1. Manuals
  2. Brands
  3. Particulate Systems Manuals
  4. Laboratory Equipment
  5. HPVA Series
  6. Operator's manual

Particulate Systems HPVA Series Operator's Manual

High pressure volumetric analyzer
Hide thumbs
Table of Contents

Advertisement

Quick Links

Download this manual
HPVA Series
High Pressure Volumetric Analyzer
Operator's Manual
V4.0
P02-42801-01
March 2011

Advertisement

Table of Contents
loading
Need help?

Need help?

Do you have a question about the HPVA Series and is the answer not in the manual?

Questions and answers

Related Manuals for Particulate Systems HPVA Series

Summary of Contents for Particulate Systems HPVA Series

  • Page 1 HPVA Series High Pressure Volumetric Analyzer Operator’s Manual V4.0 P02-42801-01 March 2011...
  • Page 2 Excel is a registered trademark of Microsoft Corporation. Windows is a registered trademark of Microsoft Corporation. © Particulate Systems 2011. All rights reserved. Printed in the U.S.A. The software described in this manual is furnished under a license agreement and may be used or copied only in...
  • Page 3 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.

  • Page 5: Table Of Contents

    Table of Contents 1. Introduction Conventions ..............1-1 Equipment Description.
  • Page 6 Table of Contents HPVA Series Operator’s Manual 4. Using the Manual Control Window Description ..............4-1 Controlling Valves .
  • Page 7 HPVA Series Operator’s Manual Table of Contents Conducting the Adsorption/Desorption Analysis ........B-10 Analyzing the Results .
  • Page 8 Table of Contents HPVA Series Operator’s Manual Mar 2011...

  • Page 9: Introduction

    1. Introduction This manual describes how to operate and maintain the HPVA High Pressure Volumetric Analyzer, Models HPVA-100 and HPVA-200. Conventions  This manual uses the following conventions:  Indicates important information pertinent to the subject matter.   Provides information that helps you prevent actions that may damage the instrument.

  • Page 10: Equipment Description

    The HPVA Series of analyzers includes two models: the HPVA-100, capable of achieving pressures up to 100 bar and the HPVA-200, capable of achieving pressures up to 200 bar. The HPVA Analyzer includes a separate degas port for drying the sample before testing. The furnace is capable of temperatures up to 500 °C, controlled with a routine which includes ramp and soak...
  • Page 11 HPVA Series Operator’s Manual Equipment Description To protect the user, the HPVA includes a hydrogen gas sensor to detect excessive levels of H2 gas should a leak in the system occur. If tripped, the safety circuit places the HPVA unit in a safe condition by removing power to the unit and closing all valves.

  • Page 12: Controls And Connectors

    Controls and Connectors HPVA Series Operator’s Manual Controls and Connectors Upper Front Panel Pressure Display Manifold Temperature Control/Display System Schematic Furnace Temp. Control/ Display Valve Switches Vent Valve Vacuum Valve Control Control Pressure Displays the manifold pressure when set to PM and the sample pressure when set to PS.
  • Page 13 HPVA Series Operator’s Manual Controls and Connectors Vacuum Valve Control Enables you to control the flow rate through vacuum valve 4. Vent Valve Control Enables you to control the flow rate through the vent valve. Valve Switches Enable you to open and close valves. You can also open and close valves 1 through 8 through the software, which is the recommended method of manual control.

  • Page 14: Sample Compartment

    Controls and Connectors HPVA Series Operator’s Manual Sample Compartment Thermocouple Connectors Degas Port Analysis Port Temperature Control Vessel Furnace Temperature Control Vessel Maintains the temperature of the sample during an experiment. Analysis Port Port used to perform an experiment. Thermocouple Connectors Connect the furnace thermocouples to the instrument....

  • Page 15: Rear Panel

    HPVA Series Operator’s Manual Controls and Connectors Rear Panel Bath Communication Vacuum Vent Alarm Alarm Reset On/Off Power Cord Gas1 Gas2 Gas3 Switch Connector Bath Connects the recirculating bath to the instrument. Communication Connects the computer to the instrument. Vacuum Connects the vacuum pump to the instrument....

  • Page 16: Turning The Analyzer On And Off

    Turning the Analyzer On and Off HPVA Series Operator’s Manual Connects the nitrogen or compressed air supply for the pneumatic valves to the instrument. Gas1 Connects an analysis gas to the instrument. Gas2 Connects another analysis gas to the instrument....

  • Page 17: Main Menu

    Configure Hardware Enables you to change parameters that affect the operation of the analyzer. Help Displays the HPVA Series Operator’s Manual on the screen. Use the Bookmarks and Table of Contents to find the information you need. Exit Closes the HPVA software.

  • Page 18: Starting And Exiting The Hpva Software

    Starting and Exiting the HPVA Software HPVA Series Operator’s Manual Starting and Exiting the HPVA Software  To start the HPVA software, click the HPVA icon on your desktop or select the software using the appropriate Windows function. To close the HPVA software, click the Exit button on the HPVA Main Menu.

  • Page 19: Specifications

    HPVA Series Operator’s Manual Specifications Specifications Characteristic Specification Environment Temperature: 10 to ºC, operating; -10 to 55 ºC, storing or shipping Humidity: 20 to 80% relative, non-condensing Physical Height 35 in. (88.9 cm) Width: 20 in. (50.8 cm) Depth: 20 in. (50.8 cm)
  • Page 20 Specifications HPVA Series Operator’s Manual 1-12 Mar 2011...

  • Page 21: Performing An Experiment

    • Running an experiment Preparing the Sample Requirements The following items are required to prepare a sample and perform an experiment with the HPVA  analyzer. Supplied by User Supplied by Particulate Systems • Ultrasonic bath • Sample holder assembly •...

  • Page 22: Cleaning The Sample Cylinder

    Preparing the Sample HPVA 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 500ml of warm water. Fill the bowl of the ultrasonic unit with enough water to cover the sample cylinder.
  • Page 23 HPVA 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.

  • Page 24: Weighing The Sample

    Preparing the Sample HPVA Series Operator’s Manual Weighing the Sample Tare a 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.

  • Page 25: Assembling The Sample Holder

    HPVA Series Operator’s Manual Preparing the 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. Assembling the Sample Holder 1.
  • Page 26 Preparing the Sample HPVA Series Operator’s Manual  Connector 3. Use the two wrenches (5/8-in and 3/4-in) to tighten the connector an additional 1/8 turn. Mar 2011...

  • Page 27: Degassing The Sample

    HPVA Series Operator’s Manual Degassing the Sample 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...
  • Page 28 Degassing the Sample HPVA Series Operator’s Manual 3. Tilt the furnace, then insert the sample holder assembly into the furnace. 4. Connect the sample holder to the degas port by first ensuring that the O-ring is in place in the degas port.
  • Page 29 HPVA Series Operator’s Manual Degassing the Sample 6. Using two wrenches (3/4-in and 5/8-in) tighten the nut just until snug.   the connector nut, doing so could damage the Do not over tighten port fitting. 7. Begin the sample evacuation by opening valve 9 as shown. Note that the valve 9 indicator on the...
  • Page 30 Degassing the Sample HPVA Series Operator’s Manual 8. Slowly open the isolation valve on the sample holder by turning it completely counterclockwise. Turn isolation valve counterclockwise 9. Monitor the external vacuum gauge to ensure that vacuum is reached. 10. Set the temperature to the desired level by holding the left FURNACE button and the up or down button as needed.
  • Page 31 HPVA Series Operator’s Manual Degassing the Sample 12. Close valve 9. The valve 9 indicator on the front panel will turn off. 13. Set the furnace to 0 °C and allow the sample to cool to room temperature. 14. Remove the sample holder from the degas port after the sample has cooled to room temperature by using two wrenches (3/4-in and 5/8-in) to loosen the connector nut.

  • Page 32: Attaching The Sample Holder To The Analysis Port

    Attaching the Sample Holder to the Analysis Port HPVA Series Operator’s Manual Attaching the Sample Holder to the Analysis Port 1. Connect the temperature control vessel by attaching the supply and return 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.
  • Page 33 HPVA Series Operator’s Manual Attaching the Sample Holder to the Analysis Port 2. Place the sample holder in the temperature control vessel by tilting the temperature control vessel and placing the sample holder in the vessel. 3. Connect the sample holder to the analysis port by first ensuring that the O-ring is in place in the port.
  • Page 34 Attaching the Sample Holder to the Analysis Port HPVA Series Operator’s Manual 4. Attach the sample holder to the analysis port and hand-tighten the connector nut. 5. Using two wrenches (3/4-in and 5/8-in) tighten the nut just until snug. ...

  • Page 35: Purging The System

    HPVA Series Operator’s Manual Purging the System Purging the System When the HPVA is performing an experiment or being operated in manual control mode, the valve switches on the front panel should be placed and remain in the closed (down) position.
  • Page 36 Purging the System HPVA Series Operator’s Manual 2. Open valves 1 and 3 as shown below. Check the Manifold pressure displayed on the screen. There should be no pressure on the manifold (reading should be 1 bar or less). 24.00 1.000...
  • Page 37 HPVA Series Operator’s Manual Purging the System 6. Open valve 8 and pressurize the instrument until the Sample pressure displayed on the screen reads 15 bar. 24.00 15.000 31.00 15.000 7. Close valve 8. 8. Open valve 2. 9. Adjust the Vent control knob on the front panel of the instrument to allow pressure to vent.
  • Page 38 Purging the System HPVA Series Operator’s Manual 14. When the system reaches full vacuum, open the isolation valve on the sample holder by turning it completely counterclockwise. Turn isolation valve completely counterclockwise 15. Plug the temperature probe cable into the connector on the instrument.
  • Page 39 HPVA Series Operator’s Manual Purging the System 19. Close all valves 24.00 1.000 31.00 1.000 20. You are now ready to run the experiment. Mar 2011 2-19...

  • Page 40: Running The Experiment

    Running the Experiment HPVA Series Operator’s Manual Running the Experiment The Adsorption option on the Main Menu is used to define and perform experiments. This function involves two windows: • The System Experiment Definition window allows you to enter a sample ID and sample information....
  • Page 41 HPVA Series Operator’s Manual Running the Experiment 2. Choose one of the following: • To enter a new set of experiment parameters, proceed to step 3. • To use an existing set of experiment parameters: a. Click Recall Template to display the Select Experiment Template File to Load window.
  • Page 42 Running the Experiment HPVA Series Operator’s Manual 9. Click Add to add run parameters to the experiment. The HPVA System Step Isotherm: Define Run window is displayed. 10. Add the parameters for the run, then click OK. Refer to Define Run Window, page 2-29 for a description of the fields on this screen.

  • Page 43: Viewing The Experiment

    HPVA Series Operator’s Manual Viewing the Experiment Viewing the Experiment 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.
  • Page 44 Viewing the Experiment HPVA Series Operator’s Manual View Parameters This command displays the Modify Current Run Parameters window, which enables you to change parameters for any step that has not completed. 2-24 Mar 2011...
  • Page 45 HPVA Series Operator’s Manual Viewing the Experiment View FS Data This command enables you to view free space data. Ambient: the free space at ambient temperature is shown. Analysis: the free space at the analysis temperature is shown. The 1st row shows values at ambient temperature.

  • Page 46: Adjusting Flow Valves

    Viewing the Experiment HPVA Series Operator’s Manual Adjusting Flow Valves The Vent valve control on the instrument’s front panel adjusts the flow rate through the vent valve. If the flow rate is high, you may not be able to achieve accurate dosing pressures. If the flow rate is low, the length of the experiment will be increased.

