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Running the Experiment

HPVA Series Operator’s Manual

2-20

Mar 2011

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.



•

The System Step Isotherm Define Run window allows you to specify the experiment parameters.



The HPVA 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 cre-

ated, you can use it for other experiments by just loading it into the System Definition window 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 experiment, and
viewing the isotherm. Refer to “Definitions of Fields in the System Windows” on page 2-27 for details
about the fields on this window.

1. Click

Adsorption

on the Main Menu to display the System Experiment Definition window.

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Содержание HPVA Series

Страница 1: ...HPVA Series High Pressure Volumetric Analyzer Operator s Manual V4 0 P02 42801 01 March 2011...

Страница 2: ...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 b...

Страница 3: ...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...

Страница 4: ......

Страница 5: ...ighing the Sample 2 4 Assembling the Sample Holder 2 5 Degassing the Sample 2 7 Attaching the Sample Holder to the Analysis Port 2 12 Purging the System 2 15 Running the Experiment 2 20 Viewing the Ex...

Страница 6: ...sing Tab 5 8 Adsorption Tab 5 10 Free Space Tab 5 11 6 Troubleshooting and Maintenance Troubleshooting 6 1 Resetting the Pressure Limit 6 4 Entering the Slope 6 5 Replacing Degas and Analysis Port O R...

Страница 7: ...HPVA Series Operator s Manual Table of Contents Mar 2011 iii Conducting the Adsorption Desorption Analysis B 10 Analyzing the Results B 16 INDEX...

Страница 8: ...Table of Contents HPVA Series Operator s Manual iv Mar 2011...

Страница 9: ...tions 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 Prov...

Страница 10: ...antity of gas adsorbed by the sample This process is repeated at given pressure intervals until the maximum pre selected pressure is reached Each of the resulting equilib rium points volume adsorbed a...

Страница 11: ...iewed 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 ty...

Страница 12: ...PM and the sample pressure when set to PS The display is useful as a quick reference a more accurate reading of the pressure can be displayed on the software screen Manifold Temperature Control and D...

Страница 13: ...is the recommended method of manual control Valve 9 can be controlled by the switch only System Schematic A schematic of the manifold showing valve status A valve indicator turns on when the valve is...

Страница 14: ...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...

Страница 15: ...strument Vacuum Connects the vacuum pump to the instrument Vent Connects vent tubing to the instrument Alarm Turns on when power is applied to the instrument or when the H2 sensor is triggered Alarm R...

Страница 16: ...n on the back panel of the analyzer 3 The alarm indicator will turn off 4 Wait 30 to 60 minutes to allow the manifold temperature to stabilize To turn off the analyzer 1 Ensure that the analyzer is ve...

Страница 17: ...onditions 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 i...

Страница 18: ...name extensions used by the HPVA software File Type Extension Data file generated only if Advanced Mode is activated primarily used to troubleshoot the instrument contains data for everything that oc...

Страница 19: ...Monoxide and Carbon Dioxide Pressure Pressure range HPVA 100 vacuum to 100 bar HPVA 200 vacuum to 200 bar Pressure transducer Pressure reading accuracy is 0 04 full scale with a stability of 0 1 Compu...

Страница 20: ...Specifications HPVA Series Operator s Manual 1 12 Mar 2011...

Страница 21: ...mple 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 Long stemmed pi...

Страница 22: ...er 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 Pi...

Страница 23: ...e 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...

Страница 24: ...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 cylind...

Страница 25: ...semble the sample holder by placing the gasket on the sample cylinder as shown below Gasket Note that the gasket can be used only once Reusing the gasket may cause leaks at the sample holder connectio...

Страница 26: ...Connector Nut Preparing the Sample HPVA Series Operator s Manual 2 6 Mar 2011 3 Use the two wrenches 5 8 in and 3 4 in to tighten the connector an additional 1 8 turn...

Страница 27: ...11 2 7 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 sa...

Страница 28: ...lt 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 O ring 5 Attach the...

Страница 29: ...wrenches 3 4 in and 5 8 in tighten the nut just until snug Do not over tighten the connector nut doing so could damage the port fitting 7 Begin the sample evacuation by opening valve 9 as shown Note t...

Страница 30: ...ockwise 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 Allow th...

Страница 31: ...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 15 Remove the sample ho...

Страница 32: ...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...

