

pump connection

These O-rings must be properly

greased and must not be worn or
cracked.

Check the O-rings and grease or

replace as necessary.
Vent valves 2 and 4 are open, Close both valves, flush with
allowing ambient air to be helium, then vacuum.
ingested.
Lower adsorption than Contaminated gas lines. Place gas bottles close to the
expected analyzer. Using gas line
extenders on gas bottles located
in remote areas may degrade gas
quality and reduce pressure.

Mar 2013 6-1

Troubleshooting HPVAII Series Operator’s Manual

What Happened Why What To Do

Instrument shuts off Hydrogen sensor has been Clear the hydrocarbon source,
unexpectedly triggered, indicating that there is then turn the instrument back
a hydrogen leak in the on.
instrument. May also be
triggered by other hydrocarbon
sources in the lab.
Valves will not operate Gas bottle depleted. Replace the gas bottle. Refer to
Connecting a Replacement Gas
Bottle, page 6-5.
For nitrogen or compressed air, Check the pressure and ensure
the pressure on the gas line is that pressure reading is at least
less than 75 psi. 75 psi.
When the system is The transducers may need to be Call your service representative.
under vacuum, a value zeroed.
of 0 is not shown in the
pressure display.
Inaccurate temperature RTD’s may need to be Call your service representative.
reading shown in one recalibrated.
of the temperature
displays
Target pressure not Gas level in tank is too low. Replace the gas bottle.
reached
Refer to Connecting a
Replacement Gas Bottle, page
6-5.
The pressure limit entered in the Enter the correct pressure limit.
Instrument Configuration
window does not match the Refer to Resetting the Pressure
pressure set on the regulator. For Limit, page 6-3.
example, if you are using CO2
or methane, the pressure limit
must be set below the maximum
output of the regulator.
Degas or analysis not O-rings in ports are missing, Replace the port O-ring.
progressing as it should worn, or damaged.
Refer to Replacing Degas and
Analysis Port O-Rings, page 6-
3.

6-2 Mar 2013

HPVAII Series Operator’s Manual Troubleshooting

Resetting the Pressure Limit

1. Select Configure Hardware from the HPVAII main menu.

2. Make sure the Instrument tab is selected.

3. Enter the maximum pressure for the gas you are using in the Pressure limit field.

4. Click Save.

Replacing Degas and Analysis Port O-Rings

The degas and analysis ports contain an O-ring that must be present when degassing or analyzing a
sample. Ensure that the O-ring is present before performing either procedure.

If an O-ring becomes worn or damaged, it should be replaced. A damaged O-ring may cause leaks
at the port, and inaccurate results.

O-ring

Mar 2013 6-3

Connecting Gases HPVAII Series Operator’s Manual

Connecting Gases

Guidelines for Connecting Gases

Use these guidelines when installing regulators and gas lines:

• Place gas bottles close to the analyzer. Using gas line extenders on gas bottles located in
remote areas may degrade gas quality and reduce pressure.

• Use a retaining strap (or other appropriate tether) to secure the gas bottle.

• Carefully route the gas lines from the bottle to the analyzer; avoid overlapping or entangl-
ing lines.

• Label the gas line at the instrument inlet for proper identification and maintenance.

• Ensure that the gas bottle is closed before connecting to the analyzer.

The following instructions describe a typical installation. Some configurations require additional
components, such as regulator expansion kits, when one gas source will be used for several
operations or when the gas bottle cannot be located close to the analyzer.

Disconnecting the Depleted Bottle

1. Close the gas bottle shut-off valve, then open the regulator shut-off valve.

Gas Bottle
shut-off valve

Regulator
shut-off
valve

2. The HPVA II high-pressure gauge should read at or near one bar with the supply valve (6, 7,
or 8) open. If not, open Valve 3 (gas inlet) and Valves 2 and 4 (vent) and allow the pressure to
purge from the lines. Then close all valves.

6-4 Mar 2013

HPVAII Series Operator’s Manual Connecting Gases

3. Use an appropriate wrench to loosen the nut at the regulator/gas bottle connection, then
remove the regulator from the bottle.

There are right- and left-handed connections. Be sure you are loosening in
the correct direction. Left-handed connections are indicated if the nut
contains a groove.

You do not have to disconnect the gas line from the regulator or the instrument.

4. Replace the protective cap on the depleted bottle, disconnect the retaining strap, and remove
the bottle from its current location.

Connecting a Replacement Gas Bottle

Move the replacement bottle close to the instrument and tether it into place.

When connecting hazardous gases, be sure to vent properly and follow the
safety procedures established for your lab.

1. Use an appropriate cylinder wrench to remove the protective cap from the replacement bottle.

Mar 2013 6-5

Connecting Gases HPVAII Series Operator’s Manual

2. Attach the gas regulator to the connector on the gas bottle. Hand-tighten the nut, then use an
appropriate wrench to tighten an additional 3/4 turn.

Do not overtighten the fitting; doing so may cause a leak.

3. If you disconnected the gas line from the regulator, reconnect it now.

4. Check for leaks at the high-pressure side of the regulator and in the connector.

HIgh-pressure Gauge

Regulator
shut-off Gas Bottle
valve shut-off valve

Regulator
control knob
Regulator
connector nut

a. Turn the regulator control knob fully counterclockwise.

b. Be sure the regulator shut-off valve is fully closed.

c. Slowly open the gas bottle shut-off valve, then close it.

d. Apply leak-detector fluid at the connection. If bubbles form, tighten the regulator
connector nut.

5. If you disconnected the gas line to the instrument inlet, reconnect it now.

6-6 Mar 2013

HPVAII Series Operator’s Manual Connecting Gases

6. Set the instrument pressure.

Low-pressure gauge

Regulator Gas Bottle

Shut-Off valve Shut-Off valve

Regulator
Control knob

a. Be sure the Regulator shut-off valve is closed.

b. Open the Gas bottle shut-off valve.

c. Use the Regulator Control knob to set the desired pressure. A pressure of 15 bar or less is
recommended for initial leak testing and gas flow.

d. Open the Regulator shut-off valve to allow pressure to flow to the instrument.

e. Close the Gas bottle shut-off valve.

f. Using the Manual Control window, open Valve 3 to allow the pressure to be read on the
screen.

1.000

1000.00

35.00

25.00

Mar 2013 6-7

Connecting Gases HPVAII Series Operator’s Manual

g. Open the appropriate gas inlet valve for the gas being replaced. You should see an increase
in pressure indicating the valve is open and gas is flowing into the manifold.

h. Open Valves 2 and 4 to allow the gas to vent.

i. Close Valve 4 and observe the pressure increase. If the pressure is increasing slowly, you
may want to open the applicable metering valve to allow a more rapid flow for flushing
the lines.

j. Allow the pressure to reach 15 bar, then open Valve 4 and allow the pressure to vent to
atmosphere.

k. Repeat this pressure build and vent process nine more times to ensure only pure gas is
being flowed through the system.

l. Using the Manual Control windos, close all valves.

7. Ensure that the gas pressure is set to the following:

Analysis gas 1500 psi (103 bar) for an HPVAII-100

3000 psi (206 bar) for an HPVAII-200
Helium gas 20 psi (1.37 bar)
Compressed air 75 to 80 psi (5.2 to 5.5 bar)

8. Adjust the gas metering valve (page 6-9) for proper gas inlet flow.

6-8 Mar 2013

HPVAII Series Operator’s Manual Adjusting the Metering Valves

Adjusting the Metering Valves

The metering valves control the pressure of the gas flow into the unit. It is very
important that they are set correctly to ensure proper dosing without
overshooting pressure points as well as to conserve gas.

There are three metering valves inside the instrument; one for each gas line. When you change
gases or need to adjust the flow of a gas follow these procedures.

1. Remove the rear panel from the instrument.

2. The metering valves are located on the lower right side of the instrument.

The valves are, from let to right, Gas 1, Gas 2, and Gas 3 (Helium).

Fully close the metering valve for the appropriate gas line.

3. Select Manual Control from the HPVAII main menu.

Mar 2013 6-9

Adjusting the Metering Valves HPVAII Series Operator’s Manual

4. Make sure all the shut-off valves shown in the schematic are closed.

1.000

1000.00

35.00

25.00

5. Turn on the gas at the gas bottle.

6. Using the Manual Control screen, open valve 3 so that pressure can be read.

1.000

1000.00

35.00

25.00

6-10 Mar 2013

HPVAII Series Operator’s Manual Adjusting the Metering Valves

7. Open the gas line valve, for example, valve 6 for Gas Line 1.

2.133

1000.00

35.00

25.00

8. Slightly open the metering valve.

9. Observe the Manifold pressure (HP) shown on the Manual Control screen. The pressure
should rise approximately 1 bar every 3 to 5 seconds.

