Page 1 ® II P URFACE REA AND OROSITY NALYZER PERATOR ANUAL 303-42800-01 Sep 2023 (Rev M )
Page 2 Copyright The software described in this manual is furnished under a license agreement and may be used or copied only in accordance with the terms of the agreement. ____________________________________________________________________________ Copyright © 2013 - 2023. Micromeritics Instrument Corporation. All rights reserved.
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 4 The company has R&D and manufacturing sites in the USA, UK, and Spain, and direct sales and service operations throughout the Americas, Europe, and Asia. Micromeritics systems are the instruments-of-choice in more than 10,000 laboratories of the world’s most innovative companies and prestigious government and academic institutions.
Page 5 4356 Communications Drive Norcross, GA 30093-2901 USA Phone: 1-770-662-3636 Fax: 1-770-662-3696 www.Micromeritics.com Instrument Service or Repair Phone: 1-770-662-3666 International: Contact your local distributor or call 1-770-662-3666 Service.Helpdesk@Micromeritics.com Micromeritics Application Support Support@Micromeritics.com TriStar II Plus Operator Manual 303-42800-01 (Rev M ) — Sep 2023...
Page 6: About This Manual
About this Manual BOUT THIS ANUAL The following can be found on the Micromeritics web page (www.micromeritics.com). Calculations document (PDF) Parts and Accessories Error Messages document (PDF) Smart VacPrep Operator Manual (PDF) Operator Manual (PDF) Vacuum Pump Guide (PDF) This manual contains instructions for installations in standard and 21CFR11 environments.
Page 7: General Safety
The 3030 TriStar II Plus sound level is below 80 dBA. Hearing protection is optional. The 3030 TriStar II Plus has a safety shield. Ensure it is in place when operating the instrument. Proper maintenance is critical to personnel safety and smooth instrument operation and performance.
Page 8 TriStar II Plus provides high sample throughput and advanced data analysis features to the user. The TriStar II Plus software gives the user the ability to interactively evaluate isotherm data and reduce the time required to obtain surface area and porosity results.
Page 9 EFUP (for example, battery modules) and are marked to reflect such. The Environmentally Friendly Use Period is valid only when the product is operated under the conditions defined in the product manual. TriStar II Plus Operator Manual 303-42800-01 (Rev M ) — Sep 2023...
Page 10 Read the Safety Data Sheet (SDS) and be aware of the hazards of mercury and know what to do in the event of a spill or an exposure incident. TriStar II Plus Operator Manual viii 303-42800-01 (Rev M ) — Sep 2023...
Page 11: Table Of Contents
2 - 22 Export Files 2 - 23 List Files 2 - 24 Software Uninstall 2 - 25 Software Updates 2 - 25 Software in 21CFR11 Environments 2 - 26 TriStar II Plus Operator Manual 303-42800-01 (Rev M ) — Sep 2023...
Page 12 6 - 15 Perform a Sample Analysis 6 - 17 Perform a Sample Tube Free Space Analysis 6 - 20 Perform an Empty Tube Analysis 6 - 23 TriStar II Plus Operator Manual 303-42800-01 (Rev M ) — Sep 2023...
Page 13 8 - 4 BET Surface Area Report 8 - 6 BJH Adsorption/Desorption Report 8 - 8 DFT Pore Size Report 8 - 14 DFT Surface Energy Report 8 - 17 TriStar II Plus Operator Manual 303-42800-01 (Rev M ) — Sep 2023...
Page 14 Guidelines for Connecting Gases 11 - 4 Replace a Gas Cylinder 11 - 5 Clean and Verify the Gas Line 11 - 9 Enable Manual Control 11 - 11 TriStar II Plus Operator Manual 303-42800-01 (Rev M ) — Sep 2023...
Page 15 B - 1 Models Based on Classical Theories B - 13 DFT Model References B - 16 C Free-Space Correction C - 1 D Maintain High-Purity Gases D - 1 TriStar II Plus Operator Manual xiii 303-42800-01 (Rev M ) — Sep 2023...
Page 16 Sample Data Worksheet for Gas Adsorption E - 1 F Exported Data Example F - 1 TriStar II Plus EU Declaration of Conformity DoC - 1 TriStar II Plus Operator Manual 303-42800-01 (Rev M ) — Sep 2023...