Страница 33: ...rt Mar 2011 2 13 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 an...

Страница 34: ...perator s Manual 2 14 Mar 2011 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 Do not over tig...

Страница 35: ...ened position during a software operation it will override the software and may damage the instrument 1 Click Manual Control from the Main Menu to display the Manual Control screen 24 00 1 000 1 000 3...

Страница 36: ...pressure displayed on the screen There should be no pressure on the manifold reading should be 1 bar or less 31 00 1 000 24 00 1 000 3 Open valve 4 until the pressure reaches about 0 5 bar then close...

Страница 37: ...0 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 10 When the pressure reaches 1 bar or less close valve 2 11 Repeat...

Страница 38: ...e completely counterclockwise 15 Plug the temperature probe cable into the connector on the instrument 16 Insert the temperature probe into the temperature control vessel Temperature Probe Connector 1...

Страница 39: ...HPVA Series Operator s Manual Purging the System Mar 2011 2 19 19 Close all valves 24 00 1 000 1 000 31 00 20 You are now ready to run the experiment...

Страница 40: ...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 i...

Страница 41: ...k Load c Enter an experiment ID in the Expt ID field c Make any desired changes d Proceed to Step 10 3 Enter an ID for the experiment 4 Enter an Operator ID for the experiment 5 Under Use Sample Ports...

Страница 42: ...ow page 2 29 for a description of the fields on this screen 11 Repeat steps 9 and 10 for each run you wish to add to the experiment 12 When you have finished entering information click Run Experiment...

Страница 43: ...m 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 Manifold The current Manifold temperature and...

Страница 44: ...e Experiment HPVA Series Operator s Manual 2 24 Mar 2011 View Parameters This command displays the Modify Current Run Parameters window which enables you to change parameters for any step that has not...

Страница 45: ...analysis temperature The columns are described below Pm0 Initial manifold pressure Tm0 Initial manifold temperature Ps0 Initial sample pressure Ts0 Initial sample temperature PmA Manifold pressure bef...

Страница 46: ...flow rate is low the length of the experiment will be increased Close the valve slightly if the instrument is having diffi culty achieving dosing pressures within the specified tolerance Open the valv...

Страница 47: ...ated will use this name Operator ID Enter the name or initials of the operator Use Sample Ports Check port 1 The window shows ports 1 through 4 however the models covered in this manual the HPVA 100 a...

Страница 48: ...pically used above 2 bar with a factor of 1 5 If you select this option use the arrow keys to select the pressure in the Use below field and the value in the Value field Recall Template Click this but...

Страница 49: ...the maximum equilibration time in minutes in the Max Equilib Time field Control Method Select the temperature control method to be used during the experiment Click Bath if a recirculation bath or cryo...

Страница 50: ...ure check Mixture Pressure Steps This table lists the pressures the sample holder will reach during the experiment when the standard dosing mode is used To enter a pressure step enter the pressure in...

Страница 51: ...f the Measure FS box is not checked enter the experiment free space volume of the sample tube in this field OK Click OK to save the run parameters and return to the System Experiment Definition window...

Страница 52: ...Definitions of Fields in the System Windows HPVA Series Operator s Manual 2 32 Mar 2011...

Страница 53: ...ta isotherms Displays the raw data collected by the HPVA program during an experiment Enables you to copy and paste data into other programs such as Microsoft Word or to save data in a variety of form...

Страница 54: ...perties 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 Both the name and symbol are listed so th...

Страница 55: ...e Tc K 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 d...

Страница 56: ...pt at each pressure point in the isotherm using a volumetric basis This correction should only be used if the blank sample tube analysis was performed at the same temperature in the same pressure rang...

Страница 57: ...meter 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 t...

Страница 58: ...taining all the raw data from the experiment is displayed When you select Read Short Data File the following are displayed Volume Adsorbed isotherm PCT Information about the experiment Calculations fo...

Страница 59: ...ing the experiment information is a table of the data collected Column Heading Description Elap Time min Elapsed time in the experiment Pm bar Manifold pressure P1 bar Sample pressure Tm deg C Manifol...

Страница 60: ...the legend etc 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 Read Short Data File fr...

Страница 61: ...1 3 9 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 spreadshe...

Страница 62: ...Displaying Experiment Data HPVA Series Operator s Manual 3 10 Mar 2011 5 You can click the isotherm tab to display an isotherm of the experiment data An example is shown below...

Страница 63: ...ing Description ReqPm Requested pressure by the user Target Pm Manifold target pressure for dosing PmA Pressure of manifold before dosing TmA Temperature of manifold before dosing ZA Compressibility o...

Страница 64: ...pressibility of adsorbate at Ps and Ts Vs NAds Volume of adsorbate in sample cylinder after dosing ZXL Compressibility of adsorbate at Ps and TmA Vxl Volume of adsorbate in lower stem after dosing ZXU...

Страница 65: ...e Excel functions such as Cut Copy and Save As to transfer data to other programs Refer to your Excel documentation for more information Follow the instructions for Read Short Data File page 3 8 with...

Страница 66: ...Displaying Experiment Data HPVA Series Operator s Manual 3 14 Mar 2011...

Страница 67: ...n and close valves and if a temperature control bath or cryostat is used to set the sample temperature 24 00 1 000 1 000 31 00 Manifold temperature Manifold pressure Sample pressure Sample temperature...

Страница 68: ...ressure 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 valves in the schematic are described below Val...

Страница 69: ...mperature 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 Double click the left mouse button...

Страница 70: ...Setting the Sample Bath Temperature HPVA Series Operator s Manual 4 4 Mar 2011...

Страница 71: ...known volume cylinder Calibration should be performed only by authorized service personnel Changing the Data Directory The Data Directory is the folder in which the files produced by the system are pl...

Страница 72: ...prior to performing an experiment The tabs and their associated dialogs are described below Instrument Tab Serial Number Enter the instrument s serial number If a number is not entered or a wrong num...

Страница 73: ...n change the directory in which data files are written this can be done more conveniently by selecting Change Data Directory from the Main Menu Advanced Mode Check this box to run the instrument in Ad...

Страница 74: ...e port transducers Models HPVA 100 and HPVA 200 have only one sample port Sample ports 2 through 4 are not applicable for these models Manifold Temp Shows the slope and intercept for the linear calibr...

Страница 75: ...nalysis temperature allowed if Bath is selected on the System Step Isotherm window when preparing for an experiment Max Bath Temp Enter the maximum analysis temperature allowed if Bath is selected on...

Страница 76: ...AX task associated with the vent servo valve Multiplier Vacuum Vent Increase this value to increase the speed of the vacuum servo valve decrease it to increase the servo precision Increase this value...

Страница 77: ...ostat is to be used during analyses check this box Port Enter the serial port used to connect the cryostat controller to the computer Bit Rate Enter the speed of the connection between the cryostat co...

Страница 78: ...d to the desired pressure points listed in the System Step Isotherm window and vent the sample after each pressure point the Low and High Pressure Factors will be ignored Selective Adsorption The syst...

Страница 79: ...pressures below this pressure the system will use the vacuum servo or needle valve to reach desired pressures Vent Line Flush Flush if Below If any dose pressure in the isotherm analysis is below thi...

Страница 80: ...ring dosing Below Threshold The dose pressure must be within the value entered here for the system to continue during dosing Temperature Tolerance The sample temperature must be within this value to b...

Страница 81: ...Expand Time During the analysis the system will open valve 1 to dose the sample for this amount of time before closing the valve and waiting for equilibration Dose Pressure The pressure the manifold...

Страница 82: ...ance The temperature tolerance allowed for the ambient and analysis temperatures during the free space analysis this value Evac Expand Evac Time The amount of time the system will evacuate the sample...

Страница 83: ...not obtained Some common opera tional 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...

Страница 84: ...ydrocarbon source then turn the instrument back on Valves will not operate Gas bottle depleted For nitrogen or compressed air the pressure on the gas line is less than 75 psi Replace the gas bottle Re...

Страница 85: ...Configuration window does not match the pressure set on the regulator For example if you are using CO2 or methane the pressure limit must be set below the maximum output of the regulator Enter the cor...

Страница 86: ...Manual 6 4 Mar 2011 Resetting the Pressure Limit 1 Select Configure Hardware from the HPVA main menu 2 Make sure the Instrument tab is selected 3 Enter the maximum pressure for the gas you are using i...

Страница 87: ...e HPVA main menu 2 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 HPVA 200 20 6843 The HPVA 100 and HP...

Страница 88: ...nes 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 tethe...