  • Page 47: Definitions Of Fields In The System Windows

    HPVA Series Operator’s Manual Definitions of Fields in the System Windows Definitions of Fields in the System Windows Define New Experiment Window Exp ID Enter the experiment identifier. The data files created will use this name. Operator ID Enter the name or initials of the operator....
  • Page 48 Definitions of Fields in the System Windows HPVA Series Operator’s Manual Notes (1) and (2) Enter any additional notes about the sample here, for example, the degas time. Low Pressure Factor If you check this option, the system will not dose the manifold to a pressure exceeding the Value times the desired sample pressure in the pressure table if it is below the entered pressure.

  • Page 49: Define Run Window

    HPVA Series Operator’s Manual Definitions of Fields in the System Windows Define Run Window Equilibration Criteria Specifies when the system has reached equilibrium after each step in the adsorption/desorption procedure. Enter the pressure to be reached and the number of minutes in which it should be reached.
  • Page 50 Definitions of Fields in the System Windows HPVA Series Operator’s Manual Ambient Temp: Enter the temperature of the air in the laboratory in °C. Hold: Enter the number of minutes the system will wait once the sample RTD reaches the ambient temperature....
  • Page 51 HPVA Series Operator’s Manual Definitions of Fields in the System Windows Exper FS If the Measure FS box is not checked, enter the experiment free space volume of the sample tube in this field. Click OK to save the run parameters and return to the System Experiment Definition window....
  • Page 52 Definitions of Fields in the System Windows HPVA Series Operator’s Manual 2-32 Mar 2011...

  • Page 53: Viewing Experiment Results

    3. Viewing Experiment Results Experiment data are viewed in the Microsoft® Excel Macro that was installed during installation of the HPVA. The macro preforms the following: • Calculates free space data for both the ambient volume and the analysis temperature volume. •...

  • Page 54: Read Me Tab

    Running the Macro HPVA Series Operator’s Manual Read Me Tab The ReadMe tab displays information about the HPVA Macro. Gases Tab The Gases Tab displays the gas properties used in calculations. The columns contained on this sheet are: Adsorbate The name of the adsorbate is listed on one line and its symbol on the next line.

  • Page 55: Parameters Tab

    HPVA Series Operator’s Manual Running the Macro The critical temperature expressed in Kelvin. NistName The National Institute of Standards name of the adsorbate. This is the name the REFPRO software recognizes when called for compressibility data. Molecular Weight The molecular weight of the adsorbate.
  • Page 56 Running the Macro HPVA Series Operator’s Manual Parameter Settings Set Baseline Set this option to TRUE if a blank tube analysis was performed. Otherwise, set it to FALSE. When set to TRUE, this option corrects errors in an analysis by using data collected from a blank tube analysis.

  • Page 57: Compile Error Message

    HPVA Series Operator’s Manual Compile Error Message Parameter Settings Density Correction If you entered free space data in the HPVA Define Run window from an empty sample tube prior to the analysis, set this option to TRUE. The program will prompt you for the density of the sample.

  • Page 58: Displaying Experiment Data

    Displaying Experiment Data HPVA Series Operator’s Manual Displaying Experiment Data Experiment data can be displayed in one of two formats: • Long Data File • Short Data File  When you select Read Long Data File from the HPVA menu, a spreadsheet containing all the raw data from the experiment is displayed.
  • Page 59 HPVA Series Operator’s Manual Displaying Experiment Data 3. A sheet similar to the one shown below is displayed. 4. Information about the sample is displayed in the first several rows. Following the experiment information is a table of the data collected.

  • Page 60: Read Short Data File

    Displaying Experiment Data HPVA Series Operator’s Manual Read Short Data File The Short Data file displays two graphs, 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 sym- bols, modify the legend, etc.
  • Page 61 HPVA Series Operator’s Manual Displaying Experiment Data 4. A spreadsheet similar to the following is displayed. A PCT graph of the experiment data is displayed and the Save As dialog is 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.
  • Page 62 Displaying Experiment Data HPVA Series Operator’s Manual 5. You can click the isotherm tab to display an isotherm of the experiment data. An example is shown below. 3-10 Mar 2011...
  • Page 63 HPVA Series Operator’s Manual Displaying Experiment Data 6. You can click the file name tab to display experiment data and the volume dosed and volume adsorbed calculations. The columns in the calculation tables are described below. Column Heading Description ReqPm...
  • Page 64 Displaying Experiment Data HPVA Series Operator’s Manual Column Heading Description Vol Dosed Volume of adsorbate dosed to sample this step Total Dosed Total volume of adsorbate dosed to sample Pressure of sample after dosing Temperature of sample after dosing Compressibility of adsorbate at Ps and Ts...