10. Adjust the metering valve as necessary to obtain the appropriate gas flow.

11. Close the valves on the Manual Control screen, then open valves 2 and 4 to vent.

1.000

1000.00

35.00

25.00

Mar 2013 6-11

Adjusting the Metering Valves HPVAII Series Operator’s Manual

12. To recheck the pressure:

a. Close valves 2 and 4.

b. Open valve 3 and observe the pressure as you open the gas valve (valve 6 in our example).
There should be an initial rapid increase followed by a steady pressure increase.

2.133

1000.00

35.00

25.00

13. After observing a steady pressure increase, close valve 6.

14. Open valves 2 and 4 to vent.

15. After venting, close the Manual Control screen.

6-12 Mar 2013

 7. ORDERING INFORMATION

Use one of the following methods to order components for the HPVAII Series analyzers:

• Call Customer Service at (770) 662-3636

• Contact your local sales representative

When ordering, please use the information provided below to place your order.

Part Number Item and Description

P02-25805-00 Gas inlet line, stainless steel, 8 ft.
P02-31701-00 Furnace insulator top, half
003-51123-00 Fuse, 6.25 Amp, 3AG, Slow Blow
003-51134-01 Fuse, 5.0 Amp, 5x20 mm, Slow Blow
004-25040-01 Gasket, 1/4 in., stainless steel, silver plated; for sample cylinder
004-27056-01 Filtered gasket, 60 micron; for sample cylinder when fine powders used
P02-25821-00 Sample cylinder, 2 cc
P02-25827-00 Sample cylinder, 10 cc
P02-25846-00 Sample tube funnel
004-25466-02 O-ring -010 60 Duro Viton F, for degas or analysis port
P02-25820-00 Sample isolation valve
P02-25823-00 Sample tube stem, used with sample isolation valve
P02-33012-00 Cryogenic Kit, includes Dewar and accessories
P02-34013-00 Sample Chamber Assembly, 0.75 cc
004-16847-00 Reference Material, 5A Zeolite, high pressure

Mar 2013 7-1

 A. ERROR MESSAGES

This appendix contains the error messages that may be encountered while operating the HPVAII
Series instruments and using the Excel macro; they are listed in alphabetical order.

Compile Error: Can’t find project or library.

Cause: Excel was unable to locate the requested project library.

Action: Refer to Compile Error Message, page 5-6 for instructions.

Error (number) while preparing to write (path-to-ini-file)

Cause: The application initialization file is missing from the HPVAII System
applications directory.

Action: Verify that all HPVAII System applications and the HPVASys.ini file
are in the same directory.

Instrument .ini file could not be found: (path-to-ini-file)

Cause: The application initialization file is missing from the HPVAII System
applications directory.

Action: Verify that all HPVAII System applications and the HPVASys.ini file
are in the same directory.

One or more hardware errors were found. Unable to continue.

Cause: Initialization of the National Instruments data acquisition device failed.

Action A: Verify proper installation of the HPVAII software and that no

additional updates from National Instruments have been installed.

Action B: Verify that the USB device and external cables are properly connected
and powered on.

Mar 2013 A-1

Appendix A HPVAII Series Operator’s Manual

Trigger output voltage (V) is out of range. Trigger will not be set.

Cause: While in the selective adsorption dosing mode, the requested trigger
signal voltage was over 10 volts or under -10 volts.

Action: Verify that the selective adsorption trigger voltage is within the range
of +10 to -10 volts.

Trigger signal is not ready.

Cause: While in the selective adsorption dosing mode, the trigger signal to the
external analytical instrument (GC or mass spec) could not be enabled.

Action A: Verify that the selective adsorption dosing mode was properly selected.

Action B: Verify proper installation of the HPVAII software and that no additional
updates from National Instruments have been installed.

Action C: Verify that the board and external cables are properly connected.

Unable to load UI.

Cause: The application initialization failed to load due to unavailable resources.

Action: Verify that there is available free memory on the computer to run the
HPVAII software.