Страница 89: ...then open the regulator shut off valve Gas Bottle shut off valve Regulator shut off valve 2 Both gauges should read at or near zero if not open the gas inlet valve 3 and the vent valve 2 and allow the...

Страница 90: ...e into the instrument cabinet and return the instrument to a safe condition When using toxic or flammable gases additional venting of the cabinet may be required When connecting hazardous gases be sur...

Страница 91: ...urn the regulator control knob fully counterclockwise b Slowly open the gas bottle shut off valve then close it c Observe the pressure on the high pressure gauge d If the pressure is stable proceed wi...

Страница 92: ...gauge reads 15 psi 1 03 bar b Open the regulator shut off valve c Open the gas bottle shut off valve and flow gas for 10 to 30 seconds d Close the gas bottle shut off valve 5 If you disconnected the g...

Страница 93: ...ng pressure points 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...

Страница 94: ...ves HPVA Series Operator s Manual 6 12 Mar 2011 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...

Страница 95: ...ve 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 10 Adju...

Страница 96: ...e 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 34 2 After observing a ste...

Страница 97: ...sulator 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...

Страница 98: ...Ordering Informatioin HPVA Series Operator s Manual 7 2 Mar 2011...

Страница 99: ...ing from the HPVA System appli cations directory Action Verify that all HPVA System applications and the HPVASys ini file are in the same directory Instrument ini file could not be found path to ini f...

Страница 100: ...mode was properly selected Action B Verify proper installation of the HPVA software and that no additional updates from National Instruments have been installed Action C Verify that the board and ext...

Страница 101: ...missions to the directory in which the HPVA 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 dat...

Страница 102: ...racters 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 l...

Страница 103: ...nter the ambient and analysis free space values previ ously found prior to the adsorption desorption routine When the volumetric calculations are performed by the HPVA Excel macro the mass and density...

Страница 104: ...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 3 Place an isothermal jacket on the stem...

Страница 105: ...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 8 Using two wrenches 3 4 in and 5 8 in tighten t...

Страница 106: ...tion 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 It is important to set...

Страница 107: ...ter 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 liqu...

Страница 108: ...xperiment 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...

Страница 109: ...nto 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 Doing so will cause the free...

Страница 110: ...ct 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 spac...

Страница 111: ...Weigh the sample Refer to Weighing the Sample page 2 4 7 Assemble the sample holder Refer to Assembling the Sample Holder page 2 5 8 Degas the sample to remove any moisture or CO2 from the sample Refe...

Страница 112: ...ing 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...

Страница 113: ...tion Analysis Mar 2011 B 11 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 tig...

Страница 114: ...Manual B 12 Mar 2011 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 Expe...

Страница 115: ...alysis 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 necess...

Страница 116: ...Conducting the Adsorption Desorption Analysis HPVA Series Operator s Manual B 14 Mar 2011 22 Place the dewar cover on top of the dewar 23 Place the strap around the dewar cover and tighten...

Страница 117: ...lapsed the HPVA will begin the analysis 27 When the analysis is complete the results will be available in the Excel HPVA macro as described in the next topic 28 After the analysis has completed close...

Страница 118: ...the dry mass of the sample Enter the mass of the sample after the analysis then click OK 7 You will then be prompted to enter the sample density Enter the sample density then click OK Since the macro...

Страница 119: ...ve 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 9 You can click the isotherm tab to display an isother...

Страница 120: ...Analyzing the Results HPVA Series Operator s Manual B 18 Mar 2011...

Страница 121: ...9 5 2 Connectors rear panel 1 7 sample compartment 1 6 Control Method 2 29 Controls 1 4 Conventions used in manual 1 1 Cryogenic analysis performing B 1 Cryostat Correction 3 4 D Data file 1 10 Data L...

Страница 122: ...alve 2 10 Isotherm displaying 2 23 3 10 L Links 1 1 Long data file 1 10 3 6 Low pressure factor 2 28 M Macro Security 3 1 Main menu 1 9 Maintenance system 6 1 Manifold pressure 1 4 2 23 5 4 RTD 5 4 te...

Страница 123: ...line 3 4 Short data file 1 10 3 6 3 8 3 13 Slope 5 4 6 5 Software starting and stopping 1 10 Specifications 1 11 System Configuration window 5 2 System Experiment Definition window 2 20 T Tasks tab 5...

Страница 124: ...Index HPVA Series Operator s Manual Index 4 Mar 2011...

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