  • Page 65: Read Helium Data File

    HPVA Series Operator’s Manual Displaying Experiment Data Read Helium Data File The Helium Data file displays two graphs, as well as information about the free space analysis and cal- culations. When the graphs are displayed, you can use Excel charting functions to change curve colors, add symbols, modify the legend, etc.
  • Page 66 Displaying Experiment Data HPVA Series Operator’s Manual 3-14 Mar 2011...

  • Page 67: Using The Manual Control Window

    4. Using the Manual Control Window Description The Manual Control Window shows a schematic of the HPVA System and can be used to manually open and close valves and, if a temperature control bath or cryostat is used, to set the sample temperature.

  • Page 68: Controlling Valves

    Controlling Valves HPVA Series Operator’s Manual Controlling Valves The nine valves are represent by numbered icons. 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. Yel- low indicates a closed valve and green indicates an open valve.

  • Page 69: Setting The Sample Bath Temperature

    HPVA Series Operator’s Manual Setting the Sample Bath Temperature Setting the Sample Bath Temperature If a temperature control bath or cryostat is configured with the instrument, you can set the bath temper- ature using the Manual Control screen as follows: 1.
  • Page 70 Setting the Sample Bath Temperature HPVA Series Operator’s Manual Mar 2011...

  • Page 71: Configuring The System

    5. Configuring the System This chapter describes how to use the following options on the Main Menu: • Calibration • Change Data Directory • Configure Hardware Calibrating the System The Calibration option requires the use of a known volume cylinder. Calibration should be performed only by authorized service personnel.

  • Page 72: Configuring The Hardware

    Configuring the Hardware HPVA Series Operator’s Manual Configuring the Hardware When you select Configure Hardware on the Main Menu, the System Configuration window is displayed. System Configuration Window The System Configuration window contains 8 tabs of parameters that you can edit prior to performing an experiment.

  • Page 73: Tasks Tab

    Main Menu). Advanced Mode Check this box to run the instrument in Advanced Mode. To prevent damage to the system, this option should only be enabled at the direction of a Micromeritics/Particulate Systems service representative. Tasks Tab Analog Input Tasks Lists the tasks configured with the NI MAX software used to read data from the instrument.

  • Page 74: Analog Input Tab

    System Configuration Window HPVA Series Operator’s Manual Digital Output Tasks Lists the tasks configured with the NI MAX software used to control the instrument valves. These tasks are configured during software installation. Analog Input Tab Manifold Pressure Shows the slope and intercept for the linear calibration of the manifold transducer.

  • Page 75: Analog Output Tab

    HPVA Series Operator’s Manual System Configuration Window Analog Output Tab Calibration Enter the values to be used for the temperature calibration of the temperature control bath.  Limits Min Bath Temp Enter the minimum analysis temperature allowed if Bath is selected on the System Step Isotherm window when preparing for an experiment....

  • Page 76: Instrument Options Tab

    System Configuration Window HPVA Series Operator’s Manual Instrument Options Tab Servo Configured If the instrument is configured with servo valves, this option must be selected. If the instrument is configured with needle valves, this option must be cleared. Digital Output Tasks The NI MAX task associated with the vacuum servo valve.
  • Page 77 HPVA Series Operator’s Manual System Configuration Window Gas Multipliers Enter the values used to control the servo valve based on the gas in the system. If a cryostat is to be used during analyses, check this box.  Cryostat Configured...

  • Page 78: Dosing Tab

    System Configuration Window HPVA Series Operator’s Manual Dosing Tab Select on of three dosing mode options from the drop-down list: Dosing Mode Standard The system will dose the sample to the desired pressure points listed in the System Step Isotherm window without evacuating the sample tube between points.
  • Page 79 HPVA Series Operator’s Manual System Configuration Window Selective Adsorption Mode Evac Time The amount of time the system evacuates the sample tube between pressure points when Selective Adsorption Mode is enabled. Sampling Pressure After equilibration, the system will vent the manifold to this pressure before triggering the external device to collect data.

  • Page 80: Adsorption Tab

    System Configuration Window HPVA Series Operator’s Manual Adsorption Tab Pressure Tolerance Threshold The pressure at which the dose pressure tolerance below (this value) is different from the pressure tolerance above (this value).  Above Threshold The dose pressure must be within + the value entered here for the system to continue during dosing.

  • Page 81: Free Space Tab

    HPVA Series Operator’s Manual System Configuration Window Vent Time The amount of time the vent remains open after the third helium fill/vent cycle. Vent Expand Vent Pressure During the adsorption experiment, the system will be considered vented if at or below this pressure. ...
  • Page 82 System Configuration Window HPVA Series Operator’s Manual Max Equil Time The maximum time allowed for equilibration during the free space analysis.  Temperature Tolerance The temperature tolerance allowed for the ambient and analysis temperatures during the free space analysis ( + this value)....

  • Page 83: Troubleshooting And Maintenance

    6. Troubleshooting and Maintenance The HPVA system has been designed to provide efficient and continuous service. However, certain 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: •...
  • Page 84 Troubleshooting HPVA Series Operator’s Manual What Happened What to Do Low degas adsorption Contaminated 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.
  • Page 85 HPVA Series Operator’s Manual Troubleshooting What Happened What to Do Pressure cycling Gas is venting out of the Adjust the Vent valve on the (continued) manifold too fast. instrument’s front panel. Target pressure not Gas level in tank is too low.

  • Page 86: Resetting The Pressure Limit

    Troubleshooting HPVA Series Operator’s Manual Resetting the Pressure Limit Select Configure Hardware from the HPVA main menu. Make sure the Instrument tab is selected. Enter the maximum pressure for the gas you are using in the Pressure limit field. Click Save.

  • Page 87: Entering The Slope

    HPVA Series Operator’s Manual Troubleshooting Entering the Slope Select Configure Hardware from the HPVA main menu. Make sure the Analog Input tab is selected. Enter the correct slope in Manifold Pressure and Sample 1 Pressure fields as follows: HPVA-100 = 13.7895...

  • Page 88: Replacing Degas And Analysis Port O-Rings

    Connecting Gases HPVA Series Operator’s Manual Replacing Degas and Analysis Port O-Rings Each of the ports, degas and analysis, contains an O-ring that must be present when degassing or ana- lyzing a sample. Ensure that the O-ring is present before performing either procedure.

  • Page 89: Required Items

    HPVA Series Operator’s Manual Connecting Gases Required Items. Particulate Systems Supplied User Supplied Stainless steel gas tubing Analysis gas (recommended purity 99.999%) Two 7/16-in. wrenches Helium (recommended purity 99.999%) Clean compressed air and air line Regulators for gas bottles Disconnecting the Depleted Bottle 1.

  • Page 90: Connecting A Replacement Gas Bottle

    Connecting Gases HPVA Series Operator’s Manual 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.
  • Page 91 HPVA Series Operator’s Manual Connecting Gases Do not overtighten the fitting; doing so may cause a leak. 3. Check for leaks at the high-pressure side of the regulator and in the connector. HIgh-pressure Gauge Gas Bottle Shut- Off valve Regulator...
  • Page 92 Connecting Gases HPVA Series Operator’s Manual c. Close the regulator shut-off valve to stop flow. d. Close the gas bottle valve. 5. Set the instrument pressure. Low-pressure Gauge Regulator Gas Bottle Shut-Off Shut-Off valve valve Regulator Control knob a. Turn the regulator control knob clockwise until the low-pressure gauge reads 15 psi ...

  • Page 93: Adjusting The Metering Valves

    HPVA 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.
  • Page 94 Adjusting the Metering Valves HPVA Series Operator’s Manual 4. Make sure all the shut-off valves shown in the schematic are closed. 5. Turn on the gas at the gas bottle. 6. On the Manual Control screen, open valve 3 so that pressure can be read.
  • Page 95 HPVA Series Operator’s Manual Adjusting the Metering Valves 7. On the Manual Control screen, open the gas line valve, for example, valve 6 for Gas Line 1. 8. Slightly open the metering valve. 9. Observe the Manifold pressure (Pm) shown on the Manual Control screen. The pressure should rise approximately 1 bar every 10 to 20 seconds.
  • Page 96 Adjusting the Metering Valves HPVA Series Operator’s Manual 12. To recheck the pressure: a. Close valve 2. a. 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.

  • Page 97: Ordering Information

    7. Ordering Information Components for the HPVA Series analyzers can be ordered using one of the following methods: • Call Customer Service at (770) 662-3636 • Contact your local sales representative When ordering, please use the information provided below to place your order.
  • Page 98 Ordering Informatioin HPVA Series Operator’s Manual Mar 2011...

  • Page 99: Error Messages

    A. Error Messages This appendix contains the error messages that may be encountered while operating the HPVA Series instruments; they are listed in alphabetical order. Changes made to the pressure steps table affect steps that have already run. Cause: You attempted to update the pressure table that modified pressure points already collected.
  • Page 100 Appendix A HPVA 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.
  • Page 101 HPVA Series Operator’s Manual Appendix A Unable to read info from .ini file Cause: The application initialization file is missing from the HPVA System appli- cations directory. Action: Verify that all HPVA System applications and the HPVASys.ini file are in the same directory.
  • Page 102 Appendix A HPVA Series Operator’s Manual You must enter a valid Expt ID before you can run. (list of unavailable characters) Cause: The entered Experiment ID contains invalid characters. Action: Use an alternate experiment ID. You must enter an Expt ID before you can run.

  • Page 103: Performing A Cryogenic Analysis

    Description This appendix contains instructions for performing an analysis with the optional Cryogenic Kit, avail- able from Particulate Systems. Due to helium interaction with samples at cryogenic temperatures, it is difficult to find the true analy- sis free space of the sample tube with the sample present. Therefore, we recommend that you first find the ambient and analysis free space volumes of the empty sample tube to be used in the analysis.

  • Page 104: Measuring Free Space

    Measuring Free Space HPVA 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 2-2.) 2. Assemble the sample holder. (Refer to Assembling the Sample Holder, page 2-5.)
  • Page 105 HPVA Series Operator’s Manual Measuring Free Space 5. Ensure that the O-ring is in place in the analysis port. O-ring 6. Tilt the dewar and insert the sample holder. 7. Attach the sample holder to the sample port and hand-tighten the connector nut.
  • Page 106 Measuring Free Space HPVA Series Operator’s Manual 9. Select the Adsorption option from the HPVA main menu. The Experiment Definition: New window is displayed. 10. Enter information in the fields in this window. (Refer to Define New Experiment Window, page 2-27).
  • Page 107 HPVA Series Operator’s Manual Measuring Free Space 11. Click Add to enter the analysis conditions for the free space measurement. The Define Run window is displayed. 12. Select the External Temperature Control Method radio button. 13. Enter the Experiment and Ambient temperatures.
  • Page 108 Measuring Free Space HPVA Series Operator’s Manual 17. Click Run Experiment. 18. The software will find the ambient temperature free space volume. When this step is completed, you will be prompted to make the temperature change. 19. Fill the dewar with liquid nitrogen to the top of the isothermal jacket.
  • Page 109 HPVA Series Operator’s Manual Measuring Free Space 21. Place the strap around the dewar cover and tighten. 22. Insert the temperature probe into the dewar. 23. Click OK.  Do not remove the sample tube from the analysis port between the ambient temperature volume analysis and the analysis temperature volume analysis.

  • Page 110: Displaying The Free Space

    Measuring Free Space HPVA Series Operator’s Manual Displaying the Free Space 1. Open the Excel Macro. 2. Select Read Short Data File from the HPVA menu. 3. Select He Data Files (*HIHe) from the File Type drop-down list. 4. 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.

  • Page 111: Preparing The Sample

    HPVA Series Operator’s Manual Preparing the Sample Preparing the Sample 1. Remove the sample holder from the analysis port. 2. Remove the isothermal jacket. 3. Allow the sample holder to return to room temperature. 4. Remove any condensation that formed on the exterior of the sample holder.
  • Page 112 Conducting the Adsorption/Desorption Analysis HPVA Series Operator’s Manual Conducting 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.
  • Page 113 HPVA Series Operator’s Manual Conducting the Adsorption/Desorption Analysis 5. Attach the sample holder to the sample port and hand-tighten the connector nut. 6. Using two wrenches (3/4-in and 5/8-in) tighten the nut just until snug. Note, do not over tighten the connector nut, doing so could damage the port fitting.
  • Page 114 Conducting the Adsorption/Desorption Analysis HPVA Series Operator’s Manual 7. Select the Adsorption option from the HPVA main menu. The Experiment Definition: New window is displayed. 8. Enter information in the fields in this window. (Refer to Define New Experiment Window, page 2-27).
  • Page 115 HPVA Series Operator’s Manual Conducting the Adsorption/Desorption Analysis 10. Select the External Temperature Control Method radio button. 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.
  • Page 116 Conducting the Adsorption/Desorption Analysis HPVA Series Operator’s Manual 22. Place the dewar cover on top of the dewar. 23. Place the strap around the dewar cover and tighten. B-14 Mar 2011...
  • Page 117 HPVA Series Operator’s Manual Conducting the Adsorption/Desorption Analysis 24. Insert the temperature probe into the dewar. 25. Click OK. 26. Once the system has reached the desired temperature and the hold time has elapsed, the HPVA will begin the analysis.
  • Page 118 Analyzing the Results HPVA Series Operator’s Manual Analyzing the Results 1. Open the Excel Macro. 2. Click the Parameter tab if the Parameter page is not already displayed. 3. Make sure the Density Correction is set to TRUE. 4. Select Read Short Data File from the HPVA menu.
  • Page 119 HPVA Series Operator’s Manual Analyzing the Results 8. A PCT graph of the experiment data is displayed and the Save As dialog is 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.
  • Page 120 Analyzing the Results HPVA Series Operator’s Manual B-18 Mar 2011...
  • Page 121 HPVA Series Operator’s Manual Index INDEX Adsorbate, 3-2 Data file, 1-10 Adsorbate Name, 2-30 Data Logging Interval, 2-30 Adsorption command, 1-9, 2-20 Define New Experiment Window, 2-27 Adsorption tab, 5-10 Define Run window, 2-20, 2-22, 2-29 Advanced mode, 5-3 Degas...
  • Page 122 Index HPVA Series Operator’s Manual types, 1-10 Main menu, 1-9 Free space Maintenance, system, 6-1 measure, 2-30 Manifold Free Space tab, 5-11 pressure, 1-4, 2-23, 5-4 Furnace, 1-2 RTD, 5-4 connecting thermocouple, 2-7 temperature, 1-4, 2-23, 4-1 control, 1-4 Manual Control...
  • Page 123 HPVA Series Operator’s Manual Index Thermocouple connectors, 1-6 Transducers Read Long Data File, 3-6 accuracy, 1-11 Read Me tab, 3-2 pressure, 1-11 Read Short Data File, 3-6 Troubleshooting chart, 6-1 Recall Template command, 2-21 Reset, alarm, 1-7 Run Experiment command, 2-22...
  • Page 124 Index HPVA Series Operator’s Manual Index-4 Mar 2011...

Table of Contents