Unable to open instrument log <(path-to-log)>

Cause: The instrument log file failed to open.

Action: Verify that you have write permissions to the directory specified for your
data files.

A-2 Mar 2013

HPVAII Series Operator’s Manual Appendix A

Unable to open template file.

Cause: The selected template file has been corrupted or is not a proper template
file.

Action: Select another template file for analysis.

Unable to read info from .ini file

Cause: The application initialization file is missing from the HPVAII System
applications directory.

Action: Verify that all HPVAII System applications and the HPVASys.ini file are in
the same directory.

Unable to write calibration file (file name)

Cause: Writing of the calibration file failed.

Action A: Verify that there is available disk space to write the calibration file.

Action B: Verify that all HPVAII System applications and calibration file are in the
same directory.

Action C: Verify that you have write permissions to the directory in which the
HPVAII System applications are installed.

Unable to write template file to the data directory: (file path)

Cause: The template file failed to write to the specified data directory.

Action A: Verify that there is available disk space to write the template file.

Action B: Verify that you have write permissions to the specified data directory.

Mar 2013 A-3

Appendix A HPVAII Series Operator’s Manual

Unable to write the .ini file (path-to-ini-file)

Cause: Writing of the application initialization file failed.

Action A: Verify that there is available disk space to write the application
initialization file.

Action B: Verify that all HPVAII system applications and the HPVASys.ini file are in
the same directory.

Action C: Verify that you have write permissions to the directory in which the
HPVAII System applications are installed.

You must enter a valid Expt ID before you can run. (list of unavailable characters)

Cause: You entered an Experiment ID containing invalid characters.

Action: Use an alternate experiment ID.

You must enter an Expt ID before you can run.

Cause: The Experiment ID is blank.

Action: Enter a valid Experiment ID before continuing.

You need to define at least one run.

Cause: You attempted to proceed with an isotherm experiment with no defined

experimental runs.

Action: Define the conditions for at least one experimental run before continuing.

A-4 Mar 2013

 B. CRYOGENIC ANALYSIS

This appendix contains instructions for performing an analysis with the optional Cryogenic Kit,
available from Particulate Systems.

Due to helium interaction with microporous samples at cryogenic temperatures, it can be difficult
to find the true analysis free space of the sample tube with the sample present. Therefore, we rec-
ommend that you first find the ambient and analysis free-space volumes of the empty sample tube
to be used in the analysis. After you perform the free-space routine, you can then place the sample
into the sample tube and prepare it for analysis. The HPVAII software allows you to enter the
ambient and analysis free-space values previously found prior to the adsorption/desorption
routine.

When the volumetric calculations are performed by the HPVAII Excel macro, the mass and density
of the sample are used to find the sample’s physical volume. This volume is subtracted from the
ambient and analysis free-space values originally entered into the HPVAII software. This corrects
the blank sample tube free-space values for the volume of the sample and provides accurate vol-
umes to be used for the isotherm calculations.

Mar 2013 B-1

Measuring Free Space HPVAII Series Operator’s Manual

Measuring Free Space

Performing a Blank Tube Experiment

1. Clean and dry the sample cylinder (refer to Cleaning the Sample Cylinder, page 3-2).

2. Assemble the sample holder (refer to Assembling the Sample Holder, page 3-5).

3. Place an isothermal jacket on the stem of the sample holder.

4. Place the dewar stand and empty dewar under the analysis port, then plug in the temperature
probe.

5. Ensure that the O-ring is in place in the analysis port.

O-ring

B-2 Mar 2013

HPVAII Series Operator’s Manual Measuring Free Space

6. Tilt the dewar and insert the sample holder.

7. Attach the sample holder to the sample port and hand-tighten the connector nut.

8. Using the 3/4-in. and 5/8-in. wrenches, tighten the nut just until snug.

Do not over-tighten the connector nut, doing so could damage the port
fitting.

Mar 2013 B-3

Measuring Free Space HPVAII Series Operator’s Manual

9. Select the Adsorption option from the HPVAII main menu; the Experiment Definition: New
window is displayed.

10. Enter information in the fields of this window (refer to Experiment Definition New, page 4-
2).

It is important to set the Sample Weight to 1 (or a value greater than 0) or

the analysis will not be able to start.

B-4 Mar 2013

HPVAII Series Operator’s Manual Measuring Free Space

11. Click Add to enter the analysis conditions for the free-space measurement; the Step Isotherm
Define Run window is displayed.

12. Select the External Temperature Control Method option.

13. Enter the Experiment and Ambient temperatures.

14. Set the Experiment Hold time to about 60 minutes, but no less than 45 minutes. This is
necessary because when the warm sample tube is submerged into a liquid cryogen bath, it
takes at least 45 minutes for the sample tube to equilibrate and create a stable temperature
within the tube.

15. Click OK to return to the Experiment Definition: New window.

16. Open the sample isolation valve on the sample tube.

17. Click Run Experiment; the software determines the ambient temperature free-space volume.
When this step is complete, you are prompted to make the temperature change.

Mar 2013 B-5

Measuring Free Space HPVAII Series Operator’s Manual

18. Fill the dewar with liquid nitrogen to the top of the isothermal jacket.

19. Place the dewar cover on top of the dewar.

20. Place the strap around the dewar cover and tighten.

21. Insert the temperature probe into the dewar.

B-6 Mar 2013

HPVAII Series Operator’s Manual Measuring Free Space

22. Click OK.

Do not remove the sample tube from the analysis port between the
ambient temperature volume analysis and the analysis temperature
volume analysis. Doing so will cause the free space analysis to be
compromised.

23. When the analysis is complete, the results can be viewed using the Excel HPVII macro as
described in the next topic.

Displaying the Free Space

1. Open the Excel Macro.

2. Select Free Space Report from the Parameters tab.

3. Select the helium data file created during the free-space analysis. A report, which includes
Ambient Free Space and Analysis Free Space (measured in cc STP) is displayed. Below is an
example, with the free space volumes highlighted.

4. The free-space volumes of the sample tube can be used for future adsorption/desorption
analyses as long as the analysis temperature does not change. We recommend that you record
these volumes for future use.

Mar 2013 B-7

Preparing the Sample HPVAII Series Operator’s Manual

Preparing the Sample

1. Remove the sample holder from the analysis port.

2. Allow the sample holder to return to room temperature.

3. Remove the isothermal jacket.

4. Remove any condensation that formed on the exterior of the sample holder.

5. Disassemble the sample holder.

6. Weigh the sample (refer to Weighing the Sample, page 3-4).

7. Re-assemble the sample holder. (Refer to Assembling the Sample Holder, page 3-5).

8. Degas the sample to remove any moisture or CO2 from the sample (refer to Degassing the
Sample, page 3-6).

Make sure the isothermal jacket is removed from the sample holder before
degassing the sample. The isothermal jacket cannot withstand the heat
during the degas process.

9. When the degas is complete, close the Sample isolation valve on the sample holder.

10. Cool the sample holder to room temperature.

B-8 Mar 2013

HPVAII Series Operator’s Manual Performing the Adsorption/Desorption Analysis

Performing the Adsorption/Desorption Analysis

1. Place the isothermal jacket on the sample tube.

2. Place the dewar stand and empty dewar under the analysis port, then plug in the temperature
probe.

3. Ensure that the O-ring is in place in the analysis port.

O-ring

4. Tilt the dewar and insert the sample holder.

Mar 2013 B-9

Performing the Adsorption/Desorption Analysis HPVAII Series Operator’s Manual

5. Attach the sample holder to the sample port and hand-tighten the connector nut.

6. Using the 3/4- and 5/8-in. wrenches, tighten the nut just until snug.

Do not overtighten the connector nut. Doing so could damage the port
fitting.

B-10 Mar 2013

HPVAII Series Operator’s Manual Performing the Adsorption/Desorption Analysis

7. Select the Adsorption option from the HPVAII main menu; the Experiment Definition: New
window is displayed.

8. Enter information in the fields in this window (refer to Experiment Definition New, page 4-
2).

9. Click Add to display the Define Run window.

Mar 2013 B-11

Performing the Adsorption/Desorption Analysis HPVAII Series Operator’s Manual

10. Select the External Temperature Control Method option.

11. Enter the pressure steps that are desired for the sample to reach during analysis:

a. Enter or select a pressure in the Pressure field.

b. Click Add to add the pressure to the table.

12. Enter temperature settings similar to those used for the free-space analysis.

13. Deselect the Measure FS option.

14. Enter the ambient free space from the free-space analysis in the Ambient FS field.

15. Enter the experiment free space from the free-space analysis in the Exper FS field.

16. Set the Hold time to about 60 minutes, but no less than 45 minutes. This is necessary because
when the warm sample tube is submerged into a liquid cryogen bath, it takes at least 45
minutes for the sample tube to equilibrate and create a stable temperature within the tube.

17. Click OK to return to the Experiment Definition New window.

18. Open the sample isolation valve on the sample tube.

19. Click Run Experiment; you are prompted to bring the sample tube to the desired analysis
temperature.

20. Fill the dewar with liquid nitrogen to the top of the isothermal jacket,

B-12 Mar 2013

HPVAII Series Operator’s Manual Performing the Adsorption/Desorption Analysis

21. Place the dewar cover on top of the dewar.

22. Place the strap around the dewar cover and tighten.

23. Insert the temperature probe into the dewar.

24. Click OK.

• Once the system has reached the desired temperature and the hold time has elapsed, the
HPVAII will begin the analysis.

• When the analysis is complete, the results can be viewed in the Excel HPVAII macro as
described in the next topic, Viewing the Results, page B-14.

25. After the analysis has completed, close the sample isolation valve.

Mar 2013 B-13

Viewing the Results HPVAII Series Operator’s Manual

26. Remove the sample from the analysis port and allow it to warm to room temperature.

27. The sample container can then be removed from the sample holder and reweighed to find the
dry mass of the sample.

Viewing the Results

1. Open the Excel Macro.

2. Click the Parameter tab if the Parameter page is not already displayed.

3. Select the Density Correction option in the Free Space area.

4. Select Isotherm Report on the Parameter tab.

5. Select the short data file (extension HISH) from the analysis you performed, then click OK.

6. You are prompted to enter the dry mass of the sample.

Enter the mass of the sample after the analysis, then click OK.

7. You are then prompted to enter the sample density.

Enter the sample density, then click OK.

Since the macro knows the mass and density of the sample, it simply divides the sample mass
by the density to find the physical volume of the sample. This volume is subtracted from the
entered ambient and analysis temperature volumes that were entered into the HPVAII
software prior to analysis. These corrected values are used for the calculations for
constructing the volume of gas absorbed at each pressure step of the experiment.

B-14 Mar 2013

HPVAII Series Operator’s Manual Viewing the Results

8. A list of the experiment data and the Save As dialog are displayed. If you would like to save
the data in an Excel spreadsheet, enter a file name or accept the default name, then click
Save.

9. You can click the Isotherm tab to display an isotherm of the experiment data or the PCT tab
to display the weight percentage plot.

Mar 2013 B-15

 C. SOFTWARE INSTALLATION

The HPVAII software should be installed in the order given in these instructions.

1. Insert the HPVAII installation disk into a CD drive.

If an AutoPlay dialog displays, click X in the upper right-hand corner to

close it.

2. Right-click on the Start icon and open Windows Explorer. Navigate to the CD drive
containing the installation disk; double-click on the drive to open the installation CD.

The installation disk contains several folders. It is important that you install the HPVA II
system following the order in these instructions for a proper installation. Keep Windows
Explorer open (minimized when not using).

3. Double-click on HPVA 2 System Installer.

a. Double-click the Setup.exe file.

b. Select I agree to the license agreement, then click Next.

c. Click Next again, a progress dialog displays as the program is being installed. When
installation is complete, a dialog indicating so is displayed. Click Finish to close the
dialog.

d. A dialog prompting you to restart is displayed, click Restart before proceeding.

Mar 2013 C-1

Appendix C HPVAII Series Operator’s Manual

4. Maximize Windows explorer and open the HPVA Calibration folder.

a. Locate the cal(serial number) file, right-click and select Copy.

b. Navigate to the installed location on your local hard drive.

c. Right-click and select Paste.

d. Locate and open the HPVAsys.ini file.

e. Scroll down to the [Instrument] section. On the first line, delete the word DEMO (DO
NOT delete the quotes) and enter the instrument serial number; this example uses serial
number 1101.

f. Select File > Save, then close the window.

C-2 Mar 2013

HPVAII Series Operator’s Manual Appendix C

5. Open Windows Explorer and double-click the REFPRO 8 Installer folder.

a. Double-click the SETUP.EXE file; the REFPROP Install Shield Wizard is displayed.

Click Next.

b. Select I accept the terms in the license agreement and click Next.

c. Click Change and change the Folder name to C:\Program Files\NIST\REFPROP7\.

Click OK, then Next.

Mar 2013 C-3

Appendix C HPVAII Series Operator’s Manual

d. Click Install on the next screen to install REFPROP. When installed, click Finish to
close the window.

6. Maximize Windows Explorer and open the VC ++ 2008 x86 Runtime folder.

a. Double-click the VC_x86Runtime.exe file.

Some computers may display a Maintenance mode window. Click Repair,

then Next to continue.

b. Click Finish on the Setup complete dialog when it displays to close the dialog.

7. Maximize Windows Explorer and open the HPVA Macro folder.

a. Right-click on the Macro Excel file and copy to your desktop.

b. Open the Macro Excel file.

c. Depending on the security settings of Excel, you may receive some type of security
warning. If so, make sure Excel macros are enabled.

C-4 Mar 2013

HPVAII Series Operator’s Manual Index

INDEX

A sample compartment, 2-2

Control Method, 4-4
Adsorbate, 5-5
Controls, 2-1
name, entering, 4-5
Controls, front panel, 2-1
Adsorption
Conventions, used in manual, 1-2
command, 3-17
Cryogenic analysis, 5-4
tab, 4-19
performing, B-1
Advanced mode, 4-11
Cryogenic option, 7-1
Alarm reset, 2-3
Cryostat
Analog Input tab, 4-13
configuration, 4-16
Analog input tasks, 4-12
temperature correction, 5-3
Analog Output tab, 4-14
Cycle dosing mode, 4-17, 4-18
Analog output tasks, 4-12
Analysis
CO2, 5-4 D
Analysis parameter file, 2-6
Analysis port, 2-2, 3-10 Data
replacing O-ring, 6-3 collection points, 4-5
Analyzer file, 2-6
description, 1-3 Data Logging Interval, 4-5
manually controlling valves, 4-7 Define run, 4-4
models, 1-3 Degas port, 2-2
ordering parts, 7-1 attaching sample holder, 3-7
purging, 3-12 replacing O-ring, 6-3
specifications, 1-5 Degas sample, 3-6
troubleshooting, 6-1 Digital Output, 4-12
turning on and off, 2-4 Directory, changing data, 4-9
weight and dimensions, 1-5 Dose pressure, 4-5
Dosing
modes, 4-17
B pressure, free space analysis, 4-21
Dosing tab, 4-17
Bath
Dry Weight dialog, 5-7
recirculation, 4-4
temperature and voltage limits, 4-14
Bath Temperature dialog, 4-8 E
BET Surface Area report, 5-3
Blank tube experiment, B-2 Electrical specifications, 1-5
Equilibration criteria, 4-4
Equipment description, 1-3
C Error messages, 5-6, A-1
Excel macro compile error, 5-6
Calculation tables, 5-8
Evacuation time, 4-5, 4-22
Calibration command, 4-1
Excel macro, 1-4, 5-1
Cautions, defined, 1-2
Gases tab, 5-5
Change Data Directory command, 4-9
Isotherm tab, 5-9
CO2 analysis, 5-4
Parameters tab, 5-2
Computer requirements, 1-6
PCT tab, 5-10
Configure Hardware command, 4-10
Read Me tab, 5-6
Connectors
Run tab, 5-8
rear panel, 2-3

Mar 2013 Index-1

Index HPVA Series Operator’s Manual

Exit command, 4-22 Helium flush, 4-20

Experiment Helium free space data file, 2-6
blank tube, B-2 Help command, 4-22
cryogenic, B-1 Hold time, setting, 4-5
hold time, 4-5 Hover menu, 2-6
parameters, specifying, 4-2 Hydrogen gas sensor, 1-4
performing, 3-17
setting temperature, 4-5
starting, 4-3 I
viewing isotherm, 3-20 Instrument Options tab, 4-15
viewing results, 5-1 Instrument tab, 4-10
Experiment Definition New window, 4-2 Intercept, 4-13
Isolation valve, 3-9
Isotherm
F report, 5-7
Files tab, 5-9
analysis parameters, 2-6 Isotherm, displaying in Excel macro, 5-9
data, 2-6 Isotherm, displaying with software, 3-20
helium free space data, 2-6
long data, 2-6
names, 2-6 L
short data, 2-6 Langmuir equation fit, 5-4
types, 2-6 Langmuir Surface Area report, 5-3
Free space Linear calibrations, 4-13
entered, 4-6 Long data file, 2-6
measure, 4-5, 4-6 Long Data report, 5-12
report, 5-11
Free Space tab, 4-21
Front panel, 2-1 M
Furnace, 1-3 Macro Security, 5-1
connecting thermocouple, 3-6 Main menu, 2-5
control, 2-1 Maintenance, 6-1
temperature display, 2-1 replacing port O-ring, 6-3
Manifold
pressure, 4-13
G RTD, 4-13
Gas temperature, 2-1, 4-7
adsorbate, 5-5 temperature display, 2-1
connecting new bottle, 6-4 Manual Control screen, 4-7
connecting to analyzer, 6-4, 6-5 Mass, entering sample, 5-7
disconnecting bottle, 6-4 Metering valves, adjusting, 6-9
entering name of, 4-5
guidelines, 6-4
properties, 5-5 N
selecting port, 4-5 Notes, defined, 1-2
Gases tab, 5-5
Gases, types of, 1-5
Gasket, sample holder, 3-5 O
Graph, selecting type to display, 3-20 On/Off switch, 2-3
Open dialog, 5-7
Operator’s manual
H conventions, 1-2
H2 Fault, 2-1 organization, 1-1

Index-2 Mar 2013

HPVAII Series Operator’s Manual Index

O-rings, replacing in ports, 6-3 Sample compartment, 2-2

Schematic, 4-7
Selective Adsorption dosing, 4-17
P Sensor, hydrogen gas, 1-4
Panels Serial number, entering, 4-10
front, 2-1 Servo valves, threshold pressure, 4-17
rear, 2-3 Short data file, 2-6
Parameters Slope, 4-13
editing, 4-3 Software
entering, 3-18 hover menus, 2-6
used in calculations, 5-2 installation, C-1
Parameters tab, 5-2 starting and exiting, 2-6
Parts, ordering, 7-1 Specifications, 1-5, 1-6
PCT tab, 5-10 Standard dosing mode, 4-17
Port Step Isotherm Define Run window, 4-4
analysis, 2-2 System Configuration window, 4-10
degas, 2-2, 3-7 System valves, 4-7
Pressure
entering steps, 4-5
manifold, 4-13 T
range, 1-5 Tasks tab, 4-12
sample, 4-7 Temperature
table, 4-5 manifold, 2-1, 4-7
tolerance, 4-19 probe, 3-15
transducer, 1-5 sample bath, 4-8
Pressure limit, 4-10 setting, 4-5
resetting, 6-3 specifications, 1-5
tolerance, 4-19
tolerance, free-space analysis, 4-21
R Temperature control vessel, 2-2
Read Me tab, 5-6 Template, 3-17
Recall Template command, 3-18 loading, 3-18, 4-3
Recirculation bath, 4-4 saving, 4-3
Reference material, 7-1 Thermocouple connectors, 2-2
Reset, alarm, 2-3 Total Pore Volume report, 5-3
Run Experiment command, 3-19 Transducers
Run tab, 5-8 accuracy, 1-5
pressure, 1-5
Troubleshooting chart, 6-1
S
Sample
assembling the holder, 3-5 U
attaching to analysis port, 3-10 Unrestricted evacuation pressure, 4-11
bath temperature, 4-8
connecting to degas port, 3-7
cylinder, cleaning, 3-2 V
data, 5-12 Vacuum error, 6-1
degassing, 3-6 Vacuum gauge, 4-13
entering mass, 5-7 Valves
preparing, 3-1 description, 4-7
pressure, 4-7 manually controlling, 4-7
RTD, 4-13 metering, 6-9
weighing, 3-4 opening and closing, 3-12, 4-8

Mar 2013 Index-3

Index HPVA Series Operator’s Manual

Vent line flush, 4-18 W

Volume adsorbed, 5-8
Warnings, defined, 1-2
Volume dosed, 5-8
Weight Percentage plot, 5-10

Index-4 Mar 2013