Page 17: Analyzer Components For Tristar Ii Plus
During analysis, the elevator optionally lowers after the free space measurement to allow evacuation, then is raised and continues the analysis. TriStar II Plus Operator Manual 1 - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 18 B. RS-232 port Component Description Port for a shielded Ethernet cable allowing communication between Ethernet Port the analyzer and the computer. Not used. RS-232 port TriStar II Plus Operator Manual 1 - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 19 Gas inlet valves Inlet valves for analysis gases. Power cord For connecting the analyzer to the power supply and for powering the connector analyzer on and off. and power switch TriStar II Plus Operator Manual 1 - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 20: Equipment Options And Upgrades
Dewar and the recirculating liquids. The Chiller Dewar Quick Start Guide is located on the Micromeritics web page. The FlowPrep applies both heat and a stream of inert gas to the...
Page 21 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).
Page 22: Gas Requirements And Purity
Appropriate two-stage regulators which have been leak-checked and specially cleaned are required. Pressure relief valves should be set to no more than 30 psig (200 kPag). All gases should be of a purity listed below. Gas regulators can be ordered from Micromeritics. Parts and accessories are located on the Micromeritics web page.
Page 23: Specifications For The Tristar Ii Plus
Same as nitrogen unit, plus the capability to perform krypton sur- Krypton Unit face area analyses at lower pressures The TriStar II Plus should be operated in a properly vented environment when using flammable or toxic gases. TriStar II Plus Operator Manual 1 - 7 303-42800-01 (Rev M ) —...
Page 24 Degree of Ingress IPX0 Protection Physical Height 74 cm (29 in.) Width 40 cm (16 in.) Depth 51 cm (20 in.) Weight 37 kg (82 lbs) TriStar II Plus Operator Manual 1 - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 25 For 21 CFR Part 11 environments, permission may be limited to the installation directory. Drives USB port Due to continuous improvements, specifications are subject to change without notice. TriStar II Plus Operator Manual 1 - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 27: About The Software
In addition to customizable standard reports, user-defined calculations and reports can be created through the Advanced reports feature (using Python). Data can be manipulated and displayed interactively using MicroActive reports. TriStar II Plus Operator Manual 2 - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 28: Menu Structure
Use to manage open windows and display a list of open windows. A Window checkmark appears to the left of the active window. Use to access the embedded operator manual, Micromeritics web page, Help and information about the application. TriStar II Plus Operator Manual 2 - 2 303-42800-01 (Rev M ) —...
Page 29: Common Fields And Buttons
Selects the number of copies to print. This field is only enabled when Copies Print is selected. When working with tables, deletes the selected information. Delete Selects the report destination. Destination TriStar II Plus Operator Manual 2 - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 30 Print Removes the selected file or files from the list. Remove Selects another file where the values will replace the current file’s val- Replace ues. TriStar II Plus Operator Manual 2 - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 31 View Instrument Log. Displays recent analyses, calibrations, errors, or messages. Enabled only in Service Test Mode. Instrument Schematic. Displays a schematic of the analyzer system. TriStar II Plus Operator Manual 2 - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 32: File Status, Description, And Location
Sample files that are currently being used in an automatic degas oper- Preparing ation. This status is applicable only if using the Smart VacPrep degasser. TriStar II Plus Operator Manual 2 - 6 303-42800-01 (Rev M ) — Sep 2023...
Page 33 The density conversion factor in the adsorptive properties file is used to convert quantity adsorbed to volume of condensed adsorptive. TriStar II Plus Operator Manual 2 - 7 303-42800-01 (Rev M ) — Sep 2023...
Page 34: Keyboard Shortcuts
When in the File Selector window, opens the file search box. When in the File Selector window, opens the address bar. Opens the File Selector window listing report options files. Cascades open windows. TriStar II Plus Operator Manual 2 - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 35 Opens the shortcut menu of either the selected component on the ana- Shift + F9 lyzer schematic when manual control is enabled or the onscreen reports. TriStar II Plus Operator Manual 2 - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 36: Option Presentation
Enables (or disables) the splash screen upon application startup. Show Splash Screen To change the view for the selected window, use the drop-down list at the bottom of the sample file editor. TriStar II Plus Operator Manual 2 - 10 303-42800-01 (Rev M ) — Sep 2023...
Page 37 A sample file must be created for each analysis. The file can be created prior to or at the time of analysis. The sample file identifies the sample, guides the analysis, and specifies report options. TriStar II Plus Operator Manual 2 - 11 303-42800-01 (Rev M ) — Sep 2023...
Page 38: Libraries
However, when deleting files or folders from within a library, they are deleted from their original file storage location. Deleted files and folders can be recovered from the Recycle Bin located on the Windows desktop. TriStar II Plus Operator Manual 2 - 12 303-42800-01 (Rev M ) — Sep 2023...
Page 39: Methods
The Method drop-down list displays only those methods applicable to the open sample file type. Developer Group view in a 21CFR environment Default Method Examples Default Method Examples TriStar II Plus Operator Manual 2 - 13 303-42800-01 (Rev M ) — Sep 2023...
Page 40 Specify a default numeric string to use as a prefix in the Sample field Sequence number when a new sample file is created. This number increments with [text box] each sample file created. TriStar II Plus Operator Manual 2 - 14 303-42800-01 (Rev M ) — Sep 2023...
Page 41: Configure The Analyzer
Change IP. Displays the Board ID dialog, which describes the circuit boards in the analyzer. Use the Board drop-down list to select a board to view. TriStar II Plus Operator Manual 2 - 15 303-42800-01 (Rev M ) — Sep 2023...
Page 42: Unit Selection
Use to specify how data should appear on the application windows and reports. This menu option is not available if using Restricted option presentation in a standard installation environment. TriStar II Plus Operator Manual 2 - 16 303-42800-01 (Rev M ) — Sep 2023...
Page 43: Instrument Status
When the displayed value is 30 or less, the value is dis- played in red. Red negative numbers display if maintenance is past due. TriStar II Plus Operator Manual 2 - 17 303-42800-01 (Rev M ) — Sep 2023...
Page 44 The mean, two-sigma, minimum, and maximum values display. The gauge is updated when a P logged with nitrogen as the adsorptive and a bath temperature of 77±2 K. TriStar II Plus Operator Manual 2 - 18 303-42800-01 (Rev M ) — Sep 2023...
Page 45: Show Instrument Log
Select the logs to display. Analysis/ Calibration/ Message [check box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 2 - 19 303-42800-01 (Rev M ) — Sep 2023...
Page 46 Closed Valve. Yellow indicates a closed valve. When manual control is disabled, closed valves appear white. Servo Valve. Closed. Servo Valve. Open. Elevator. Sample Tube. Cannot be manually controlled. TriStar II Plus Operator Manual 2 - 20 303-42800-01 (Rev M ) — Sep 2023...
Page 47: Show Instrument Schematic
Lower. Select Lower to lower the elevator. When it is moving, press the keyboard space bar to stop the movement (or right-click and select Stop from the menu). Stop. Stops the elevator from moving. TriStar II Plus Operator Manual 2 - 21 303-42800-01 (Rev M ) — Sep 2023...
Page 48: Show Status
Converts StarDriver files (.MGD extension) to a sample file with a .SMP file extension. Only those files with a .MGD file extension display in the Name column. TriStar II Plus Operator Manual 2 - 22 303-42800-01 (Rev M ) — Sep 2023...
Page 49: Export Files
1. Click List and open an .SMP file. 2. Select an experiment and the applicable options. 3. Click OK. TriStar II Plus Operator Manual 2 - 23 303-42800-01 (Rev M ) — Sep 2023...
Page 50: List Files
Select one or more files from the file selector, click List, then provide the file destination. Example of File List TriStar II Plus Operator Manual 2 - 24 303-42800-01 (Rev M ) — Sep 2023...
Page 51: Software Uninstall
Micromeritics application are correctly installed. If UAC is not enabled, right-click the setup.exe installer file and select Run as administrator. The most current version of the instrument software can be found on the Micromeritics web page (www.micromeritics.com).
Page 52 Windows 10 Professional or Windows 10 Enterprise or higher. Management of users and groups is performed in Windows Users and Groups. The Micromeritics Confirm application enables laboratory managers to develop analysis methods, enforce industry standards, and produce audit trails. It also enables laboratory analysts to perform analyses and produce reports.
Page 53: Software In 21Cfr11 Environments
Developer Group mic_[analyzer model number]_developer. Members of the Developer group: have rights to all functions of the Micromeritics application - includ- ing Advanced option presentation which allows the creation and modification of methods, sample files, and parameter files. can run an analysis.
Page 54 Select either Advanced (when in Basic view) or Basic (when in Advanced view). Advanced view / Developer group Basic view / Analyst group TriStar II Plus Operator Manual 2 - 28 303-42800-01 (Rev M ) — Sep 2023...
Page 55 Provides the option to create and name a new folder in the Confirm application folder. This option may not be available depending on how the IT Administrator configures Windows permissions. TriStar II Plus Operator Manual 2 - 29 303-42800-01 (Rev M ) — Sep 2023...
Page 56: Uninstall Software In 21Cfr11 Environments
To uninstall the software, double-click the uninstall.exe file located in the software installation directory, then follow the prompts. To uninstall the Micromeritics Confirm application, the owner of the application directory and its contents must be set to the account of the administrator that is removing the application installation.
Page 57: Sample Files
To change the view for the selected window, use the drop-down list at the bottom of the sample file editor. TriStar II Plus Operator Manual 3 - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 58: Create Sample Files
Sample Tube parameters are edited on the Sample Description tab. The Degas Conditions tab displays only if enabled in Options > Option Presentation > Show Degas Conditions TriStar II Plus Operator Manual 3 - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 59 Bar Code [text box] * sample lot number, sample ID, etc. Enter comments to display in the report header about the sample or Comments [text box] analysis. TriStar II Plus Operator Manual 3 - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 60 Common Fields and Buttons on page 2 - * This field label may have been renamed or may not display if modified in Options > Default Methods. TriStar II Plus Operator Manual 3 - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 61: Open A Sample File
Prepared Tabbed file editor No Analysis Complete Analyzing MicroActive report window Entered File Editor Example for CFR21 Advanced or Developer view Basic or Analyst view TriStar II Plus Operator Manual 3 - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 62 To view the tabbed file editor for a sample file with a Complete status, select Advanced from the view selector drop-down list at the bottom of the window. In 21CFR11 environments, this feature is applicable to members of the Developer group only. TriStar II Plus Operator Manual 3 - 6 303-42800-01 (Rev M ) — Sep 2023...
Page 63: Manually Enter Data
3. Open another sample file using the Advanced option presentation. 4. On the Sample Description tab, select Manually entered in the Type of Data group box. TriStar II Plus Operator Manual 3 - 7 303-42800-01 (Rev M ) — Sep 2023...
Page 64 5. In the view selector drop-down list at the bottom of the window, click Advanced, then select Isotherm. 6. Ensure that all parameter fields are set appropriately, then click Paste. TriStar II Plus Operator Manual 3 - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 65 Relative Pressure Quantity Adsorbed (cm3/g STP) 0.108629 50.6657 0.22288 60.7813 0.339909 71.3095 0.459512 84.4172 0.577447 102.672 0.654583 121.707 0.760074 179.096 0.855713 334.565 0.958511 394.675 0.996251 403.793 Silica Alumina : Desorption Relative Pressure Quantity Adsorbed (cm3/g STP) 0.996251 403.793 0.86016 389.626 TriStar II Plus Operator Manual 3 - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 66 3 Sample Files 0.753567 256.264 0.664418 133.099 0.542416 96.7366 0.422295 79.7351 0.346371 71.5994 0.2519 62.8256 0.152718 54.2336 0.103389 49.5803 TriStar II Plus Operator Manual 3 - 10 303-42800-01 (Rev M ) — Sep 2023...
Page 67 5. Open the .TXT file. The data from the original sample file is imported and displayed. If an error message displays instead, verify that the .TXT file format is correct. TriStar II Plus Operator Manual 3 - 11 303-42800-01 (Rev M ) — Sep 2023...
Page 69: Parameter Files
The following file types can exist as part of the sample file as well as individual parameter files. Parameter File Types File Extension File Type .ADP Adsorptive Properties .ANC Analysis Conditions .DEG Degas Conditions .MTH Method .RPO Report Options .STB Sample Tube TriStar II Plus Operator Manual 4 - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 70: Adsorptive Properties
Factor determined by obtaining the ratio of the gas density (STP) to Density conversion the liquid density. This field is disabled if Non-condensing Adsorptive factor [text box] is selected. where ρ gas density at STP TriStar II Plus Operator Manual 4 - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 71 Click to edit the Psat vs Temperature table. The table contains sat- Psat vs T [button] uration pressures and their corresponding temperatures. To edit, click in a field and enter the value. TriStar II Plus Operator Manual 4 - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 72 Estimate of the molecular size used in calculating the thermal Therm. tran. transpiration correction. hard-sphere diameter [text box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 4 - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 73: Analysis Conditions
Adsorptive Properties on page 4 - 2. Use to browse for an Analysis Conditions file that contains analysis Analysis Conditions condition parameters to be used in the analysis. [drop-down box] TriStar II Plus Operator Manual 4 - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 74 The ending relative pressure and the dose amount (entered or as the fraction of the previous quantity adsorbed) for each target range are shown. TriStar II Plus Operator Manual 4 - 6 303-42800-01 (Rev M ) — Sep 2023...
Page 75 Measure: Lower Dewar for evacuation. If the Dewar is to be lowered for evacuation, select this option and enter the length of time for evac- TriStar II Plus Operator Manual 4 - 7 303-42800-01 (Rev M ) — Sep 2023...
Page 76 Analysis free space. Empty sample tube gas capacity measured with the Dewar raised. Calculate. Use to have the free space measurement calculated using the sample and tube parameters. TriStar II Plus Operator Manual 4 - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 77 During desorption, this field is treated as a maximum volume decrement value. Absolute / Relative pressure tolerance. TriStar II Plus Operator Manual 4 - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 78 1. Analysis bath temperature (not used for krypton analyses). Measures the p on a continuous basis. Allows the meas- urement of each data point without slowing the analysis. TriStar II Plus Operator Manual 4 - 10 303-42800-01 (Rev M ) — Sep 2023...
Page 79 While leak testing slightly increases analysis time, it prevents the continuation of analysis and collection of erroneous data if a leak exists. TriStar II Plus Operator Manual 4 - 11 303-42800-01 (Rev M ) — Sep 2023...
Page 80 (strictly increasing pressures) followed optionally by one desorption branch (strictly decreasing pressures). For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 4 - 12 303-42800-01 (Rev M ) — Sep 2023...
Page 81: Degas Conditions
If using a FlowPrep or a VacPrep use the heating phase section for reference only. The Degas Conditions tab displays only if enabled in Options > Option Presentation > Show Degas Conditions. The Smart VacPrep Operator Manual can be found on the Micromeritics web page (www.micromeritics.com). TriStar II Plus Operator Manual 4 - 13 303-42800-01 (Rev M ) —...
Page 82 Time. How long the sample is to be held at the specified temperature before beginning to cool down. Temperature Ramp Rate. The rate at which the temperature will change while advancing to the hold temperature. TriStar II Plus Operator Manual 4 - 14 303-42800-01 (Rev M ) — Sep 2023...
Page 83 Vacuum level. Evacuation time starts when the vacuum level is reached. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 4 - 15 303-42800-01 (Rev M ) — Sep 2023...
Page 84: Report Options
PTIONS File > Open > [.RPO File] (or click the Report Options tab when in Advanced option presentation) The Calculations document can be found on the Micromeritics web page (www.micromeritics.com). Additional reports are available using the Reports menu. Use to specify report options for data collected from an analysis or manually entered data. Report Options files also help in customizing report details such as axis scale, axis range, column headings, and components of thickness curve equations.
Page 85 Select then enter a report title to appear on the report header. Show report title [check box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 4 - 17 303-42800-01 (Rev M ) — Sep 2023...
Page 86: Sample Tube
It [check box] is generally a good practice to use filler rods for samples having less than 100 square meters of total surface area. TriStar II Plus Operator Manual 4 - 18 303-42800-01 (Rev M ) — Sep 2023...
Page 87 Select the seal type to be used. Vacuum seal type [group box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 4 - 19 303-42800-01 (Rev M ) — Sep 2023...
Page 89: Degassing
Most solid materials absorb moisture and other contaminants when exposed to the atmosphere. The sample must be clean when an analysis is performed. The degas process heats the sample to remove the moisture and contaminants. The Smart VacPrep Operator Manual can be found on the Micromeritics web page (www.micromeritics.com). EGAS ON THE MART Equipment Options and Upgrades on page 1 - 4...
Page 90 13. Position the Dewar cover approximately 3/4 in. (19 mm) below the sample port nut. 14. Slide the Psat tube into the Psat slot in the Dewar cover and retighten the Psat tube connector nut. TriStar II Plus Operator Manual 5 - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 91 B. Ferrule C. Connector nut D. Isothermal jacket 15. Install the Dewar onto the elevator and Close the sample compartment door. 16. Begin the analysis. TriStar II Plus Operator Manual 5 - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 93: Perform An Analysis
When pouring liquefied gases from one container to another: cool the receiving container gradually to minimize thermal shock pour the liquified gas slowly to prevent splashing vent the receiving container to the atmosphere TriStar II Plus Operator Manual 6 - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 94: For Glass Dewars
If the Dewar has a protective mesh covering, do not remove it. This cover minimizes the risk of flying particles should the Dewar be knocked over, dropped, or broken. TriStar II Plus Operator Manual 6 - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 95: Prepare For Analysis
4. 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 15 minutes. TriStar II Plus Operator Manual 6 - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 96 9. 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 before the sample tube is installed on the analysis port. TriStar II Plus Operator Manual 6 - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 97: Create The Sample File
Large granules or chunks may be loaded with forceps. Analysis results are expressed in units of surface area per gram of sample; therefore, it is important to know the true sample mass. TriStar II Plus Operator Manual 6 - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 98 Mass of the sample tube set with the sample. Subtract the Mass of empty sample tube set from the Mass of sample tube set plus sample. TriStar II Plus Operator Manual 6 - 6 303-42800-01 (Rev M ) — Sep 2023...
Page 99: Degas The Sample
3. Subtract the Mass of empty sample tube set (Before Degas) from the Mass of Sample tube set plus sample (After Degas) to obtain the sample’s mass. Record this value as Mass of sample (After Degas). TriStar II Plus Operator Manual 6 - 7 303-42800-01 (Rev M ) — Sep 2023...
Page 100: Sample Tube Installation
Dewar cover and slide the cover up. Ensure the tapered side of the cover is facing downward. 3. Insert the sample tube through one of the holes in the cover. TriStar II Plus Operator Manual 6 - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 101 Do not allow the sample tube connector nut drop onto the bottom of the tube as it may break the tube. Use the proper size frit for the sample port. The analyzer will not operate properly if an incorrect size is used. TriStar II Plus Operator Manual 6 - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 102 6. Slide the sample tube connector nut up the tube until it comes in contact with the port fitting (the ferrule and O-ring will move along with the connector nut). Then, turning clockwise, hand tighten the connector nut to the sample connector. TriStar II Plus Operator Manual 6 - 10 303-42800-01 (Rev M ) — Sep 2023...
Page 103: Fill And Install The Dewar
2. Insert the dipstick and check the level of the analysis bath liquid. Condensation should not exceed the level indicator mark. TriStar II Plus Operator Manual 6 - 11 303-42800-01 (Rev M ) — Sep 2023...
Page 104 TriStar II Plus Operator Manual 6 - 12 303-42800-01 (Rev M ) — Sep 2023...
Page 105: Perform A Krypton Analysis
Idle state at the bottom of the window. When analysis is complete, remove the sample tube and store (or dispose) of the sample material as applicable. TriStar II Plus Operator Manual 6 - 13 303-42800-01 (Rev M ) — Sep 2023...
Page 106 6 Perform an Analysis TriStar II Plus Operator Manual 6 - 14 303-42800-01 (Rev M ) — Sep 2023...
Page 107: Perform A Quickstart Analysis
Idle state at the bottom of the window. When analysis is complete, remove the sample tube and store (or dispose) of the sample material as applicable. TriStar II Plus Operator Manual 6 - 15 303-42800-01 (Rev M ) — Sep 2023...
Page 108 [drop-down box] selected for analysis conditions. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 6 - 16 303-42800-01 (Rev M ) — Sep 2023...
Page 109: Perform A Sample Analysis
If any selected sample file specifies an Adsorptive Dose Method from port 3 and a sample file is selected for port 3, an error message displays indicating the problem and the Start window will remain active. TriStar II Plus Operator Manual 6 - 17 303-42800-01 (Rev M ) — Sep 2023...
Page 110 Generates reports to the selected destination when the analysis is Report after analysis complete. [button] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 6 - 18 303-42800-01 (Rev M ) — Sep 2023...
Page 111 0.1 <= P < 10: 4 digits, P >= 10: 2 digits. Relative pressure will show 3 more digits than absolute pressure. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 6 - 19 303-42800-01 (Rev M ) — Sep 2023...
Page 112 After clicking Next, acknowledge that empty sample tubes have been installed on the selected ports by clicking Next again. Wait for the free space measurement to complete. TriStar II Plus Operator Manual 6 - 20 303-42800-01 (Rev M ) — Sep 2023...
Page 113: Perform A Sample Tube Free Space Analysis
This is used by the free space Calculate option. 2. Go to the Analysis Conditions tab and click Free Space. TriStar II Plus Operator Manual 6 - 21 303-42800-01 (Rev M ) — Sep 2023...
Page 114 6 Perform an Analysis 3. Select Calculate. 4. Save the sample file and run the analysis. TriStar II Plus Operator Manual 6 - 22 303-42800-01 (Rev M ) — Sep 2023...
Page 115: Perform An Empty Tube Analysis
Idle state at the bottom of the window. When analysis is complete, remove the sample tube and store (or dispose) of the sample material as applicable. TriStar II Plus Operator Manual 6 - 23 303-42800-01 (Rev M ) — Sep 2023...
Page 116: Perform A Reference Material Analysis
Gas Line on page 11 - 9. See. Ensure the helium is 99.999% pure. The measured free space is too high. This indicates the helium may not be pure enough. TriStar II Plus Operator Manual 6 - 24 303-42800-01 (Rev M ) — Sep 2023...
Page 117: About Reports
Reports > Start Report Starts the selected report. Select a file from the Files list. Ensure the selected file has a status of either Complete or Analyzing. TriStar II Plus Operator Manual 7 - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 118: Heat Of Adsorption Report
Add Samples [button] Removes all entries from the table. Clear Samples [button] Specifies the range of surface coverage to include in the report. Edit Quantities [button] TriStar II Plus Operator Manual 7 - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 119 Tabular report numeric values contributed by each sample. [check box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 7 - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 120: Spc Report
The selected items display as graph variable selections in Reports > Regression Report and graph selections in Reports > Control Chart. If report options for NLDFT Advanced PSD are required, click More. TriStar II Plus Operator Manual 7 - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 121: Regression Report
Select additional sample files to add to the report. Samples [button] Save as Default [button] Click to save selected report options as default report settings. TriStar II Plus Operator Manual 7 - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 122 Use these options to plot the regression of up to three y-axis variables against the x-axis variable. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 7 - 6 303-42800-01 (Rev M ) — Sep 2023...
Page 123: Control Chart Report
Autoscale. Allows the y-axis to be scaled automatically. To specify a range, deselect this option and enter a range in the From and To fields. TriStar II Plus Operator Manual 7 - 7 303-42800-01 (Rev M ) — Sep 2023...
Page 124 Select then enter a report title to appear on the report header. Show report title [check box] Generates a tabular report of the included samples that contains the Tabular report numeric values contributed by each sample. [check box] TriStar II Plus Operator Manual 7 - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 125 Days. Number of days elapsed from the first file placed on the list, which is the earliest-analyzed file. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 7 - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 126: Microactive Reports
Plots may be edited by selecting the data points or data point range to be included in the plots and modifying the parameters. When a report is edited, the results are immediately reflected in the plots and summary data. TriStar II Plus Operator Manual 7 - 10 303-42800-01 (Rev M ) — Sep 2023...
Page 127: Interactive Reports
Right-click to display a popup menu to include reports; enable or select overlays; edit curves, axes, legends, titles; and copy and paste the data in a graph or in tabular format. 5. Click Save. TriStar II Plus Operator Manual 7 - 11 303-42800-01 (Rev M ) — Sep 2023...
Page 128: Evaluate Report Results
The analysis data should be inspected for evidence of experimental error. The traditional method of confirming the quality of the experiment is to repeat the analysis. Toward that end, Micromeritics’ analyzers log and report the exact conditions of each analysis.
Page 129 A problem with either ambient or analysis free space values may indicate a free space measurement error and affect all calculations of quantity adsorbed. TriStar II Plus Operator Manual 7 - 13 303-42800-01 (Rev M ) — Sep 2023...
Page 130 Technology, Webb, P. and Orr, C., (1997). Most of the information in this article is extracted from Analytical Methods in Fine Particle Technology, Webb, P. and Orr, C., (1997). TriStar II Plus Operator Manual 7 - 14 303-42800-01 (Rev M ) — Sep 2023...
Page 131 McClellan, A.L., and Harnsberger, H.F., Journal of Colloid and Interface Science, 23, 577 (1967). Thomson, W., Phil. Mag. S., 42, 448 (1871). TriStar II Plus Operator Manual 7 - 15 303-42800-01 (Rev M ) — Sep 2023...
Page 132 Everett, D.H. and Powl, J.C., J. Chem Soc., Faraday Trans. 1, 72, 619 (1976). Dubinin, M. and Radushkevich, L.V., Proc. Acad. