Micromeritics TriStar II 3020 Operator's Manual

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TriStar

II 3020

Operator's Manual

V3.00

302-42828-01

Dec 2013

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Page 1 ® TriStar II 3020 Operator’s Manual V3.00 302-42828-01 Dec 2013...
Page 2 MicroActive is a trademark of Micromeritics Instrument Corporation. © Micromeritics Instrument Corporation 2012-2013. 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...
Page 3 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.
Page 5: Table Of Contents
TriStar II 3020 Table of Contents TABLE OF CONTENTS 1. GENERAL INFORMATION Introduction ..............1-1 Organization of the Operator’s Manual .
Page 6 Table of Contents TriStar II 3020 Opening Sample Information Files..........3-8 Opening Files with a Status of Complete, Analyzing, or Entered .
Page 7 TriStar II 3020 Table of Contents 5. FILE MENU Introduction ..............5-1 Common Fields and Buttons - File Menu Options .
Page 8 Table of Contents TriStar II 3020 6. UNIT MENU Introduction..............6-1 Common Fields and Buttons - Unit Menu Options .
Page 9 TriStar II 3020 Table of Contents t-Plot ..............7-28 BJH Adsorption Cumulative Pore Volume .
Page 10 Table of Contents TriStar II 3020 A. FORMS Sample Data Worksheet ............A-3 B.
Page 11 TriStar II 3020 Table of Contents Control Chart Variables ........... . C-40 Summary Report .
Page 12 Table of Contents TriStar II 3020 Smart VacPrep Operator Manual viii 302-42828-01 - Nov 2013...
Page 13: General Information
Introduction This manual provides details on software installation, program menu options and operating instruc- tions. This chapter contains information on the TriStar II 3020 system hardware and software components. To help you operate the analyzer system more efficiently, refer to: •...
Page 14 Organization of the Operator’s Manual TriStar II 3020 Description (continued) Chapter Chapter 7 REPORTS MENU Provides a description of the Reports menu options and field and button definitions. Chapter 8 OPTIONS MENU Provides a description of the Options menu options and field and button definitions.
Page 15: Conventions
Equipment Description The TriStar II 3020 is an automated gas adsorption analyzer with three ports allowing up to three sam- ples to be analyzed simultaneously. It also features a dedicated port for measuring the saturation pressure (Po) on a continuous basis. Surface areas as low as 0.01 m...
Page 16: Krypton Option
Pumps available from Micromeritics are equipped with an anti-suckback valve. An oil-based or oil-free vacuum pump can be used with the analyzer (an oil-free pump is required if the Krypton option is installed). Appropriate vacuum pumps are available from Micromeritics. Refer INFORMATION, page 10-1.
Page 17: Degasser
The Help menu provides access to the online manual and instructional videos on using the software. The TriStar II 3020 program offers a Windows interface with an easy way to collect, organize, archive and reduce raw data and store sample information files for later use. The reports can be generated to screen, paper, or exported for use in other applications.
Page 18: Specifications
Specifications TriStar II 3020 Specifications The analyzer has been designed and tested to meet the following specifications: Characteristic Specification Pressure Measurement Absolute Range: 0 to 950 mmHg Resolution: Within 0.05 mmHg Accuracy: Within 0.5% Linearity: Within 0.25% of full scale (transducer manufacturer’s specification) Relative range:...
Page 19 TriStar II 3020 Specifications Specification (continued) Characteristic Manifold Temperature Accuracy: ± 0.25 ºC Resolution: Within 0.1 ºC Vacuum System Nitrogen unit: Must accommodate 20 × 10 mmHg or better; uses oil-based or oil- free vacuum pump Krypton unit: Must accommodate 0.1 × 10 mmHg;...
Page 20 Specifications TriStar II 3020 Specification (continued) Characteristic Computer Minimum requirements: • 1 GHz or faster 32 bit (x86) or 64 bit (x64) processor • 2 GB RAM • 40 GB minimum hard drive (formatted in NTFS) (one partition) • Video Adapter capable of 1024 × 768 minimum resolution •...
Page 21: User Interface
TriStar II 3020 Introduction 2. USER INTERFACE Introduction This chapter contains information on the analyzer hardware and software components of the TriStar II 3020. • Shortcuts • File name conventions • Menu Structure Instrument Components and Connectors Front Panel Power Indicator...
Page 22 Instrument Components and Connectors TriStar II 3020 Sample Compartment Three sample ports Saturation pressure (Po) tube Diagram of port locations Elevator Component Description For installing up to three sample tubes. Sample ports For measuring the saturation pressure. Po tube Diagram of port numbers and locations.
Page 23: Rear Panel
TriStar II 3020 Instrument Components and Connectors Rear Panel Analysis inlet valves Vacuum pump connector Maximum Helium inlet valve inlet pressure On/Off switch Power cord connector Component Description • Analysis - inlets V8, V9 and V14 are for analysis gases.
Page 24: Side Panel
Turning the Analyzer On and Off TriStar II 3020 Side Panel Ethernet port RS232 connector Connector Description Port for an Ethernet cable allowing communication between the analyzer Ethernet port and the computer. Used by service personnel to perform calibration procedures.
Page 25: Turning The Analyzer Off
TriStar II 3020 Using the Software Turning the Analyzer Off Always exit the analysis program before turning off the computer. Failure to do so could result in loss of data. It is recommended that the analyzer be powered on at all times. If it does become necessary to turn it off, perform the following steps: Select File >...
Page 26: Shortcut Keys
Using the Software TriStar II 3020 Shortcut Keys Shortcut keys can be used to activate some menu commands. Shortcut keys or key combinations (when applicable) are listed to the right of the menu item. Another shortcut method of accessing a menu or function is to use the Alt key plus the underlined let- ter in the menu command.
Page 27: Files
TriStar II 3020 Using the Software Function (continued) Shortcut Key(s) Start a report Close all open reports Generate a Heat of Adsorption report Exit the application Alt + F4 List sample information files Shift + F2 List analysis conditions files...
Page 28: File Name Conventions
For sample information files, a default file name (the next available sequence number) and a default extension display. For Sample tube, Degas conditions, Analysis conditions, Adsorptive properties and Report options, only a default extension displays. The following table lists the default file extensions assigned to files in the TriStar II 3020 application: File Type Default File Name Extension .SMP...
Page 29: Menu Structure
TriStar II 3020 Using the Software Menu Structure All application functions are located on menus accessed from the menu bar. Each menu contains com- mands and, in some cases, a submenu. A submenu is indicated when the command is followed by an arrow.
Page 30: Window Menu
Use to arrange the windows on the computer screen and display a list of Window open windows. Refer to Menu, page 2-10. Window Use to access the online operator’s manual, Micromeritics web page, and Help videos. Refer to Menu, page 2-11. Help Window Menu The Window menu lists open files and provides the ability to rearrange the way open windows display.
Page 31: Help Menu
TriStar II 3020 Using the Software Help Menu The Help menu provides access to the online operator’s manual, the Micromeritics web page, online instructional videos, and information about the analyzer. Help Menu Option Description Provides access to the online operator’s manual.
Page 32 Using the Software TriStar II 3020 2-12 302-42828-01 - Dec 2012...
Page 33: Operating Procedures
TriStar II 3020 Introduction 3. OPERATING PROCEDURES Introduction This chapter contains information on: • specifying sample defaults • creating sample files in Advanced, Basic and Restricted formats • preparing samples and performing an analysis • printing file contents, listing file statistics, exporting isotherm data, and converting sample files •...
Page 34: Advanced Format
Specifying Sample Defaults TriStar II 3020 Advanced Format The values specified in the parameter portions of the default sample file (Sample Tube, Degas Condi- tions, Analysis Conditions, Adsorptive Properties, and Report Options) are saved as the defaults for new sample files. To navigate from one set of parameters to another, click the parameter tab at the top of the window.
Page 35: Basic Format
TriStar II 3020 Specifying Sample Defaults Enter Operator, Submitter and Bar Code identification information in the respective text boxes. To omit the field and information in the sample files, select the Omit checkbox to the right of the field. The labels for the Sample, Operator, Submitter and Bar Code fields can be modified by overwriting the default field labels.
Page 36 Specifying Sample Defaults TriStar II 3020 Go to Options > Sample Defaults. In the Sequence Number alpha/numeric text box, specify a default file name string. The Sequence Number field must contain a minimum of three (3) numbers. This number is incrementally sequenced and displays in the File name text box in the File >...
Page 37: Restricted Format
TriStar II 3020 Specifying Sample Defaults Restricted Format Restricted format presents the sample information file in the same manner as the Basic format except that the operator cannot switch to Advanced format. This format is password protected and is typically used in laboratories where sample parameters must remain constant, for example, in pharmaceutical laboratories.
Page 38: Defining Sample Information Files
Defining Sample Information Files TriStar II 3020 Defining Sample Information Files A sample information file must be created for each analysis. This file can be created in advance or at the time of analysis. The sample information file identifies the sample, guides the analysis, and speci- fies report options.
Page 39: Basic Or Restricted Format
TriStar II 3020 Defining Sample Information Files If SPC (Statistical Process Control) information is to be reported, enter appropriate information in the User Parameters group box. These are user-definable parameters that can be entered and tracked along with other statistical process control data.
Page 40: Opening Sample Information Files
Defining Sample Information Files TriStar II 3020 In the Sample field, enter a sample description. In the Mass group box, choose whether to enter mass manually or to have the system automatically calculate mass. Enter a value for sample mass and/or density. Refer to Sample Files, page 5-8.
Page 41: Opening Files With A Status Of Preparing, Prepared, Or No Analysis
TriStar II 3020 Defining Sample Information Files Opening Files with a Status of Preparing, Prepared, or No Analysis Select File > Open > Sample Information. To sort the file list by status, click the Mic Status column header. Select the file to open in the Name column and click Open (or double click the file name).
Page 42: Defining Parameter Files
Defining Parameter Files TriStar II 3020 Defining Parameter Files The following file types can exist as part of the sample information file as well as individual parameter files: • Sample tube • Degas conditions • Analysis conditions • Adsorptive properties •...
Page 43: Sample Tube
TriStar II 3020 Defining Parameter Files Sample Tube Prior to creating the Sample Tube file, perform a blank analysis using the default sample tube. The data obtained from this analysis will be used in the Sample Tube file. Refer to...
Page 44: Degas Conditions
Defining Parameter Files TriStar II 3020 Degas Conditions Degassing is a required step in preparation for the analysis; however, this section is only applicable if using the SmartPrep Degasser. This section contains degassing instructions that will be sent to the SmartPrep Degasser equipment.
Page 45: Analysis Conditions
TriStar II 3020 Defining Parameter Files Analysis Conditions Analysis conditions specify the data used to guide an analysis. Go to File > Open > Analysis Conditions or use the F3 keyboard shortcut. Enter a name in the File name text box. Click Open.
Page 46: Adsorptive Properties
Defining Parameter Files TriStar II 3020 Adsorptive Properties Adsorptive properties provide the adsorptive (analysis gas) characteristics for the analysis. Go to File > Open > Adsorptive Properties or use the F4 keyboard shortcut. Enter a name in the File name text box. Click Open.
Page 47: Report Options
TriStar II 3020 Defining Parameter Files Select the Non-condensing Adsorptive checkbox if this file is to be used for a non-condensing gas. Enter information in the following text boxes: • Maximum manifold pressure • Non-ideality factor • Density conversion factor •...
Page 48 Defining Parameter Files TriStar II 3020 Click OK to create the file. Enter a description in the Description text box. Select Show report title and enter a title to appear on the report header. Deselect this option to omit a report title.
Page 49: Preparing For Analysis
Sample tubes and filler rods must be clean and dry before samples are added and weighed. The follow- ing table indicates which materials are supplied by Micromeritics and which are supplied by the user. The procedures following the table are recommended.
Page 50 Preparing for Analysis TriStar II 3020 Fill the sample tubes with warm water and place them in the ultrasonic cleaning unit. Then place the filler rods in the unit. Turn on the ultrasonic cleaning unit for approximately fifteen minutes. Use rubber gloves to ensure no oils or residue are transferred to the clean tubes and filler rods and remove the sample tubes and filler rods from the unit.
Page 51: Determining The Sample Mass
TriStar II 3020 Preparing for Analysis Remove the sample tubes and filler rods from the oven and allow to cool. Do not insert the filler rods at this time. Filler rods are inserted just before the sample tube is installed on the analysis port.
Page 52 Preparing for Analysis TriStar II 3020 Place the sample tube set on the sample weighing support and place it on the balance. Record the stabilized weight on the Sample Data Worksheet as [A] Mass for empty sample tube set. Remove the sample weighing support and sample tube set from the balance.
Page 53: Degassing The Sample
[C] Sample mass (Before Degas). Degassing the Sample After the sample has been weighed, use a degassing unit to remove any contaminants which may have adsorbed to the surface or pores. Appropriate degassing units are available from Micromeritics. Refer INFORMATION, page 10-1. ORDERING If using the SmartPrep degasser, a menu displays on the program menu bar.
Page 54: Installing The Analysis Dewar
Preparing for Analysis TriStar II 3020 Insert the Po tube into the center hole of the Dewar cover and slide the cover up. Ensure the tapered side of the cover is facing downward. Insert the sample tube through one of the holes in the cover.
Page 55 TriStar II 3020 Preparing for Analysis For glass Dewars: • Use a plastic stirring rod when stirring substances in a Dewar containing liquefied gases (or other materials of extremely low temperature). Do not use a glass or metal stirring rod unless it has a protective coating.
Page 56: Performing An Analysis
Performing an Analysis TriStar II 3020 For best results, if the Dewar has not been used for a while, allow approximately 30 minutes for the temperature of the Dewar to stabilize with the bath liquid. Then recheck the level of the bath liquid.
Page 57: Sample Analysis
TriStar II 3020 Performing an Analysis Sample Analysis Select Unit [n] > Sample Analysis. To manually close all instrument valves, click the Close Valves button Click Browse and select a sample information file for each port to be used. Verify the information populated into the sample identification, density and mass fields. This information is pulled from the selected file.
Page 58: Quickstart Analysis
Performing an Analysis TriStar II 3020 QuickStart Analysis When using the QuickStart option, it is not necessary to prepare sample files in advance. Sample files are assigned automatically and given default conditions. File contents can be replaced if necessary using the Browse button.
Page 59: Krypton Analysis
TriStar II 3020 Performing an Analysis When the analysis is complete, remove the sample tube and store (or dispose) of the sample material as applicable. Use caution when removing the sample tube if using a hanging filler rod. The sample tube O-ring or Dewar cover may snag the filler rod retaining ring.
Page 60: Blank Analysis
Performing an Analysis TriStar II 3020 Blank Analysis Use this method to perform a blank analysis with no sample data. The blank analysis is used primarily for diagnostic purposes to look for instrument problems. The blank analysis should result in zero adsorptive.
Page 61: Generating Reports
TriStar II 3020 Generating Reports Generating Reports Reports > Start Report > [file] (or use the F8 keyboard shortcut) Select the report in the Name column. The selected report name appears in the File name text box. To select more than one file, hold down the Ctrl key on the keyboard while selecting the files.
Page 62 Generating Reports TriStar II 3020 Click a tab across the top of the window to review each report. 3-30 302-42828-01 - Dec 2012...
Page 63: Printing Files
TriStar II 3020 Printing Files Printing Files Provides the option to print the contents of one or more sample files to either the screen, a printer, or to a file. Go to File > Print > [file type] > [file].
Page 64: Listing Files
Listing Files TriStar II 3020 Click Print. The following example shows a sample information file printed to the screen. Listing Files Provides the option to create a list of sample file information, for example, file name, date / time the file was created or last edited, file identification and file status.
Page 65: Exporting Isotherm Data
TriStar II 3020 Exporting Isotherm Data In the Report Settings window, select one of the following: • Preview - to send the file to the screen. • Print - to send the file to the default printer. • Copies - select the number of copies to print. This field is only enabled when Print is selected.
Page 66: Format Of Exported Data
Exporting Isotherm Data TriStar II 3020 Format of Exported Data The output file consists of five columns containing elapsed time during analysis, absolute pressure, rel- ative pressure, quantity adsorbed, and quantity dosed. Description Operator Submitter Sample Mass * Type of Data...
Page 67: Converting Files
TriStar II 3020 Converting Files In the Export Settings window, select one of the following: • Preview - to send the file to the screen. • Print - to send the file to the default printer. • Copies - select the number of copies to print. This field is only enabled when Print is selected.
Page 68 Converting Files TriStar II 3020 Click Open. The file is automatically converted to a .SMP file and the following window displays. Click OK to close the window. 3-36 302-42828-01 - Dec 2012...
Page 69: Generating Graph Overlays
TriStar II 3020 Generating Graph Overlays Generating Graph Overlays Use the graph overlay function to compare multiple graph options. Graphical lines are differentiated by the use of varying colored symbols outlined on a legend. Overlays may be generated in two ways: •...
Page 70 Generating Graph Overlays TriStar II 3020 If overlaying this type of Then... report... a.) In the Selected Reports list box, highlight Isotherm and click Edit. b.) On the Isotherm Report Options window, select a plot in • Isotherm the Selected Reports group box then click the Options button to the right of the selected plot.
Page 71 TriStar II 3020 Generating Graph Overlays On the Report Options tab, click the Overlays button. Click Browse to the right of the Sample [n] field. Select the file containing the graph to overlay and click Open. After selecting up to eight files, click OK to return to the Report Options tab.
Page 72 Generating Graph Overlays TriStar II 3020 10. The report screen displays with tabs across the top of the screen. Click each tab to view the reports. 3-40 302-42828-01 - Dec 2012...
Page 73: Multiple Graph Overlays
TriStar II 3020 Generating Graph Overlays Multiple Graph Overlays Multiple graph overlays can only be generated for: • BJH Adsorption • BJH Desorption • DFT Pore Size • DFT Surface Energy • Dollimore-Heal Adsorption • Dollimore-Heal Desorption • Horvath-Kawazoe • MP-Method...
Page 74 Generating Graph Overlays TriStar II 3020 From the Report Options window, in the Selected Reports list box, select a sub-report and click Edit. Select the report variable Click Edit Click the dropdown arrow on the Overlay field and select a second variable to overlay. Click OK to return to the Report Options window.
Page 75 TriStar II 3020 Generating Graph Overlays Select Reports > Start Report. Select the file created in the previous steps and click Open. To select more than one file, hold down the Ctrl key on the keyboard while selecting the files.
Page 76 Generating Graph Overlays TriStar II 3020 3-44 302-42828-01 - Dec 2012...
Page 77: Software And Setup Modifications
This allows: • the creation or editing of sample and parameter files • the generation of reports on completed sample files Review the Micromeritics PROGRAM License Agreement for restrictions on the use of another copy of the analysis program. ...
Page 78: Installing The Software
Installing the Software TriStar II 3020 Installing the Software The following prerequisites must be completed prior to installing the software: • Configure an Ethernet port on the computer to communicate with the analyzer. Refer to CONFIGURATION, page D-1. ETHERNET • Attach the analyzer to the computer’s configured Ethernet port and turn on the power to the analyzer.
Page 79 TriStar II 3020 Installing the Software On the Ethernet Introduction screen, verify that all prerequisites have been met. If not, click Cancel and complete the steps, then restart the installation program. Do not proceed with installation until these tasks have been completed. If the prerequisites have been met, click Next.
Page 80 Installing the Software TriStar II 3020 On the Choose Install Location screen, verify that enough disk space is available to continue the installation. If not, click Cancel and free up the minimum required disk space. If the disk space is OK, click Next to accept the default installation directory or click Browse to change the installation location, then click Next.
Page 81 TriStar II 3020 Installing the Software When installation completes, the TriStar II 3020 Installed screen displays. Click Next. The Analyzer Configuration screen is used to configure the system for each analyzer and serial number to be installed. In the Step 1 group box: If...
Page 82 Installing the Software TriStar II 3020 a.) In the Step 2 group box, enter the serial number for each analyzer to be attached to this computer. The analyzer’s serial number label is located near the power switch. b.) Click Next On the Ethernet Ports screen, select one option from the following table If...
Page 83 TriStar II 3020 Installing the Software 10. The Calibration File Installation screen displays. Calibration files are located on a separate calibration CD. Replace the setup CD with the calibration CD and browse to the calib directory. To prevent the CD from AutoPlay, press and hold down the Shift key before closing the CD door.
Page 84 Installing the Software TriStar II 3020 12. If installing a SmartPrep at this time, on the Configure SmartPrep screen, select the number of SmartPrep instruments to be installed and the Com Port connected to the first SmartPrep. Click Next. If not installing the SmartPrep, select None for step 1 and click Next.
Page 85 14. The Product Registration screen displays. Click the appropriate link to register the product or to log into your portal or click Next to register later. 15. The Completing the TriStar II 3020 Setup screen displays. Select one of the following: • Reboot now •...
Page 86: Starting The Setup Program
Installing the Software TriStar II 3020 Starting the Setup Program To start the setup program: Ensure that the analysis program is not operating and the analyzer is idle. Insert the setup CD into the CD-ROM drive. The setup program starts automatically.
Page 87: Installing Software Updates Or Reverting To A Previous Version
TriStar II 3020 Installing the Software Installing Software Updates or Reverting to a Previous Version When performing a software update, existing data files are not overwritten. There are three types of subsequent installations: • a later version than the current installation •...
Page 88 Micromeritics representative before proceeding. Reverting to a previous version can damage existing sample files. The TriStar II 3020 Installed screen displays. Click Next. The TriStar II 3020 Reinstalled screen displays. Select one of the following: • Reboot now • I want to manually reboot later...
Page 89: Adding An Analyzer
TriStar II 3020 Installing the Software Select the Create a desktop icon checkbox to have the system install a program shortcut onto the desktop. Click Finish. Adding an Analyzer An Ethernet switch is required when connecting multiple analyzers. After connecting the Ethernet switch, continue with the Software, page section.
Page 90: Software
Installing the Software TriStar II 3020 Software Start the setup program. The Welcome screen displays. Click Next. On the Select Task screen, select Add an analyzer. Click Next. 4-14 302-42828-01 - Dec 2012...
Page 91 TriStar II 3020 Installing the Software On the Add Analyzer screen, enter the serial number of the analyzer being added. Click Next. The Calibration File Installation screen displays. Calibration files are located on a separate calibration CD. Replace the setup CD with the calibration CD and browse to the calib directory.
Page 92 Installing the Software TriStar II 3020 The Analyzer S/N [n] Installed screen indicates a successful install. Click Next. The Analyzer Added screen displays. Click Finish. 4-16 302-42828-01 - Dec 2012...
Page 93: Moving An Analyzer From One Pc To Another Pc
TriStar II 3020 Installing the Software Moving an Analyzer from One PC to Another PC This section provides instructions on moving a configured analyzer (along with its status, calibration, and log files) from one computer (Source PC) to a another (Destination PC). This operation does not move sample or parameter files.
Page 94 Installing the Software TriStar II 3020 On the Move Analyzer screen, use the dropdown list to select the source analyzer to be moved. Click Next. On the new Move Analyzer screen, select the new destination for the analyzer to be moved. This location is where the Analyzer SN [n] Installer.exe file will be located.
Page 95 TriStar II 3020 Installing the Software The Analyzer Installer Created screen displays. Click Finish. a.) Remove the CD from the CD-ROM drive and store in a safe location. b.) Disconnect the Ethernet cable from the Source computer and reconnect it to the configured Ethernet port on the Destination computer.
Page 96: Removing An Analyzer
Installing the Software TriStar II 3020 On the Analyzer Installed screen, click Finish. Sample and parameter files are not copied and moved with the analyzer. Use a file management program such as Explorer or a backup/restore utility to move these ...
Page 97 TriStar II 3020 Installing the Software On the Select Task screen, select Remove an analyzer. Click Next. On the Remove Analyzer screen, from the dropdown list, select the unit and serial number of the analyzer to be removed. Click Next.
Page 98: Changing Analyzer Setup
Installing the Software TriStar II 3020 The Analyzer Removed screen displays. Click Finish. Changing Analyzer Setup This section provides instructions on how to change an analyzer’s Ethernet port in case of an Ethernet port malfunction. Ensure that the new Ethernet port has been configured.
Page 99 TriStar II 3020 Installing the Software On the Select Task screen, select Change analyzer setup. Click Next. On the Ethernet Ports screen, select one option from the following table: If... Then... the configured port is listed Select the port then click Next to proceed to the next step.
Page 100: Reinstalling Calibration Files For An Analyzer
Installing the Software TriStar II 3020 On the Analyzer Configuration Updated screen, click Finish. Reinstalling Calibration Files for an Analyzer Calibration files specific to the analyzer are contained on the original calibration CD only and not on an update CD.
Page 101 TriStar II 3020 Installing the Software On the Select Task screen, select Reinstall calibration files for an analyzer. Click Next. On the Reinstall Calibration Files screen, select the unit and serial number from the dropdown list. Click Next. 302-42828-01 - Dec 2012...
Page 102 Installing the Software TriStar II 3020 The Calibration Files Installation screen displays. Calibration files are located on a separate calibration CD. Replace the setup CD with the calibration CD and browse to the calib directory. To prevent the CD from AutoPlay, press and hold down the Shift key before closing the CD door.
Page 103: Importing An Analyzer From A Previous Installation On This Pc
TriStar II 3020 Installing the Software On the Analyzer Calibration Reinstalled screen, click Finish. Importing an Analyzer from a Previous Installation on this PC This section provides instructions on importing an analyzer from a previous installation on the same Start the setup program. On the Welcome screen, click Next.
Page 104 Installing the Software TriStar II 3020 On the Select Task screen, select Import an analyzer from a previous installation on this PC. Click Next. On the Import Analyzer screen, click the Browse button to locate the installation directory of the previously installed instrument, then select the serial number of the instrument files to be imported.
Page 105 TriStar II 3020 Installing the Software When the previously installed files have been imported, the Analyzer SN [n] Installed screen displays. Click Next. On the Analyzer Added screen, click Finish. 302-42828-01 - Dec 2012 4-29...
Page 106: Adding Or Modifying Smartprep
Installing the Software TriStar II 3020 Adding or Modifying SmartPrep This section provides instructions on how to configure the software to connect up to four SmartPrep instruments. Start the setup program. On the Welcome screen, click Next. On the Select Task screen, select Add or Modify SmartPrep. Click Next.
Page 107 On the Configure SmartPrep screen, select the number of SmartPrep units to be installed and the Com Port for the first SmartPrep unit. Click Next. On the Completing the TriStar II 3020 Setup screen, to place a shortcut icon on the desktop, select the Create a desktop icon checkbox. Click Finish to complete the process.
Page 108: Uninstalling The Analysis Program
This section provides instructions on uninstalling the analysis program, status files, analyzer setup files and resulting empty directories. It does not remove data files. Double-click the uninstall.exe file located in the directory where the TriStar II 3020 files are installed.
Page 109 TriStar II 3020 Uninstalling the Analysis Program The Completing the TriStar II 3020 Uninstall screen displays. Click Finish to close the setup program. 302-42828-01 - Dec 2012 4-33...
Page 110 Uninstalling the Analysis Program TriStar II 3020 4-34 302-42828-01 - Dec 2012...
Page 111: File Menu
TriStar II 3020 Introduction 5. FILE MENU Introduction This chapter contains information specific to the File menu options used to manage sample and param- eter files. This chapter provides details of File menu options, commonly used functions and buttons, and field descriptions.
Page 112 Common Fields and Buttons - File Menu Options TriStar II 3020 Description (continued) Field or Button Browse button Click to search for a file. Select from a file in the Name column and click Open or double click the file name in the Name column to open (or import) the file.
Page 113 TriStar II 3020 Common Fields and Buttons - File Menu Options Description (continued) Field or Button From / To text boxes When working with report parameters screens, enter the From and To range for autoscaling the X- and/or Y-axes. Name column A list of files in the selected directory.
Page 114: Open
Open TriStar II 3020 Open Opens a sample file or a parameter file. • Sample Information files - the File name text box contains the next sequential file name generated by the program. The sample information file extension is .SMP.
Page 115: Save As
TriStar II 3020 Save As Save As Saves the active window as another file type or file name. • Saves a file in the active window under a different file name. • Saves a subset (parameter) of the sample file in the active window as a standalone parameter file, for example, select Analysis Conditions from the Save As menu to create a standalone parameter file of the analysis conditions portion of the active sample file.
Page 116: Save All
Save All TriStar II 3020 Save All Saves all active windows under the current file names. Close Closes the active window. If changes were made and not yet saved, a prompt displays providing the option to save the file. Close All Closes all active windows.
Page 117: Convert
TriStar II 3020 Convert Convert Converts the following sample file types to be compatible with the TriStar II 3020 application: File Type File Name Convention SIcarbon.DAT ASAP 2000 SMcarbon.DAT ASAP 2000 Micropore SIcarbon.DAT ASAP 2400 SKcarbon.DAT ASAP 2405 carbon.MGD StarDriver NOTE: Substitute the word carbon (shown above) for the actual filename.
Page 118: Sample Information Files
Sample Information Files TriStar II 3020 Sample Information Files File > Open > Sample Information (or use the F2 keyboard shortcut) Each analysis must be linked with a sample information file before the analysis can proceed. A sample information file can consist of multiple parameter files; however, parameter files can also stand alone.
Page 119 TriStar II 3020 Sample Information Files Description (continued) Field or Button Bar Code text box Enter bar code reader information if a bar code reader is connected to the computer’s USB port. If a bar code reader is not used, this alpha/numeric field can be used to enter additional information about the sample;...
Page 120: Sample Tube Files
Sample Tube Files TriStar II 3020 Description (continued) Field or Button Close button Preview button Refer to Options, page 5-1. Common Fields and Buttons - File Menu Save button Sample Tube Files File > Open > Sample Tube (or click the Sample Tube tab when in Advanced format) The Sample Tube tab provides details for setting up the default settings for a Sample Tube parameter file.
Page 121: Degas Conditions File
TriStar II 3020 Degas Conditions File Description (continued) Field or Button  Use isothermal Select if an isothermal jacket is to be used. An isothermal jacket maintains jacket checkbox a constant temperature profile along the sample tube stem during an extended analysis of more than 1 or 2 hours.
Page 122: Analysis Conditions Files
Analysis Conditions Files TriStar II 3020 Description (continued) Field or Button Conditions table Enter up to five stages of degas conditions. Available columns are: • Temperature - soaking temperature with flowing gas. • Temperature Ramp Rate - rate at which the temperature is to change when advancing to the soak temperature.
Page 123 TriStar II 3020 Analysis Conditions Files Description (continued) Field or Button Absolute pressure Select to specify pressure targets in mmHg, mbar, or kPa rather than relative dosing checkbox pressure. This option is typically selected when using adsorptives at analysis conditions above the critical point of the gas; for example, H adsorption on carbon at liquid nitrogen temperature.
Page 124 Analysis Conditions Files TriStar II 3020 Description (continued) Field or Button Target Pressures Several analysis conditions files containing complete pressure tables are included with the analysis program. When using these files, it is option (continued) recommended to use the File > Save As option to save the file as a different name and edit the new file.
Page 125 TriStar II 3020 Analysis Conditions Files Description (continued) Field or Button Target Pressures Geometric towards saturation - select to insert geometrically spaced points from the saturation pressure. For example, to insert 5 points with option (continued) a 0.99 starting pressure and a 0.84 ending pressure, the following points are inserted into the table: 0.99...
Page 126 Analysis Conditions Files TriStar II 3020 Description (continued) Field or Button Target Pressures Options button • First Pressure Fixed Dose - Select this option to have the sample dosed with a specified amount of gas until the first pressure point is reached. This initial dosing quickly meets the adsorptive demand of the sample.
Page 127 TriStar II 3020 Analysis Conditions Files Description (continued) Field or Button Target Pressures • Absolute / Relative pressure tolerance - values used to determine how Options button close the actual pressure must be to each target pressure from the pressure table. At lower pressures, the relative tolerance value is lower.
Page 128 Analysis Conditions Files TriStar II 3020 Description (continued) Field or Button Dose Increments • Insert button - option (continued) Ending pressure - enter the ending pressure of this segment. Dose increment - select to have the sample dosed with a specified amount of gas for each isotherm point taken.
Page 129 TriStar II 3020 Analysis Conditions Files Description (continued) Field or Button Preparation • Evacuation rate / Unrestricted evac. from - enter the evacuation rate and the pressure at which unrestricted sample evacuation is to begin. button (continued) The option is enabled when Fast evacuation is not selected.
Page 130 Analysis Conditions Files TriStar II 3020 Description (continued) Field or Button Free Space button • Measure - select to measure the free space automatically over the sample prior to data collection. (continued) Lower Dewar for evacuation - lowers the Dewar during evacuation.
Page 131 TriStar II 3020 Analysis Conditions Files Description (continued) Field or Button pº and T button Options and descriptions: (continued) 1. Analysis bath temperature (not used for krypton analyses). Measures the p on a continuous basis. Allows the measurement of each data point without slowing the analysis.
Page 132 Analysis Conditions Files TriStar II 3020 Description (continued) Field or Button Equilibration button Click to enter values for relative or absolute pressure. Column heading reads Absolute Pressure (mmHg) when Absolute Pressure Dosing is selected Does not display when Absolute Pressure Dosing is selected.
Page 133 TriStar II 3020 Analysis Conditions Files Description (continued) Field or Button Backfill button Click to enter options for backfilling the sample tube. Indicate if the sample should be backfilled at the start and/or end of the analysis. Click the dropdown arrow and select the backfill gas to be used.
Page 134: Adsorptive Properties File
Adsorptive Properties File TriStar II 3020 Adsorptive Properties File File > Open > Adsorptive Properties (or click the Adsorptive Properties tab when in Advanced for- mat or use the F4 keyboard shortcut) The Adsorptive Properties window is used to specify the characteristics of the gases used during an analysis.
Page 135 TriStar II 3020 Adsorptive Properties File Field or Button Description (continued)  Non-condensing Select if using a non-condensing gas (adsorptive). The Absolute pressure Adsorptive checkbox dosing option on the Analysis Conditions tab must also be selected when Non-condensing Adsorptive is selected on this window.
Page 136: Report Options Files
Report Options Files TriStar II 3020 Report Options Files File > Open > Report Options [file] Use to specify report options for collected (from an analysis) or manually entered data. They also help in customizing report details such as axis scale, axis range, column headings, and components of thick- ness curve equations.
Page 137 TriStar II 3020 Report Options Files Description (continued) Field or Button Apply thermal Select to correct the temperature-induced pressure difference between the transpiration manifold and the chilled sample tube. This option is most significant for correction checkbox pressures less than approximately 1.0 mmHg. Do not use filler rods in the sample tube when applying correction for thermal transpiration.
Page 138: Summary Report
Report Options Files TriStar II 3020 Summary Report The Summary Report provides a condensed listing of selected data results. In the Selected Reports list box, highlight Summary, then click Edit. Select the data types to include in the Summary report.
Page 139 TriStar II 3020 Report Options Files Description (continued) Field or Button  Select All / • Pass/Fail [n] button - select the S A: Single-point BET checkbox to Deselect All buttons enable this button. Click the Pass/Fail [n] button to display the Pass/ Fail Options window for selection of pass/fail criteria.
Page 140: Isotherm Report Options
Report Options Files TriStar II 3020 Isotherm Report Options The Isotherm report indicates adsorption (up to saturation pressure) and desorption (down from satu- ration pressure) of a gas by a solid held at constant temperature. In the Selected Reports list box, highlight Isotherm, then click Edit.
Page 141 TriStar II 3020 Report Options Files Description (continued) Field or Button Options buttons • Autoscale X-axis - linear X-axes begin at zero. Logarithmic X-axes begin at an appropriate value. The X-axis field shows the relative or (continued) absolute pressure. • Autoscale Y-axis - Y-axes begin at zero. The Y-axis field shows the quantity of gas adsorbed.
Page 142: Bet/Langmuir Surface Area Report Options
Report Options Files TriStar II 3020 BET/Langmuir Surface Area Report Options The Langmuir and BET Surface Area windows are identical unless otherwise specified. In the Selected Reports list box, highlight BET (or Langmuir), then click Edit. • The BET calculation obtains the sample surface area value by determining the monolayer volume of adsorbed gas from the isotherm data.
Page 143 TriStar II 3020 Report Options Files Description (continued) Field or Button Pressures button Click to enter a range of pressure points or to modify table values for pressure points. If Use calculation assignments is not selected on the Analysis Conditions window, the isotherm is interpolated to these pressure points.
Page 144 Report Options Files TriStar II 3020 Description (continued) Field or Button  BET (or Langmuir) Select to generate a traditional BET (Langmuir) surface area plot used to Transform plot determine monolayer volume and BET C constant. • X-axis - linear X-axes begin at zero. The X-axis field shows the relative pressure for BET and show absolute pressure for Langmuir.
Page 145: Freundlich Report Options
TriStar II 3020 Report Options Files Freundlich Report Options The Freundlich Isotherm is an empirical isotherm used to model low-pressure adsorption data. It can also be applied to model some micropore isotherms. In the Selected Reports list box, highlight Freundlich, then click Edit.
Page 146: Temkin Isotherm Report Options
Report Options Files TriStar II 3020 Description (continued) Field or Button Freundlich Isotherm Plots the absolute pressure vs quantity adsorbed. Shows best fit line. plot checkbox • X-axis - linear X-axes begin at zero. The X-axis field shows the absolute pressure.
Page 147 TriStar II 3020 Report Options Files Description (continued) Field or Button  Absolute pressure Enter a pressure range when calculation assignments are not used. range text boxes Transform plot Plots a linear form of the Temkin isotherm. checkbox • X-axis - the X-axis field shows the logarithm of pressure (ln).
Page 148: T-Plot Report Options
Report Options Files TriStar II 3020 t-Plot Report Options The t-Plot calculation allows quantitative analysis of the area and total volume ascribed to micropores. Matrix area (the area external to micropores) is directly determined and often proves to be a valuable way of characterizing complex mixed materials.
Page 149 TriStar II 3020 Report Options Files Description (continued) Field or Button  Thickness Curve group box (continued) To import values from an existing thickness curve (.THK file), click Open and select the file containing the values. The table to be imported must be saved as ASCII text with a .THK extension.
Page 150 Report Options Files TriStar II 3020 Description (continued) Field or Button Pressure Range button Click to enter minimum and maximum relative pressures. If Use calculation assignments is not selected on the Analysis Conditions window, all of the non-outlier points of the collected data within the specified range are used for calculating the data for this report.
Page 151: Alpha-S Method
TriStar II 3020 Report Options Files Alpha-S Method The Alpha-S plot converts the standard adsorption isotherm into a dimensionless isotherm using the quantity adsorbed at a relative pressure of 0.4. In the Selected Reports list box, highlight Alpha-S Method, then click Edit.
Page 152: F-Ratio Method
Report Options Files TriStar II 3020 Description (continued) Field or Button  Alpha-S plot Select to plot data in graph format. checkbox • X-axis - the X-axis field shows the relative pressure. • Y-axis - the Y-axis field shows the quantity of gas adsorbed.
Page 153 TriStar II 3020 Report Options Files Field or Button Description Reference isotherm Click Browse to select a sample file to use as a reference for the isotherm. Select a file containing an isotherm measured from a non-porous sample of the same material as the current sample. When the referenced file is selected, the file name appears to the left of the Browse button.
Page 154: Bjh Adsorption/Desorption Report Options
Report Options Files TriStar II 3020 BJH Adsorption/Desorption Report Options The BJH calculation determines the mesopore volume/area distribution which accounts for both the change in adsorbate layer thickness and the liquid condensed in pore cores. Reports can be generated from both adsorption and desorption data.
Page 155 TriStar II 3020 Report Options Files Description (continued) Field or Button  Fraction of pores During adsorption calculations, the analysis program assumes that all open at both ends text pores are closed at one end. Occasionally, a percentage of pores may be open at both ends causing disagreement in the adsorption and desorption data or in the values for total volume and total BJH pore volume.
Page 156: Tabular Report Options
Report Options Files TriStar II 3020 Description (continued) Field or Button Pressure Range button Click to enter minimum and maximum relative pressures. If Use calculation assignments is not selected on the Analysis Conditions window, all of the non-outlier points of the collected data within the specified range are used for calculating the data for this report.
Page 157 TriStar II 3020 Report Options Files Description (continued) Field or Button Columns button Click the dropdown arrow and select the data types to include in the report. These selections indicate the column order and data contents for the report. Table button The fixed pore size table must contain a minimum of two points.
Page 158: Plot Options
Report Options Files TriStar II 3020 Plot Options The fields for all plot options are identical for specifying plotting methods and customizing plots. Highlight any plot option in the Selected Reports list box and click Edit. Field or Button Description ...
Page 159: Dollimore-Heal Adsorption/Desorption Report Options
TriStar II 3020 Report Options Files Dollimore-Heal Adsorption/Desorption Report Options This report option generates Dollimore-Heal reports from both adsorption and desorption data. In the Selected Reports list box, highlight Dollimore-Heal Adsorption (or Dollimore-Heal Desorption), then click Edit. Dollimore-Heal Adsorption/Desorption fields and buttons are identical to the BJH Adsorption/ Options, page 5-44.
Page 160 Report Options Files TriStar II 3020 Horvath-Kawazoe Report Options The Horvath-Kawazoe method plots individual peaks for different pore sizes even if the difference between one pore size and the next is only one Angstrom (0.10 nm) or less. In the Selected Reports list box, highlight Horvath-Kawazoe, then click Edit.
Page 161 TriStar II 3020 Report Options Files Description (continued) Field or Button Properties button Click to view or edit the constants describing the physical properties of the adsorbent and adsorptive. These options are disabled if Entered is selected in the Interaction Parameter group box.
Page 162 Report Options Files TriStar II 3020 Description (continued) Field or Button Properties button • Diameter at zero energy - enter the diameter of an atom at zero (continued) interaction energy: (2/5) × diameter. • Polarizability - enter the polarizability of the adsorbent (or adsorptive).
Page 163: Tabular Report Options
TriStar II 3020 Report Options Files Tabular Report Options Highlight H-K Tabular Report in the Selected Reports list box and click Edit. To customize the order and data contents of reports, click the dropdown arrow for a column, and select the data type for that column.
Page 164: Dft Pore Size Report Options
Report Options Files TriStar II 3020 Description (continued) Field or Button X-Axis / Y-Axis • X-Axis - the X-axis field shows pore radius or diameter in angstroms or nanometers. • Y-Axis - the Y-axis field shows the quantity of gas adsorbed.
Page 165 TriStar II 3020 Report Options Files Field or Button Description Type dropdown list Click the dropdown arrow to specify either: • DFT - model based on the density functional theory. • Classical - model based on the Kelvin equation and thickness for determining the pore size distribution.
Page 166 Report Options Files TriStar II 3020 Description (continued) Field or Button  Reports to Generate Click the checkbox to select the reports to generate. To edit graph details, highlight the graph option and click Edit. The Log list box Goodness of Fit and Goodness of Fit graphs cannot be edited.
Page 167: Dft Surface Energy Report Options
TriStar II 3020 Report Options Files DFT Surface Energy Report Options The DFT Surface Energy report contains the results of surface energy distribution analyses. In the Selected Reports list box, highlight DFT Surface Energy, then click Edit. DFT Surface Energy Report Options fields and buttons are identical to the DFT Pore Size Report Options, page 5-54.
Page 168: Tabular Report Options
Report Options Files TriStar II 3020 Field or Button Description  Report Type Select the checkbox to specify report types. If Astakhov is selected, either select the Optimize exponent checkbox or enter an appropriate exponent group box value in the text box.
Page 169: Transformed Isotherm Plot Options
TriStar II 3020 Report Options Files Transformed Isotherm Plot Options Highlight Transformed Isotherm in the Selected Reports list box and click Edit. The transformed Dubinin isotherm is the logarithm of quantity adsorbed as a function of the log of rel- ative pressure raised to a power.
Page 170: Pore Volume Options
Report Options Files TriStar II 3020 Pore Volume Options Highlight dV/dw Pore Volume in the Selected Reports list box and click Edit. This option plots differential pore volume as a function of pore width Field or Button Description  Plot curve / Plot Refer to Options, page 5-30.
Page 171: Mp-Method Report Options
TriStar II 3020 Report Options Files MP-Method Report Options The MP method provides pore volume distributions for microporous materials by correlating quantity adsorbed with the thickness of the adsorbed layer as determined from a user-selected thickness curve. In the Selected Reports list box, highlight MP-Method, then click the Equation button.
Page 172: Tabular Report Options
Report Options Files TriStar II 3020 Tabular Report Options Highlight MP Tabular Report in the Selected Reports list box and click Edit. To customize the order of columns 3 through 6 and data contents of reports, click the dropdown arrow for a column, and select the data type for that column.
Page 173: Options Report
TriStar II 3020 Report Options Files Description (continued) Field or Button Autoscale checkboxes Cancel button Refer to Options, page 5-1. Common Fields and Buttons - File Menu OK button Options Report The Options report provides a subset of the contents report. The Options report cannot be edited. It provides pertinent information for: •...
Page 174: Validation Report
Report Options Files TriStar II 3020 Validation Report Use this report to have the data examined by the software to determine if the results are within typical ranges. If the data selected for validation are determined to be out of range, a warning displays and suggestions are given for corrective action.
Page 175: Entered Or Collected Data File
TriStar II 3020 Entered or Collected Data File Entered or Collected Data File If Manually Entered is selected on the Advanced view of the Sample information window, an Entered Data tab displays. If Automatically Collected is selected, a Collected Data tab displays after the analysis is completed.
Page 176 Entered or Collected Data File TriStar II 3020 Field or Button Description Pressures group box For manually entered data only, select if the pressures are Relative or Absolute. Use calculation Select if calculation assignments are to be used. assignments checkbox pº...
Page 177: Unit Menu
TriStar II 3020 Introduction 6. UNIT MENU Introduction This chapter contains information specific to the Unit menu options. These options are used to run analyses on one or more units attached to a controlling computer. This chapter provides details of Unit menu options, and descriptions of commonly used functions and buttons.
Page 178: Common Fields And Buttons - Unit Menu Options
Common Fields and Buttons - Unit Menu Options TriStar II 3020 Common Fields and Buttons - Unit Menu Options The following fields and buttons are common to many of the Unit menu options. References are made to these fields and buttons throughout this manual.
Page 179 TriStar II 3020 Sample Analysis Port Activity window Status window Field or Button Description View dropdown list • Operation - select to display the current mode of operation. • Instrument Log - select to display recent analyses, calibrations, errors or messages. Refer to Log, page 6-14.
Page 180 Sample Analysis TriStar II 3020 Description (continued) Field or Button Report after analysis Click to select a print destination. button • Report after analysis checkbox - select to send the report to the screen, printer, or file in either ASCII, .XLS, or REP format.
Page 181: Quickstart Analysis
TriStar II 3020 QuickStart Analysis Description (continued) Field or Button Browse button Cancel button Refer to Options, page 6-2. Common Fields and Buttons - Unit Menu Edit button OK button QuickStart Analysis Unit [n] > QuickStart Analysis Use to analyze up to three samples of the same type using the same analysis conditions, adsorptive properties, and report options.
Page 182: Krypton Analysis
Krypton Analysis TriStar II 3020 Krypton Analysis Unit [n] > Krypton Analysis Use to perform up to three simultaneous krypton analyses. Use the following guidelines for performing krypton analyses: • All analyses must use krypton gas. An error message occurs if a gas other than krypton is specified.
Page 183: Blank Analysis
TriStar II 3020 Blank Analysis Blank Analysis Unit [n] > Blank Analysis Use to obtain sample tube parameters when using a calculated free space. A blank analysis can also be used for diagnostic purposes. Blank Analysis fields and buttons are identical to the Analysis, page 6-2.
Page 184: Enable Manual Control
Enable Manual Control TriStar II 3020 Enable Manual Control Unit [n] > Enable Manual Control Use to enable the manual control of certain system valves and elevator components. When this option is enabled, a checkmark appears to the left of the menu item. Enable this option by selecting Enable Manual Control on the menu.
Page 185: Instrument Schematic Components
TriStar II 3020 Enable Manual Control Instrument Schematic Components Component Description Valve - open. The icon color changes to green when open. Valve - closed. The icon color changes to yellow when closed. Servo Valve Elevator Sample tube - cannot be manually controlled.
Page 186: System Valves
Enable Manual Control TriStar II 3020 System Valves Select Unit [n] > Show Instrument Schematic to display the instrument schematic. Valves Description Sample ports 1 - 3 Po port Isolation valve Isolation valve Helium port Analysis gas ports 8 - 9...
Page 187: Instrument Schematic Shortcut Menus
TriStar II 3020 Enable Manual Control Instrument Schematic Shortcut Menus Each manually controlled component has a shortcut menu displaying the operations available for that particular component such as, Open, Close, Pulse. To access the shortcut menu, hover the mouse cur- sor over the component and right click.
Page 188: Show Instrument Schematic
Show Instrument Schematic TriStar II 3020 Show Instrument Schematic Unit [n] - Show Instrument Schematic Use to display an analyzer schematic. To operate the valves and elevator from this window, Manual Controls must be enabled (Unit [n] > Enable Manual Control).
Page 189: Show Status
TriStar II 3020 Show Status Show Status Unit [n] > Show Status Use to show only the status window of the analyzer. If multiple instruments are attached to the computer, the status window for each instrument is displayed in a different color.
Page 190: Show Instrument Log
Show Instrument Log TriStar II 3020 Show Instrument Log Unit [n] > Show Instrument Log Use to display a log of recent analyses, calibrations, errors or messages. This information is logged for a 7-day period for analyses and a 30-day period for messages and calibrations.
Page 191: Unit Configuration
• Change IP - click to display the Unit IP Setup window. Shows the IP address and Subnet mask assigned during installation. Do not edit these fields unless instructed by a Micromeritics service representative. • Board ID - click to read the board ID. The parameters on this window cannot be edited.
Page 192: Diagnostics
This option is typically used and/or requested by a service representative. These tests create and save files to the TriStar II 3020\Service\USERDIAG directory. The service representative may request an emailed or faxed copy of the file for diagnostic purposes.
Page 193 TriStar II 3020 Diagnostics Field or Button Description Test dropdown list Click to select the diagnostic test to run. Operator text box Enter the operator name, identifying information, etc. Repeat button Click the repeat the previous test. Enabled when the previous test is complete.
Page 194 Diagnostics TriStar II 3020 Field or Button Description Report button Click to view the diagnostic report. Report dropdown list Click the dropdown arrow to select the generated test report. Item [n] Lists the data in the two panes. Item 1 is the upper pane and Item 2, the lower pane.
Page 195: Calibration
TriStar II 3020 Calibration Calibration Unit [n] > Calibration Use to perform system calibrations. Disabled calibration options can be accessed only with the assis- tance of a service representative and are not covered in this manual. Zero Pressure Unit [n] > Calibration > Zero Pressure Use to evacuate the manifold and zero out the selected transducers.
Page 196: Match Transducers
Calibration TriStar II 3020 Match Transducers Unit [n] > Calibration > Match Transducers Use to zero and match the selected transducers to the main manifold transducer. Refer to  Transducers, page 9-26. Match Servo Valve Unit [n] > Calibration > Servo Valve Use to calibrate the servo valve to the manifold pressure transducer.
Page 197: Save To File
TriStar II 3020 Calibration Save to File Unit [n] > Calibration > Save to File Use to save the current calibration settings to a backup file which can later be reloaded using Unit [n] > Calibration > Load from File menu option.
Page 198: Load From File
Service Test Unit [n] > Service Test Use for service tests performed only with the assistance of a trained Micromeritics service representa- tive. These tests provide the service representative with troubleshooting tools and readouts. This option is enabled only when the analysis program is operating in Service Test mode. Refer to...
Page 199: Reports Menu
TriStar II 3020 Introduction 7. REPORTS MENU Introduction This chapter contains information specific to the Reports menu options used to customize and run reports. This chapter provides details of Reports menu options, commonly used functions and buttons, field-by-field descriptions, and sample reports.
Page 200: Common Fields And Buttons - Reports Menu Options
Common Fields and Buttons - Reports Menu Options TriStar II 3020 Common Fields and Buttons - Reports Menu Options The following fields and buttons are common to many of the report files. References are made to these fields and buttons throughout this chapter.
Page 201: Close Reports
TriStar II 3020 Close Reports Close Reports Reports > Close Reports (or use the F9 keyboard shortcut) Use to close all open report windows. This option is unavailable if reports are being generated. Open Report Reports > Open Report > [file] Use to open a saved report.
Page 202 SPC Report Options TriStar II 3020 If additional report options are required, click the More button. The selected items also appear as options on the Reports > Control Chart screen. (Click the Graph [n] button, then click the Statistic dropdown arrow.)
Page 203: Regression Report
TriStar II 3020 Regression Report Regression Report Reports > Regression Report Use to generate an SPC (Statistical Process Control) Regression report to determine the interdepen- dency between two variables. Up to three dependent variables (Y-axis) may be plotted against a single independent variable (X-axis).
Page 204 Regression Report TriStar II 3020 Description (continued) Field or Button Tabular report checkbox Select to generate a tabular report of the included samples. A tabular report contains the numeric values contributed by each sample.  Recalculate archived Select to have archived SPC values recalculated ensuring any changes SPC results checkbox made to the SPC Report Options are included in the new report.
Page 205: Control Chart
TriStar II 3020 Control Chart Description (continued) Field or Button Save as Default button Click to save selected report options as default report settings. Browse button Cancel button Refer to Common Fields and Buttons - Reports Menu Options, page 7-2.
Page 206 Control Chart TriStar II 3020 Field or Button Description  X Axis Order by Select the order in which X-axis statistics are placed. group box • Time - sorts by the time the files were analyzed. • File name - sorts in alphanumeric order.
Page 207 TriStar II 3020 Control Chart Description (continued) Field or Button Graph [n] buttons • Center Line group box - displays placement options for the center line in the graph. Choose Entered to specify placement of the line. (continued) • Limit Lines group box - displays limiting lines options. Lines can be placed at some multiple of the standard deviation or at specified positions (Entered).
Page 208: Heat Of Adsorption Report
Heat of Adsorption Report TriStar II 3020 Heat of Adsorption Report Reports > Heat of Adsorption Use to select sample files, define quantities and generate a Heat of Adsorption report. The isosteric heat of adsorption is an important parameter for characterizing the surface heterogeneity and for pro- viding information about the adsorbent and the adsorption capacity.
Page 209 TriStar II 3020 Heat of Adsorption Report Description (continued) Field or Button  Edit Quantities Use to specify the range of surface coverage to include in the report. button • Insert Range button - click to specify the starting and ending quantities adsorbed and number of points to insert.
Page 210: Report Features And Shortcuts
Report Features and Shortcuts TriStar II 3020 Description (continued) Field or Button  Isostere plot Select to generate a graph showing quantities of gas adsorbed versus the checkbox temperature.  Heat of adsorption Select to generate the Heat of Adsorption data in a graphical format.
Page 211: Report Header
TriStar II 3020 Report Features and Shortcuts Report Header All reports contain a header displaying file statistics. If configured, the report header can also contain a graphic and a title. • Tabular and graphical reports contain sample and instrument statistics such as analysis date / time, analysis conditions, etc.
Page 212: Report Tool Bar
Report Features and Shortcuts TriStar II 3020 Report Tool Bar Each report has a tool bar and selectable tabs across the top of the report header. To view a specific report, select its tab or select the report in the Reports list box and click Show.
Page 213 TriStar II 3020 Report Features and Shortcuts Description (continued) Field or Button Print button Displays a print window for report output. • Printer group box -  Name dropdown list and Properties button - select the printer and click the Properties button to change printout orientation, etc....
Page 214 Report Features and Shortcuts TriStar II 3020 Description (continued) Field or Button Default Style button Click to specify default report parameters for fonts and curve properties. • Font group box - Font Type list box - allows font type and attributes to be edited for the selected item.
Page 215: Report Shortcut Menus
TriStar II 3020 Report Features and Shortcuts Report Shortcut Menus Shortcut menus are accessed by right-clicking on the report header or the report body displayed on the screen. Report Header Shortcuts Display header shortcuts by right-clicking in the report header.
Page 216 Report Features and Shortcuts TriStar II 3020 Description (continued) Option Move column Right-click on the column to be moved. Select Move Column on the shortcut menu and select Left or Right for the move. Align column Right-click on the column to be aligned. Select Align Column on the shortcut menu and select Left, Right or Center.
Page 217: Graph Shortcuts
TriStar II 3020 Report Features and Shortcuts Graph Shortcuts Display graph report shortcuts by right-clicking in the body of the graph report. Option Description Autoscale all axes Returns the report to full view after using the zoom feature. Reset axis limits to Removes the cross-hair and returns the graph back to the initial setting.
Page 218 Report Features and Shortcuts TriStar II 3020 Description (continued) Option Edit curve Use to edit selected curve properties. • Title text box - use to change the title of the selected curve. • Style dropdown list - use to select another style for the collected data curve.
Page 219 TriStar II 3020 Report Features and Shortcuts Description (continued) Option Graph Label Edit axis Use to edit axis properties. • Title group box - use to edit the selected axis label. Title text box - use to modify the label of the selected axis.
Page 220 Report Features and Shortcuts TriStar II 3020 Description (continued) Option  Edit axis Autoscale minimum / maximum - select the Autoscale checkbox to enable the option. To manually specify minimum / maximum, deselect (continued) the Autoscale checkbox and enter the new amount in the text box.
Page 221: Other On-Screen Features
TriStar II 3020 Report Features and Shortcuts Other On-Screen Features Zoom Feature Use the zoom feature to closer examine graph details. To use this feature: Open the graph. Hold down the left mouse button and drag the cursor across the graphical area to be enlarged. A box will display in the area to be enlarged.
Page 222: Report Examples
Report Examples TriStar II 3020 Report Examples This section of the manual contains samples of some of the available reports. Most of the reports can be customized. 7-24 302-42828-01 - Dec 2012...
Page 223: Isotherm Linear Plot
TriStar II 3020 Report Examples Isotherm Linear Plot 302-42828-01 - Dec 2012 7-25...
Page 224: Bet Surface Area Report
Report Examples TriStar II 3020 BET Surface Area Report 7-26 302-42828-01 - Dec 2012...
Page 225: Bet Surface Area Plot
TriStar II 3020 Report Examples BET Surface Area Plot 302-42828-01 - Dec 2012 7-27...
Page 226: T-Plot
Report Examples TriStar II 3020 t-Plot 7-28 302-42828-01 - Dec 2012...
Page 227: Bjh Adsorption Cumulative Pore Volume
TriStar II 3020 Report Examples BJH Adsorption Cumulative Pore Volume 302-42828-01 - Dec 2012 7-29...
Page 228: Bjh Adsorption Dv/Dlog(W) Pore Volume
Report Examples TriStar II 3020 BJH Adsorption dV/dlog(w) Pore Volume 7-30 302-42828-01 - Dec 2012...
Page 229: Options Menu
TriStar II 3020 Introduction 8. OPTIONS MENU Introduction This chapter contains information specific to the Options menu selections used to configure the system by setting defaults for sample and parameter files. This chapter contains information on: • changing the default presentation format - Restricted, Basic, or Advanced •...
Page 230: Sample Defaults
Sample Defaults TriStar II 3020 Sample Defaults Options > Sample Defaults Use to specify default parameters for sample information files and report option files in either Advanced, Basic, or Restricted format. The Restricted format requires a password when entering or exiting the Restricted format.
Page 231: Units
TriStar II 3020 Units Units Options > Units Use to specify how data should appear on the application windows and reports. This menu option is not available if using Restricted format. Graph Grid Lines Options > Graph Grid Lines Use to select how grid lines appear on reports. This menu option is not available if using Restricted format.
Page 232: Live Graph
Basic or Restricted presentation mode. This configuration option is not available if using Restricted format presentation mode. The system default directory is the recommended location for saving report options files. The default directory is param and includes several parameter files supplied with the TriStar II 3020 program. 302-42828-01 - Dec 2012...
Page 233: Service Test Mode
Service Test mode is a password protected option used to perform certain service tests with the assis- tance of a trained Micromeritics service representative. This password is supplied by your service representative. After Service Test Mode has been enabled, the service tests are accessible from the Unit menu (Unit >...
Page 234 Service Test Mode TriStar II 3020 302-42828-01 - Dec 2012...
Page 235: Troubleshooting And Maintenance
TriStar II 3020 Introduction 9. TROUBLESHOOTING AND MAINTENANCE Introduction The analyzer has been designed to provide efficient and continuous service; however, certain mainte- nance procedures should be followed to obtain the best results over the longest period of time. This chapter includes maintenance and calibration procedures.
Page 236 Troubleshooting TriStar II 3020 What Happened What To Do Elevator is noisy The elevator screw may need Contact your Micromeritics greasing. Service Representative. Sample is not within There may be a leak into or out Refer to Inspecting and specifications.
Page 237: Preventive Maintenance
** For oil-free pumps only: After 12 to 18 months of operation, the diaphragm in the pump will wear out and the pump becomes completely inoperable. To prevent instrument downtime due to an inoperable pump, it is recommend that the diaphragm be replaced by a Micromeritics Service Rep- resentative every 12 months.
Page 238: Lubricating Elevator Drive Assembly
Lubricating Elevator Drive Assembly The elevator screw is lubricated before it leaves the factory and should not require lubricating. If the elevator starts to vibrate or becomes noisy when traveling, contact a Micromeritics Service Represen- tative for disposition. Cleaning the Analyzer The exterior casing of the analyzer may be cleaned using a clean cloth, dampened with isopropyl alco- hol (IPA), a mild detergent, or a 3% hydrogen peroxide solution.
Page 239: Replacing Port Filter (Frit) And O-Ring
TriStar II 3020 Preventive Maintenance Rinse the Dewar with warm water to melt any ice accumulation which may remain in the Dewar, then dry thoroughly. Replacing Port Filter (Frit) and O-ring A filter (frit) is located in each analysis port. If the filter is contaminated, the contaminant may adsorb or desorb during analysis, affecting the results.
Page 240: Replacing The Sample Tube O-Ring
Preventive Maintenance TriStar II 3020 Replacing the Sample Tube O-ring It is important to maintain a vacuum-tight seal near the top of the sample tube stem. If an O-ring becomes worn or cracked, it does not provide a good seal and will need to be replaced.
Page 241: Inspecting And Changing Vacuum Pump Oil
Always drain the vacuum pump while the pump is warm and disconnected from the power source. Use oil supplied by Micromeritics or refer to the vacuum pump manual for other acceptable oils. Unplug the vacuum pump from the power source.
Page 242 Preventive Maintenance TriStar II 3020 Loosen the wing nut on the clamp at the top of the oil vapor trap. Swing the clamp open and remove the trap from the hose. Grasp the handle on top of the vacuum pump and place it on a work table.
Page 243 TriStar II 3020 Preventive Maintenance Remove the plug from the oil-fill port. Oil-fill port Slowly add oil to the port until the level is midway between the indicator lines in the oil-level window when the pump is running. Midway level Do not allow oil to rise above the midway position when the pump is running.
Page 244: Replacing The Alumina In The Oil Vapor Trap
Preventive Maintenance TriStar II 3020 Replacing the Alumina in the Oil Vapor Trap The activated alumina in the oil vapor trap becomes saturated during use. The alumina should be inspected periodically and replaced when most of the alumina pellets are no longer white.
Page 245 TriStar II 3020 Preventive Maintenance Do not perform the following procedure on used alumina. The resultant oil vapors may cause a fire or an explosion. Prepare fresh alumina as follows: ° a.) Preheat the oven to 300 b.) Pour approximately 180 grams of fresh alumina into a glass or metal container (approximately 250 mL if a graduated beaker is used).
Page 246 Preventive Maintenance TriStar II 3020 Screw one of the end fittings onto the trap body. 10. Ensure the trap body is dry and the alumina is lukewarm. Pour the alumina pellets into the trap until level with the top of the trap body.
Page 247 TriStar II 3020 Preventive Maintenance Centering ring 15. Place the trap on the centering ring. 16. Open the clamp and place it around the flange of the intake port and the flange of the trap. Swing the clamp fastening screw toward the intake port until it fits into the slot in the other half of the clamp.
Page 248: Changing The Vacuum Pump Exhaust Filter
Preventive Maintenance TriStar II 3020 b.) Swing the c-clamp fastening screw around until it fits into the slot on the other half of the clamp. Tighten the wing nut securely by hand. 18. Plug the pump power cord into the power source.
Page 249: Performing A Leak Test
TriStar II 3020 Performing a Leak Test Open the clamp and place it around the exhaust port flange and the exhaust filter flange. Swing the clamp fastening screw toward the exhaust port until it fits into the slot in the other half of the clamp.
Page 250 Performing a Leak Test TriStar II 3020 Verify that all tests have a Passed status by clicking the tabs and looking for the Passed status for each test run. Click Save As and accept the default name displayed the File name field.
Page 251: Connecting Gases
TriStar II 3020 Connecting Gases Connecting Gases This procedure is also shown in one of the How-To videos located on the Help menu. Guidelines for Connecting Gases to the Analyzer 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.
Page 252: Connecting A Replacement Gas Bottle
Connecting Gases TriStar II 3020 Both gauges should read at or near zero. If not, open the regulator gas shut-off valve to release gas. It is not necessary to disconnect the gas line from the regulator or the instrument. Use an appropriate wrench to loosen the nut at the regulator/gas bottle connection then remove the regulator from the bottle.
Page 253 TriStar II 3020 Connecting Gases Use an appropriate cylinder wrench to remove the protective cap from the replacement bottle. Attach the gas regulator to the gas bottle connector. Hand-tighten the nut then use an appropriate wrench to tighten an additional 3/4 turn.
Page 254 Connecting Gases TriStar II 3020 Purge the air from the lines. Gas bottle shut-off valve Regulator shut-off valve a.) Turn the regulator clockwise until the low pressure gauge shows a few pounds of pressure. b.) Turn the regulator shut-off valve counterclockwise to open.
Page 255: Cleaning And Verifying The Gas Line
TriStar II 3020 Connecting Gases If the gas line to the instrument inlet was previously disconnected, reconnect it now. Verify the line for the newly connected gas is clean. If the previously disconnected gas has been reconnected, resume operation. If a different gas has been connected, the change must be specified in the software. Refer to Ports, page 9-25.
Page 256 Connecting Gases TriStar II 3020 Click the down arrow to the right of the Test field and select Clean and Verify Analysis Gas Line Rev [n] Test Rev [n]. Click Report after analysis and select Preview as the destination. Click OK.
Page 257 TriStar II 3020 Connecting Gases If the Leak Rate field indicates Failed, a leak is indicated between this connection. Check the connections from the instrument to the gas regulator valve. Tighten as necessary, then run the test again. Click the Instrument to Gas Bottle Shut-off Valve - 2 tab to display its report.
Page 258 Connecting Gases TriStar II 3020 Click the Gas Pressure Test - 3 tab to display its report. On the report, the Minimum field should read Passed. A Passed reading indicates all valves are in the proper state for operation. If the Minimum field indicates Failed, one or more valves is not in the proper position. Set the valves as shown below and ensure the appropriate pressure is displayed on the low-pressure gauge.
Page 259: Specifying Gas Ports
Reinstalling Calibration Files for an system unless you suspect it is out of calibration. Certain calibrations are not allowed unless performed under the direction of a Micromeritics service representative. Those calibrations are greyed out on the Calibration menu. To review calibration details of the analyzer, go to Unit [n] > Unit Configuration.
Page 260: Zero Pressure
Calibrating the System TriStar II 3020 Zero Pressure Use this option to evacuate the system and zero the transducers. Install a blank sample tube on each applicable port. Go to Unit [n] > Calibration > Zero Pressure. Ensure that all transducers are selected, then click Start. The window closes when the operation is complete.
Page 261: Servo Valve
TriStar II 3020 Calibrating the System Servo Valve Ensure the pressure transducer has been calibrated before performing this procedure. Go to Unit [n] > Unit Configuration and view the calibration information. Contact your service representative if calibration dates are not listed.
Page 262 Calibrating the System TriStar II 3020 9-28 302-42828-01 - Dec 2012...
Page 263: 10. Ordering Information
The analysis system components and accessories can be ordered using one of the following methods: • Call our Customer Service Department at (770) 662-3636 • Email orders to orders@micromeritics.com • Contact your local sales representative Please use the following information to place an order.
Page 264 TriStar II 3020 Item and Description (continued) Part Number 300-31802-03 Dewar Cover (for glass or stainless steel Dewar), for 1/2 in. sample tube Gas Bottle Accessories 004-25549-00 Reducer, 1/8 in. tube × 1/4 in. tube 004-33601-00 Expansion Kit; adds an additional outlet to the gas regulator 004-33602-00 Pressure Relief Kit;...
Page 265 TriStar II 3020 Item and Description (continued) Part Number 004-16816-00 Reference Material, Alumina, ~ 0.25 m /g, 15 g; for krypton analysis 004-16818-00 Reference Material, Glass, ~ 5.8 m /g, 10 g 004-16821-00 Reference Material, Silica alumina, ~ 215 m...
Page 266 TriStar II 3020 Item and Description (continued) Part Number 302-25821-01 Hanging Filler Rod, for 3/8 in. sample tube 302-25821-02 Hanging Filler Rod, for 1/2 in. sample tube 302-33601-00 Sample Tube Kit, 1/4 in.; includes six each sample tubes, O-rings, and plastic caps;...
Page 267 TriStar II 3020 Item and Description (continued) Part Number 302-20828-00 TriStar II 3020 - current version software 302-42828-01 TriStar II 3020 - operator’s manual Vacuum Pump and Accessories 004-16003-01 Oil, vacuum pump, 1 Liter 004-16830-00 Activated Alumina, 500 grams; for oil vapor trap...
Page 268 TriStar II 3020 10-6 302-42828-01 - Dec 2012...
Page 269: Forms
TriStar II 3020 A. FORMS This appendix contains the following form: • Sample Data Worksheet Copy and use this form as needed. 302-42828-01 - Dec 2012...
Page 271: Sample Data Worksheet
Sample Data Worksheet Use this worksheet to record the values necessary to calculate the sample mass. Sample Tube Identification:_________________________________ Sample Mass NOTE: Record all values in grams. Before Degas After Degas After Analysis ____________ A. Mass for empty sample tube set: ____________ _____________ ____________...
Page 273: Error Messages
The 1000-series error messages, used primarily for software testing, are not included in this appendix. These errors should not occur during normal operation. If a 1000- series message appears, contact a Micromeritics service representative after making backup copies of any files involved in the operation.
Page 274 2432- Invalid response from MMI ‘FILE_READ’ request. Cause: An internal processing and/or hardware error has occurred. Action: Contact a Micromeritics service representative if this error message continues. 2433- New entries have been found in this directory. Refresh the directory information?
Page 275 2447- Error writing data. Cause: An unexpected error occurred when trying to access a data file. Action: Contact a Micromeritics service representative if this error message continues. 2448- File directory [path name] is invalid. Resetting to the installation directory. Cause: A working directory specified in the .INI file is invalid or has been...
Page 276 Action: Ensure that the analyzer is connected to the computer on the communications port configured in the Setup program. Stop and restart the analyzer software. Contact a Micromeritics service representative if this error message continues. 302-42828-01 - Dec 2013...
Page 277 ON position and that the light on the front panel is illuminated. If the application continues to fail in its attempts to initialize the instrument, contact a Micromeritics service representative if this error message continues.
Page 278 An attempt was made to open a file currently being used. Action: Locate the application using the file (in the Micromeritics application, use the Windows menu item to get a list of all windows, one of which may contain this file).
Page 279 Contact a system administrator to have full rights granted. Cause B: An internal processing and/or hardware error has occurred. Action B: Contact a Micromeritics service representative if this error message continues. 2488- File [file name] cannot be opened for editing. It is already in use.
Page 280 A request to change the file’s status, for example, from automatically collected to manually entered could not be done. Action: Contact a Micromeritics service representative if this error message continues. Record the name of the sample file in which the problem occurred.
Page 281 TriStar II 3020 Appendix B 2587- Sample file [name] has no dose incremental table entries. Cause: An attempt was made to start an analysis with an empty dose increment table. Action: Add dose increment entries to the dose increment table in the analysis conditions.
Page 282: 2500 Series
A large number of windows are open and consuming the system resources available to all applications. Action: Close one or more windows on the screen. Contact a Micromeritics service representative if this error message continues. 2505- Error logger cannot be initialized. Error code [n]. Program will exit.
Page 283 The selected sample file does not have collected data and cannot be used for reporting. Action: Select a different sample file. 2521- Unable to program controller. Cause: A hardware malfunction has occurred. Action: Contact a Micromeritics service representative if this error message continues. 302-42828-01 - Dec 2013 B-11...
Page 284 2531- Controller debug port error. Cause: An internal processing and/or hardware error has occurred. Action: Contact a Micromeritics service representative if this error message continues. 2532- The instrument contains a different software version. Do you want to reset it? Cause: The application has discovered a different version of software operating in the analyzer.
Page 285 Action: Ensure that the communications cable is seated firmly in the Ethernet slot at the analyzer connection and the computer connection. Contact a Micromeritics service representative if this error message continues. 2551- Unable to establish the TCP connection with the instrument.
Page 286: 4000 Series
Open the sample file after the critical operation has completed. 2557- Cannot access web page. Cause: The Micromeritics web page for DFT models cannot be accessed. This could be caused by an ISP problem of high internet traffic. Action: Try the operation later.
Page 287 The target disk drive may be damaged or inoperative. Verify that other files may be created on the same drive. Contact a Micromeritics service representative if this error message continues. 302-42828-01 - Dec 2013...
Page 288 Appendix B TriStar II 3020 4016- Sample [sample file name] has no data for export. Cause: The file selected for export has a status of No Analysis. No export file will be created. Action: Select a file which contains analysis data.
Page 289 TriStar II 3020 Appendix B 4022- The entered bath temperature value (Po and Temperature Options of the Anal- ysis Conditions) is outside the range of the temperatures listed in the Psat vs Temperature Table (Adsorptive Properties). Cause: The entered bath temperature is outside of the range of temperatures specified in the Adsorptive Properties.
Page 290 Appendix B TriStar II 3020 4028- Dubinin calculations cannot be performed because the affinity coefficient of the analysis gas is zero. Cause: Dubinin values could not be calculated because the affinity coefficient of the analysis gas is zero. Action: Access the Dubinin Report Adsorptive options in the sample file and enter an appropriate value for the analysis gas.
Page 291 TriStar II 3020 Appendix B 4035- Cannot calculate optimized Astakhov exponent: Not enough points with a rel- ative pressure in the range [(pressure), (pressure)]. Cause: There are fewer than two valid data points in the relative pressure range specified. Astakhov reports will not be produced.
Page 292 Appendix B TriStar II 3020 4039- The isotherm does not meet the constraints of the Cheng/Yang assumption. Cheng/Yang correction will not be applied. Cause: The Cheng/Yang correction to the Horvath-Kawazoe equation requires the value of the monolayer volume as calculated from the Langmuir equation.
Page 293 TriStar II 3020 Appendix B 4042- 0.0 cannot be a starting or ending pressure for a geometric progression from low pressure. Cause: An attempt was made to generate a pressure table from a geometrically progressing range. Action: Change the 0.0 entered value.
Page 294 Appendix B TriStar II 3020 4048- Warning: An error occurred while restoring the heat of adsorption report editor. Cause: The state of the heat of adsorption report editor could not be restored. Default settings will be used. Action: No action.
Page 295 TriStar II 3020 Appendix B 4054- Fewer than two data points are inside the fitted thickness range. Cause: At least two points must be within the fitted thickness range for the t- Plot calculations. Action A: Edit the calculation assignments for the t-Plot report.
Page 296 At least two points are required in a thickness curve definition. Action: Edit the thickness curve. 4062- Error during report preparation. Cause: An internal processing error has occurred. Action: Contact a Micromeritics service representative if this error message continues. B-24 302-42828-01 - Dec 2013...
Page 297 TriStar II 3020 Appendix B 4063- The data requested on this report are not available. No subreports selected. Cause: There is no information in the sample log to report. Action: A sample file was selected which no instrument operations has been used.
Page 298 Appendix B TriStar II 3020 4072- The range of pressures selected is too small to deconvolute using this model. Cause: A null result was found using the selected model. Action: Edit data points in the table of the Collected Data window or select another sample file.
Page 299 TriStar II 3020 Appendix B 4078- Slope and Y-Intercept cannot be determined from the selected points. Cause: The Langmuir report cannot be generated from the selected points. Action: Edit the calculation assignments in the Langmuir column on the Collected Data window.
Page 300: 6000 Series
Appendix B TriStar II 3020 Action: Use the SmartPrep setup program to download the proper controller software to the instrument, or if unavailable, contact a Micromeritics service representative. 4405- Fatal communications error with SmartPrep Unit [n] - S/N: [nn]. Cause: There was a fatal error in the serial communications between the application and the SmartPrep Instrument Controller.
Page 301 TriStar II 3020 Appendix B 6010- This sample requires a different adsorptive and cannot be analyzed at the same time as the other samples. Cause: A sample file for analysis was selected that requires a different adsorptive gas than the sample files selected for the other ports.
Page 302 Action B1: Check the Dewar, remove ice and restart the analysis. Action B2: If results for Actions A and B failed, contact a Micromeritics service representative. 6020- Warning, servo valve performance is out of specification. Cause: The servo valve tried to dose to a pressure but was unable to reach it within specification.
Page 303 TriStar II 3020 Appendix B 6021- Servo calibration failed. Cause A: The maximum time was exceeded before the target pressure point was reached. The nitrogen regulator may be set too low or turned off. Action A: Set the analysis gas regulator to at least 10 psig (0.7 bar), then resume the analysis.
Page 304 Appendix B TriStar II 3020 6025- Target pressure [PRn] [PR-U] exceeded maximum manifold pressure of [PRn] [PR-U]. Analysis is canceled. Cause: An absolute pressure greater than (pressure) units was attained that exceeded the specified maximum manifold pressure. Action: The analysis was canceled. All previously collected data were stored.
Page 305 TriStar II 3020 Appendix B 6030- Dosing method choice is invalid. The Krypton analysis requires that Adsorptive Properties “Dosing Method” is set to “From Psat tube.” Cause: A file was selected for a krypton analysis that has Normal selected for the Dosing Method. Normal is for standard analyses only.
Page 306 Ensure the gas is connected properly and assigned correctly in the Unit Configuration window. Replace the tank if necessary. Cause B: The gas valve is not working properly. Action B: Contact a Micromeritics service representative if this error message continues. B-34 302-42828-01 - Dec 2013...
Page 307 Cause: There is a problem with the analyzer’s calibration. Action: Use the Setup program to reinstall the calibration files. Contact a Micromeritics service representative if this error message continues. 6557- File [file name] already selected for the analysis Cause: The same sample file is already assigned to a different port for this analysis.
Page 308 Appendix B TriStar II 3020 B-36 302-42828-01 - Dec 2013...
Page 309: Calculations
TriStar II 3020 Appendix C C. CALCULATIONS This appendix contains the calculations used in the analysis program. Saturation Pressure Saturation pressure (Po) is selected on the Po and Temperature Options dialog. It may be entered or measured in the Po tube or on port 3.
Page 310: Quantity Adsorbed Calculations
Appendix C TriStar II 3020 relative pressure for the I data point (mmHg) absolute pressure for the I data point, taken at equilibrium (mmHg) Quantity Adsorbed Calculations Free Space Measured Measured free-space volumes are calculated using the following equations: ...
Page 311: Calculated
TriStar II 3020 Appendix C Calculated The calculated free space is determined by subtracting the gas capacity of the volume occupied by the sample from the measured free space of the empty tube. V V  ------------- – V V ...
Page 312 Appendix C TriStar II 3020 Equilibration Equilibration is reached when the pressure change per equilibration time interval (first derivative) is less than 0.01% of the average pressure during the interval. Both the first derivative and average pres- sure are calculated using the Savitzky-Golay convolution method for polynomial functions.
Page 313: Thermal Transpiration Correction
TriStar II 3020 Appendix C Thermal Transpiration Correction During data reduction, thermal transpiration correction is applied to the data if the user selected Ther- mal transpiration correction from the Report Options dialog. Starting with the first collected pressure, the following calculations are performed until the pressure ratio (PC/P) is greater than or equal to 0.99.
Page 314: Bet Surface Area
Appendix C TriStar II 3020 BET Surface Area For each point designated for surface area calculations, the BET transformation is calculated as follows: ------------------------------------------------ -    1.0 P – where B is in units of g/cm STP. A least-squares fit is performed on the (P...
Page 315: Langmuir Surface Area
TriStar II 3020 Appendix C Langmuir Surface Area For each point designated for surface area calculations, the Langmuir transformation is calculated as follows: ----------- - where L is in units of g/cm A least-squares fit is performed on the (P...
Page 316: T-Plot
Appendix C TriStar II 3020 t-Plot For each point designated for t-Plot calculations, the following calculations are done: Thickness for the I point (Å): (Halsey  -------------------- -   HJP3 HJP1 (Harkins and Jura --------------------------------------------   – HJP2 ...
Page 317 TriStar II 3020 Appendix C Using the results of the above calculations, the following can be calculated: External Surface Area (m /g):        STP  /g A STP – S cm liquid/cm --------------------------------------------------------------------------------------------------------------------------------------------------------- - ...
Page 318: Bjh Pore Volume And Area Distribution
Appendix C TriStar II 3020 BJH Pore Volume and Area Distribution For adsorption data, the relative pressure and quantity adsorbed data point pairs collected during an analysis must be arranged in reverse order from which the points were collected during analysis. All calculations are performed based on a desorption model, regardless of whether adsorption or desorp- tion data are being used.
Page 319: Calculations
TriStar II 3020 Appendix C c.) The walls of the cylindrical pore - the diameter of the empty pore is required to determine the pore volume and pore area. End area is neglected. Pore Wall Insignificant compared to core length...
Page 320 Appendix C TriStar II 3020 The thickness of the remaining adsorbed layer at this relative pressure is calculated: ------------------ -   where HP1, HP2, and HP3 are Halsey Parameters 1, 2, and 3 (respectively) from the Halsey Thickness Equa- tion dialog.
Page 321 TriStar II 3020 Appendix C The total volume of gas desorbed from walls of previously opened pores is calculated:  for all previously opened pores   CSAa   where LP = length of previously opened pores as calculated in Step b(2).
Page 322 Appendix C TriStar II 3020 weighted average pore diameter and a corresponding length sufficient to account for the required volume of adsorbate. The weighted average pore diameter is calculated as follows: 2   Rc   Rc   Rc ...
Page 323 TriStar II 3020 Appendix C (not including D avgK The layer thickness change desorbed during this interval also is added to the radii corre- sponding to the ends of the pressure intervals as follows: Tw Jnew Jold for all except Rc Steps a to c are repeated for each pressure interval.
Page 324 Appendix C TriStar II 3020 (6.) dV/dlog(D) pore volume (dV/dlog(D) , cm     ---------------- dDv/d   (7.) dA/dD pore area (dA/dD /g-A): ------------------------------- - dA/dD – (8.) dA/dlog(D) pore area [dA/dlog(D) /g]:    ...
Page 325 TriStar II 3020 Appendix C CUMJ (5.) Incremental Surface Area (SAF /g): – – where SAF = 0. CUM0 (6.) dV/dD pore volume (dV/dDpF , cm /g-A)):   dV/dDpF INTERP DpF where INTERP(x) is the value interpolated from the function X = D...
Page 326: Compendium Of Variables
Appendix C TriStar II 3020 Compendium of Variables volume adsorbed expressed as a volume (cm /g STP) liquid equivalent volume of volume adsorbed (cm density conversion factor from the Adsorptive Properties dialog cm STP) relative pressure pore (or core) diameter (A) Kelvin radius (A) of core adsorbate property factor;...
Page 327: Horvath-Kawazoe
TriStar II 3020 Appendix C Horvath-Kawazoe A relative pressure lower limit is determined such that L-d never equals zero. All pressure points less than this limit are discarded. For each collected relative pressure point, values of L are chosen in an...
Page 328: Cylinder Pore Geometry (Saito/Foley
Appendix C TriStar II 3020 where: = molecular diameter (Å) from the Horvath-Kawazoe Physical Properties dialog = diameter of sample atom (Å) from the Horvath-Kawazoe Physical dialog pore width (nucleus to nucleus) (Å) equilibrium pressure (mmHg) saturation pressure (mmHg) interaction parameter (10...
Page 329: Sphere Pore Geometry (Cheng/Yang
TriStar II 3020 Appendix C Sphere Pore Geometry (Cheng/Yang) When you use the Cheng/Yang method, the following equation is solved for each value of P. The value of L is determined when the solved-for relative pressure is within 0.1% of the collected absolute pressure.
Page 330: Cheng/Yang Correction
Appendix C TriStar II 3020 ------------------ - ------------------- –     – ------------------- ------------------ - –     – – where -------------- Cheng/Yang Correction This factor corrects for the nonlinearity of the isotherm. It adds an additional term to the equations for the different geometrics: ...
Page 331: Interaction Parameter
TriStar II 3020 Appendix C Interaction Parameter The interaction parameter (IP) results from the following calculations: The Kirkwood-Muller dispersion coefficients -      6 MC ---------------------------------------------- -   ----- - ------     ...
Page 332: Additional Calculations
Appendix C TriStar II 3020 Additional Calculations Based on the previous calculations, the following can be calculated: Adjusted Pore Width (Å): (Shell to Shell) – Cumulative Pore Volume (cm /g):  where density conversion factor (cm liquid/cm STP) on the Adsorptive Properties...
Page 333: Interaction Parameter Components
TriStar II 3020 Appendix C Interaction Parameter Components Table C-1. Interaction Parameters Interaction Bath Parameter Sample Type Temperature Calculated Value* Argon 87.3 Carbon (Ross/Olivier value) 2.61 Carbon (Horvath/Kawazoe value) 5.89 Zeolite 3.19 Carbon 298.15 Carbon (Ross/Olivier value) 4.20 Dioxide Carbon (Horvath/Kawazoe value) 9.20...
Page 334 Appendix C TriStar II 3020 The following values were used to calculate the values in Table C-1. Carbon-Graphite Zeolite = 3.40 = 3.04 = 3.845 x 10 = 3.75 x 10   = 1.05 x 10 (Ross/Olivier) = 1.94 x 10 ...
Page 335: Dubinin-Radushkevich
TriStar II 3020 Appendix C Dubinin-Radushkevich The Dubinin-Radushkevich equation is as follows:  V      --------------- – ------ -  where: volume adsorbed at equilibrium pressure (cm /g STP) the micropore capacity (cm /g STP) saturation vapor pressure of gas at temperature T (mmHg)
Page 336 Appendix C TriStar II 3020 Error of Monolayer Capacity (cm /g STP): = Vo x (10 - 1.0) Micropore surface area (m /g):  Vo      6.023 10 ----------------------------------------------------------------------    22414 cm where ...
Page 337: Dubinin-Astakhov
TriStar II 3020 Appendix C Dubinin-Astakhov The Dubinin-Astakhov equation is a follows: V      --------- – ------ - E where volume adsorbed at equilibrium pressure (cm /g STP) the micropore capacity (cm /g STP) saturation vapor pressure of gas at temperature T (mmHg)
Page 338 Appendix C TriStar II 3020 Using the results of the above calculations, the following can be calculated: Monolayer Capacity (cm /g STP): = 10 Micropore Volume (cm /g): = (V x D) where density conversion factor (cm liquid/cm STP) from the Adsorptive proper- ties dialog ...
Page 339 TriStar II 3020 Appendix C Maximum Differential Pore Volume (cm /g-Å): This value is also known as frequency of the mode  E  1/3N          ------------------ - Max --------------- - ---------------------------- - --------------- - –...
Page 340 Appendix C TriStar II 3020 Equivalent Pore Diameter (Å): 1/3N   ---------------------------- - –    E     -----------------------------------------     – dV/dD Pore Volume (cm /g-Å):     – –...
Page 341: Mp-Method
TriStar II 3020 Appendix C MP-Method For each point designated for MP-method calculations, the following calculations are done: Thickness for the I point (Å): (Halsey  -------------------- -   HJP3 HJP1 (Harkins and Jura --------------------------------------------   – HJP2...
Page 342 Appendix C TriStar II 3020 Remaining pore surface area for the I point (m /g): 6 –       – D 10 – ---------------------------------------------------------------------------------- - –   10  – – where density conversion factor (cm...
Page 343: Freundlich Isotherm
TriStar II 3020 Appendix C Freundlich Isotherm The Freundlich isotherm has the form: ------- where quantity of gas adsorbed quantity of gas in a monolayer temperature-dependent constant temperature-dependent constant The pressure is absolute; typically, m > 1. In terms of quantity adsorbed,...
Page 344: Dft (Density Functional Theory
Appendix C TriStar II 3020 DFT (Density Functional Theory) The adsorption isotherm is known to convey a great deal of information about the energetic heteroge- neity and geometric topology of the sample under study. The data of physical adsorption have been used for many years as the basis for methods to characterize the surface area and porosity of adsor- bents.
Page 345: Application To Surface Energy Distribution
TriStar II 3020 Appendix C Application to Surface Energy Distribution Under certain conditions, an energetically heterogeneous surface may be characterized by a distribu- tion of adsorptive energies. The conditions are that the sample is not microporous, i.e., that adsorption is taking place on essentially a free surface with no pore filling processes at least to about 0.2 relative pressure.
Page 346: Performing The Deconvolution
Appendix C TriStar II 3020 Performing the Deconvolution The integrations in equations (2) and (3) are carried out over all surface energies or pore sizes in the model. The functions q(p,ε) and q(p,H), which we call the kernel functions, are contained in numeric form as model isotherms.
Page 347: Spc Report Variables
TriStar II 3020 Appendix C SPC Report Variables Regression Chart Variables The line of best fit for the Regression Chart is calculated by the usual Least Squares method. (Refer to BASIC Scientific Subroutines Vol II, by F.R. Ruckdeschel, Copyright 1981 BYTE Publications/ McGraw Hill, p.
Page 348: Control Chart Variables
Appendix C TriStar II 3020 Control Chart Variables  y --------- Mean  y Mean   – ----------------------------------- - StdDev – StdDev ------------------ - CoefVar Mean  PlusNSig Mean n StdDev  – MinusNSig Mean n StdDev Summary Report...
Page 349 TriStar II 3020 Appendix C g.) BJH Cumulative Desorption h.) Adsorption Total Pore Volume i.) Desorption Total Pore Volume j.) t-Plot Micropore Pore Volume See t-Plot calculations k.) Dubinin-Radushkevich Micropore Surface Area See Dubinin-Radushkevich calculations l.) Dubinin-Radushkevich Monolayer Capacity See Dubinin-Radushkevich calculations m.) Dubinin-Astakhov Micropore Surface Area...
Page 350: References
Appendix C TriStar II 3020 References Savitzky, A. and Golay, M.J.E., Anal. Chem. 36, 1627 (1964). Brunauer, S.; Emmett, P.H.; and Teller, E., J. Am. Chem. Soc. 60, 309 (1938). Langmuir, I., J. Am. Chem. Soc. 38, 2267 (1916); J. Am. Chem. Soc. 40, 1361 (1918); Phys. Rev 8, 149 (1916).
Page 351: Ethernet Configuration
TriStar II 3020 Appendix D D. ETHERNET CONFIGURATION ® This section contains instructions for configuring an Ethernet port in either Microsoft Windows 7 or Windows Vista. The instructions do not apply to any other operating system. Windows 7 Professional is recommended for the best user experience.
Page 352 Appendix D TriStar II 3020 Click Network and Sharing Center. Click the Local Area Connection for your analyzer. 302-42828-01 - Dec 2012...
Page 353 TriStar II 3020 Appendix D Click Properties. Highlight Internet Protocol Version 4 then click Properties. 302-42828-01 - Dec 2012...
Page 354 Appendix D TriStar II 3020 Click Use the following IP address then enter the following in the IP address field:  192 168 77 100. The following numbers should display in the Subnet mask field: 255.255.255.0. If not, enter them. Leave all other fields blank.
Page 355: Windows Vista
TriStar II 3020 Appendix D Windows Vista Windows 7 Professional is recommended for the best user experience. Select the Windows icon from the Status bar at the bottom of the screen, then select Control Panel. Double-click Network and Sharing Center.
Page 356 Appendix D TriStar II 3020 Click Properties. Highlight Internet Protocol Version 4 then click Properties. Click Use the following IP address and enter the following in the IP address field: 192 168 77 100. The following numbers should display in the Subnet mask field: 255.255.255.0. If not, enter them.
Page 357: Free Space Correction
TriStar II 3020 Appendix E E. FREE SPACE CORRECTION Free space is that volume of the sample tube which is unoccupied by the sample. The quantity of gas dosed into the sample tube is calculated from the difference in pressures in the manifold before and after the dose is delivered.
Page 358: Calculate
Appendix E TriStar II 3020 This method may be undesirable if: • Helium is unavailable; free space determination by the TriStar requires the use of helium • Analysis speed is a major factor; a helium free space measurement of 10 to 15 minutes is required •...
Page 359: Dft Models
TriStar II 3020 Appendix F F. DFT MODELS Theories are developed by scientists in an attempt to explain a class of observed behavior. In the exper- imental physical sciences, theories are often expressed in terms of a model that can be visualized and described mathematically.
Page 360: Molecular Simulation Methods
Appendix F TriStar II 3020 If the equilibrium distribution of the gas atoms near the surface could be described as a function of pressure and the molecular properties of the components of the system, then a model could be con- structed for the adsorption isotherm for the system.
Page 361: Density Functional Formulation
TriStar II 3020 Appendix F If the move results in a configuration of higher energy, a probability for that event is calculated, and a random number between zero and one is generated. If the generated number is smaller than the proba- bility of the event, then the move is accepted;...
Page 362 Appendix F TriStar II 3020 Figure D-1. Density Profile for Argon on Carbon at 87.3 K and a Relative Pressure of 0.5 This figure represents a cross-section of the region near the surface. Note the layerwise distribution of adsorbate; the first monolayer is sharply defined and a third layer can be distinguished. The area under the profile curve represents the amount adsorbed per unit area at this pressure.
Page 363 TriStar II 3020 Appendix F Figure D-2. Model Isotherm for Argon at 87.3 K in a 40 Å Slit in a Carbon Substrate The profiles show the density distribution from one wall to the center of the slit; the other half of the distribution is a mirror image of the profile shown.
Page 364 Appendix F TriStar II 3020 Figure D-3. Model Isotherms for Some Larger Pore Widths Argon on Carbon at 87.3 K Figure D-4 shows model isotherms for pores in the micropore size range. Note the logarithmic scale for pressure. Figure D-4. Model Isotherms in the Micropore Size Range of Pore Width Argon on Carbon at 87.3 K...
Page 365: Models Included
TriStar II 3020 Appendix F Pores of 4 Å width, barely larger than the argon atom (3.38 Å), fill at pressures below 1 millitorr. Pores below 15 Å fill before a monolayer is completed on the surface of the larger pores. In the micropore size range, the pore volume fills more gradually with pressure and the total shape of the isotherm is important in characterizing the pore size.
Page 366 Appendix F TriStar II 3020 N2 - Cylindrical Pores - Oxide Surface AR - Cylindrical Pores - Oxide Surface Cylinder Geometry Oxide Substrate Porosity Category: Nitrogen at 77 K; Argon at 87 K Method: Model isotherms were calculated using a combination of statistical mechanical calculations and exper- imental observations for macroporous silicas and MCM-41 mesoporous silicas as well as zeolites.
Page 367 TriStar II 3020 Appendix F Mietec Jaroniec, Michal Kruk, James P. Olivier and Stefan Koch, “A References: New Method for the Characterization of Mesoporous Silicas,” Proceedings of COPS-V, 1999, Studies in Surface Science, Vol 128, Characterization of porous Solids V , Unger, et al, Eds, Elsevier, Amsterdam, 2000.
Page 368 Appendix F TriStar II 3020 Oxide Substrate Porosity Category: Nitrogen at 77 K Method: Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting functions and a cylindrical pore geometry. The wall potential used is k = 30 K, typical for a silica or alumina surface.
Page 369 TriStar II 3020 Appendix F Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting functions assuming 2D model of finite slit pores having a diameter-to-width aspect ratio of 6. This model is particularly useful for microporous carbon materials. The reported pore size range is from 3.5 to 250 Å.
Page 370 Appendix F TriStar II 3020 This model is particularly useful for characterizing carbon single-wall nanotubes. The reported pore size range is from 3.5 to 1000 Å. P. Tarazona, Phys. Rev. A 31: 2672 (1985). Reference: Idem, Phys. Rev. A 32: 3148 (1985)....
Page 371: Models Based On Classical Theories
TriStar II 3020 Appendix F Ar - Zeolites Me-Form by NLDFT Cylinder Geometry Zeolite Substrate Porosity Category: Argon at 77 K Method: Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting functions and cylindrical pore geometry. The pore wall potential is described by the Lennard-Jones potential of interaction between a gas molecule and the oxide surface of an infinitely long cylinder.
Page 372: Models Included
Appendix F TriStar II 3020 quently leads to inconsistencies when carried to small mesopore sizes. If the thickness curve used is too steep, it finally will predict a larger increment of adsorptive for a given pressure increment than is actually observed; since a negative pore volume is non-physical, the algorithm must stop. Conversely, if the thickness curve used underestimates film thinning, accumulated error results in the calculation of an overly large volume of (possibly nonexistent) small pores.
Page 373: Kelvin Equation With Harkins And Jura Thickness Curve
TriStar II 3020 Appendix F Kelvin Equation with Harkins and Jura Thickness Curve N2 - Harkins and Jura Thickness Curve Slit Geometry Average Substrate Porosity Category: Nitrogen at 77 K Method: The kernel function is calculated using the Harkins and Jura equation with standard parameters: 13.99...
Page 374: Kelvin Equation With Broekhoff-De Boer Thickness Curve
Appendix F TriStar II 3020 Kelvin Equation with Broekhoff-de Boer Thickness Curve N2 - Broekhoff-de Boer Model Slit Geometry Average Substrate Porosity Category: Nitrogen at 77 K Method: The kernel function is calculated using the Broekhoff-de Boer equation with standard parameters: –...
Page 375: References
“Determination of Pore Size Distribution from Density Functional Theoretic Models of Adsorption and Condensation within Porous Solids,” J.P. Olivier and W.B. Conklin, Micromeritics Instrument Corp; presented at the International Symposium on the Effects of Surface Heterogeneity in Adsorption and Catalysts on Solids, Kazimierz Dolny, Poland (July 1992).
Page 376 Appendix F TriStar II 3020 F-18 302-42828-01 - Dec 2012...
Page 377: Maintaining High Purity Gases
Appendix G G. MAINTAINING HIGH PURITY GASES The TriStar II 3020 was designed to accurately measure the surface area of all types of materials. It is important that the gases (especially Krypton when using the Krypton option) used for these measure- ments be of highest purity, especially when analyzing low surface area samples.
Page 378: Purge Method
Appendix G TriStar II 3020 Purge Method This is the preferred method for removing trapped air. Select Unit > Enable manual control (if the instrument schematic is not displayed, select Show instrument schematic). If multiple TriStars are installed, make sure to choose the correct Unit menu.
Page 379: Evacuation Method
TriStar II 3020 Appendix G Using the Pressure Control knob, set the output pressure (gas bottle pressure gauge) to 15 psig. Loosen the fitting at the helium inlet (on the rear panel of the TriStar) until the low pressure side drops to approximately 3 psig (0.02 MPa), then tighten the fitting.
Page 380 Appendix G TriStar II 3020 Close all valves; then open valves 6, 7, and 10. Open valves 6, 7, Allow evacuation to continue for 20 minutes. This pulls a vacuum on the helium line to the gas bottle. The manifold pressure transducer should fall close to zero.
Page 381 TriStar II 3020 Index INDEX AR Cylindrical Pores - Oxide Surface model, F-8 AR DFT model, F-7 Absolute pressure dosing, 5-25 AR Modified Density Functional Model, F-9 Absolute pressure tolerance, 5-17 Argon Cylinder, multi-wall nanotube by NLDFT model, Accessories, ordering, 10-1...
Page 382 Index TriStar II 3020 Cheng/Yang leak test, 9-15 calculations, C-22 Dollimore-Heal Adsorption/Desorption report, 5-49 Pore Geometry, C-21 Dubinin Cleaning calculations, C-27 analyzer, 9-4 report, 5-57 Dewar, 9-4 tabular report options, 5-58 Close reports command, 7-3 transformed isotherm plot options, 5-59...
Page 383 TriStar II 3020 Index Report options command, 5-26 Harkins and Jura thickness curve, 5-39 Sample information files command, 5-8 Heat of Adsorption report, 7-10 Sample tube command, 5-10 Help menu Save, 5-4 Micromeritics web page, 2-11 Save All, 5-6 online...
Page 384 Index TriStar II 3020 MP-Method report calculations, C-33 Main menu bar, 2-9 MP-Method report, 5-61 Maintenance plot options, 5-62 troubleshooting, 9-1 tabular report options, 5-62 system, 9-1 videos, 2-11 Manual control accessing shortcut menu, 6-11 N2 Broekhoff-de Boer model, F-16...
Page 385 TriStar II 3020 Index Preparing file status, 2-7 Report, Validation, 5-64 Pressure Reports menu absolute pressure dosing, 5-25 close reports command, 7-3 absolute pressure tolerance, 5-17 control chart command, 7-7 offset, 6-19 heat of absorption report command, 7-10 relative, calculations, C-1...
Page 386 Index TriStar II 3020 create file, 3-11 Subnet mask file, 5-10 entering, Windows 7, D-4 How to Install Sample Tubes, video, 2-11 entering, Windows Vista, D-6 installing, 3-21 Summary report, 5-28 schematic, 6-9 calculations, C-40 replacing O-ring, 9-6 Surface area correction...
Page 387 TriStar II 3020 Index show instrument schematic command, 6-12 Zeolites Me-Form by NLDFT model, F-13 show status command, 6-13 Zero pressure calibration, 6-19 unit configuration, 6-15 Zoom feature, 7-23 Units, Options menu, 8-3 Vacuum pump changing or adding oil, 9-7...
Page 388 Index TriStar II 3020 Index-8 302-42828-01 - Dec 2012...
Page 389 MART NTELLIGENT ACUUM AMPLE REPARATION YSTEM PERATOR ANUAL 067-42800-01l Dec 2013...
Page 390 Smart VacPrep is a registered trademark of Micromeritics Instrument Corporation. _____________________________________________________________________________________ © Micromeritics Instrument Corporation 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...
Page 391 About this Manual BOUT THIS ANUAL The following icons and format may be used throughout this manual to identify notes of importance, warnings, and cautions. NOTE - Notes contain important information pertinent to the subject matter. CAUTION - Cautions contain information to help prevent actions that may damage the ana- lyzer or components.
Page 392 About this Manual Field Labels and Screen Titles Labels and Buttons Description Buttons (in the applic- Buttons in the application are represented as bold font weight and blue let- ters. Some examples are: Save, Edit, Replace All, etc. ation) Buttons (on the equip- Buttons on the equipment are represented as bold font and black letters.
Page 393 Contact Us ONTACT Micromeritics Instrument Corporation 4356 Communications Drive Norcross, GA 30093-2901, U.S.A. Phone: (770) 662-3636 Fax: (770) 662-3696 www.Micromeritics.com --------------- U.S. Inquiries U.S. Sales: (770) 662-3636 ussales@micromeritics.com --------------- Quotes, Orders, and Customer Satisfaction Customer Service: (770) 662-3636 Orders@Micromeritics.com --------------- U.S. Instrument Service Department Phone: (770) 662-3666 Smart VacPrep Operator Manual —...
Page 395 Table of Contents About this Manual Contact Us 1 About the Smart VacPrep 1 - 1 Specifications for the Smart VacPrep 1 - 3 Set the Voltage for the Smart VacPrep 1 - 3 2 About the Smart VacPrep Software 2 - 1 Add or Remove a Smart VacPrep 2 - 1 Add a Smart VacPrep unit...
Page 396 Schedule Smart VacPrep Diagnostic Test 5 - 1 6 Maintenance and Troubleshooting 6 - 1 Enable Manual Control for Smart VacPrep 6 - 1 Replace the Smart VacPrep Fuse 6 - 2 Sample Tube Installation on the Smart VacPrep 6 - 2 Oil Based Vacuum Pump 6 - 3 Inspect and Change Vacuum Pump Oil...
Page 397 1 About the Smart VacPrep BOUT THE MART The Smart VacPrep is an advanced six-port degassing system that utilizes vacuum to degas samples by heating and evacuation. Each of the ports may be operated independently of one another. Samples may be added or removed from degas ports without disturbing the treatment of other samples undergoing preparation.
Page 398 1 About the Smart VacPrep QuickStart menu option and Smart VacPrep panel buttons. Accessed from the Smart VacPrep > menu selection. Provides the option to enter commonly used Unit [n] > QuickStart Degas Conditions degas conditions for each Smart VacPrep port without the need for a sample information file. This option provides three ways to load information into QuickStart Degas Conditions: 1.
Page 399 Specifications for the Smart VacPrep PECIFICATIONS FOR THE MART The Smart VacPrep degasser has been designed and tested to meet the following specifications: Specifications for the Smart VacPrep Specification Description Automatically backfill or wait for user command Backfill Options Capacity 6 ports Heat and vacuum Degas Method...
Page 401 If a software update is required for the analyzer to support the Smart VacPrep, the software can be downloaded from the internet at this location: http://www.micromeritics.com/Smart-VacPrep-Software.aspx The degasser software is installed as a part of the analyzer installation. During installation, an IP address will be assigned to the unit allowing the unit to connect automatically during startup.
Page 402 2 About the Smart VacPrep Software DD A MART REP UNIT Smart VacPrep > Add 1. When prompted, enter the serial number of the unit being added. Duplicate serial numbers are not allowed. 2. Click Add. Initialization begins. EMOVE A MART REP UNIT Smart VacPrep > Remove 1.
Page 403 Click to display the Unit IP Setup window. The IP address and Subnet Change IP mask assigned during installation display. Do not edit these fields unless instructed by a Micromeritics service representative. Saves and closes the active window. Remove 067 Unit Click to remove the selected Smart VacPrep unit.
Page 405 3 Operate the Smart VacPrep PERATE THE MART ACKFILL THE MART ORTS Smart VacPrep > Unit [n] > Backfill Ports Use to backfill ports with gas. 1. Enter the backfill pressure in the Backfill pressure field. 2. Select the ports to be backfilled. 3.
Page 406 3 Operate the Smart VacPrep Smart VacPrep Evacuate Ports Fields and Buttons Field or Button Description Cancel Discards any changes or cancels the current process. Evacuate Options Unrestricted evac. pressure. Pressure value at which unrestricted sample evacuation should begin. Vacuum level. Specify the vacuum level to be achieved before evac- uation begins.
Page 407 QuickStart Degas Conditions 1. Go to Smart VacPrep > Unit [n] > QuickStart Degas Conditions 2. The six ports are represented by row numbers. Ports that are busy are grayed out and disabled. Edit Click for the port to be configured. 3. Enter degas conditions using one of the following methods: To select degas conditions from a Degas Conditions file, click the dropdown arrow to the right of the Degas Conditions field.
Page 408 3 Operate the Smart VacPrep 10. Install the safety shield. 11. Press the Select button for the port to be degassed. A blue LED is lit. 12. Press the Start button on the Smart VacPrep panel to start the degas process for all ports that have a blue LED lit.
Page 409 Start Smart VacPrep Degas Degas Conditions Fields and Buttons Table (continued) Field or Button Description Save Saves changes to the active window. This option is applicable only when degassing with a Smart VacPrep. Smart VacPrep Evac- uation Backfill sample tube. Indicate if the sample tube should be backfilled automatically or wait for operator response.
Page 410 3 Operate the Smart VacPrep Degas conditions remain the same from degas to degas unless the Degas Conditions file is changed or replaced by the operator. A manual evacuation can be performed on any idle degas port. The six ports are represented by row numbers. Ports that are busy are grayed out and disabled. Browse 1.
Page 411 Show Smart VacPrep Dashboard MART ASHBOARD Smart VacPrep > Unit [n[ > Show Dashboard The dashboard displays the following: Number of days until roughing pump maintenance is due Manifold outgas rate Data for the dashboard comes from the logged diagnostic data. The dashboard is automatically kept current as the relevant diagnostic data items are updated.
Page 412 3 Operate the Smart VacPrep Smart VacPrep Dashboard Gauges and Descriptions Table (continued) Field or Button Description turned on. At 110% and above, only the red LED is lit and attention is required. MART Smart VacPrep > Unit [n] > Show Log Use to display a log of recent analyses, calibrations, or messages. Analyzer Log Fields and Buttons Table Field Description...
Page 413 Show Smart VacPrep Schematic Analyzer Log Fields and Buttons Table (continued) Field Description File. Select the destination directory. Enter a new file name in the File name field, or accept the default. Select to save the file as a report sys- tem (.REP), a spreadsheet (.XLS), a portable document format (.PDF), or an ASCII text (.TXT) file format.
Page 414 3 Operate the Smart VacPrep Smart VacPrep Schematic Components Table Schematic Description Components Sample port valves 7, 8, 9 Vacuum and backfill valves Heating mantle con- Sets the ramp rate and target temperature trols MART CHEMATIC HORTCUT ENUS Each manually controlled schematic component has a shortcut menu displaying the operations available for that particular component.
Page 415 Show Smart VacPrep Status MART TATUS Smart VacPrep > Unit [n] > Show Status The Smart VacPrep Status window allows the monitoring of degas operations for a manual degas operation. Smart VacPrep Status Fields and Buttons Table Field or Button Description Cancels the current degas operation.
Page 417 Smart VacPrep > Unit [n] > Calibration > Pressure Offset Use to perform system calibration. This option evacuates the system and zeros the pressure transducer. Disabled calibration options can be accessed only with the assistance of an authorized Micromeritics service representative. Start Click to begin the process.
Page 418 4 Smart VacPrep Calibration Use to calibrate the servo valve to the manifold pressure transducer. The servo valve should always be recalibrated after a pressure calibration has been performed. The pressure transducer should be calibrated before starting this calibration procedure. 1.
Page 419 5 Smart VacPrep Diagnostics MART IAGNOSTICS IAGNOSTIC EPORT FOR MART Smart VacPrep > Unit [n] > Diagnostics > Diagnostic Test Report Displays previously run diagnostic tests. Separate directories store tests run once, daily, weekly, and monthly. CHEDULE MART IAGNOSTIC Smart VacPrep > Unit [n] > Diagnostics > Schedule Diagnostic Tests Allows the specification of one-time or periodic running of a sequence of diagnostic tests.
Page 420 5 Smart VacPrep Diagnostics Schedule Diagnostics Fields and Buttons Table Field or Button Description Available Tests drop- Select one or more tests to run unattended. Select the test and click the down list Insert button for the test to display in the Test Sequence box. Cancel Discards any changes or cancels the current process.
Page 421 6 Maintenance and Troubleshooting AINTENANCE AND ROUBLESHOOTING NABLE ANUAL ONTROL FOR MART Smart VacPrep > Unit [n] > Enable Manual Control Use to enable the manual control of certain system valves and elevator components. When this option is enabled, a checkmark appears to the left of Unit [n] >...
Page 422 6 Maintenance and Troubleshooting Smart VacPrep Schematic Components Icon Table (continued) Field or Button Description Servo Valve. Open. Sample Tube. Cannot be manually controlled. EPLACE THE MART The Smart VacPrep uses two 5 amp fuses located in a compartment adjacent to the power connector on the back of the unit.
Page 423 Oil Based Vacuum Pump 3. If using a Check Seal, verify that the Check Seal opener is installed in the sample port. 4. To attach the sample tube set to the degas port, push the sample tube in to a full stop. Secure the sample tube in place by sliding the connector nut, ferrule, and O-ring up onto the degas port and turning the connector nut clockwise.
Page 424 Change or Add Oil Drain the oil while the pump is warm and disconnected from the power source. Use oil supplied by Micromeritics or refer to the vacuum pump manual for other acceptable oils. 1. Unplug the vacuum pump from the power source.
Page 425 Inspect and Change Vacuum Pump Oil 3. Grasp the handle on top of the vacuum pump and place the pump on a work surface. 4. Place a waste container under the drain spout. 5. Remove the drain plug and drain the oil into the waste container. 6.
Page 426 6 Maintenance and Troubleshooting Do not allow oil to rise above the midway position when the pump is running. Doing so may cause oil to splash into the oil filter causing contamination. 9. Check the washer or O-ring used at the oil-filling port and replace if necessary. 10.
Page 427 Replace the Alumina in the Oil Vapor Trap 1. Disconnect the vacuum pump from the analyzer and place it on a work table. 2. Loosen the wing nut on the clamp at the top of the oil vapor trap. Swing the clamp open and remove the trap from the hose.
Page 428 6 Maintenance and Troubleshooting Prepare fresh alumina 1. Preheat the oven to 300 °C. 2. Pour approximately 180 grams of fresh alumina into a glass or metal container (approximately 250 mL if a graduated beaker is used). Place the container in the oven. 3.
Page 429 Replace the Alumina in the Oil Vapor Trap 11. Inspect the centering ring before replacing it onto the intake port. If it appears to be flattened, replace it. A flattened centering ring can cause vacuum leaks. There are two types of centering rings.
Page 430 6 Maintenance and Troubleshooting 15. Reconnect the hose from the analyzer to the oil vapor trap. a. Place the clamp around the vacuum pump hose flange and vapor trap. 16. Plug the pump power cord into the power source. Allow the pump to run a few hours (overnight if possible) to eliminate air and moisture from the fresh oil and to produce efficient vacuum operations.
Page 431 Replace the Vacuum Pump Exhaust Filter 1. Turn off the power to the pump and disconnect the pump from the power source. 2. Loosen the clamp wing nut at the vacuum pump exhaust port. Swing the clamp away from the exhaust port and remove it.
Page 433 7 Parts and Accessories for the Smart VacPrep ARTS AND CCESSORIES FOR THE MART Part Number Item and Description Cables 003-63801-01 Cable, Ethernet straight-thru; for connecting instrument to control module (computer) Gas Cylinder Accessories 004-25549-00 Reducer, 1/8 in tube × 1/4 in tube 004-33601-00 Expansion kit;...
Page 434 7 Parts and Accessories for the Smart VacPrep Part Number Item and Description Option kit, 3/8 in. ferrules and O-rings (6 ferrules and 12 O-rings) 067-33604-00 067-33605-00 Option kit, 9 mm ferrules and O-rings (6 ferrules and 12 O-rings) 260-25843-00 Sample tube ferrule, 1/2 in 300-25824-00 Sample tube nut...
Page 435 RROR ESSAGES Program error messages are listed numerically. If the Action response indicates to contact a Micromeritics service representative, record the error message, then make backup copies of any files involved in the operation. 4407 Error searching for installed Smart VacPreps. The registry could not be read..
Page 436 Cause: The temperature of the indicated mantle exceeded the maximum allowed value. Action: Ensure the power and thermocouple connectors for the mantle are properly installed. If they are, the mantle may be defective; contact your Micromeritics service rep- resentative. 4414 Error thermocouple unplugged on port [0].
Page 437 8 Error Messages 4422 The file %s does not exist. Cause: The selected file does not exist on the disk drive. Action: Select an existing file. Ensure that the file has been created before use. 4423 The sample %s is already selected on port %d. Cause: The selected sample file is already selected for use on a different port.
Page 439: Index
Index NDEX Schematic shortcut menus 3 - 10 Servo valve About this manual iii SmartVacPrep, calibrate 4 - 1 Shortcuts schematic 3 - 10 Smart VacPrep calibrate servo valve 4 - 1 Calibration calibrate, pressure offset 4 - 1 Smart VacPrep 4 - 1 calibration 4 - 1 Smart VacPrep, pressure offset 4 - 1 diagnostic test report 5 - 1...

Micromeritics TriStar II 3020 Operator's Manual

1 General Information

2 User Interface

3 Operating Procedures

4 Software and Setup Modifications

5 File Menu

6 Unit Menu

7 Reports Menu

8 Options Menu

9 Troubleshooting and Maintenance

10 Ordering Information

Forms

Error Messages

Calculations

Ethernet Configuration

Free Space Correction

Dft Models

Maintaining High Purity Gases

Index

Quick Links

Need help?

Questions and answers

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Summary of Contents for Micromeritics TriStar II 3020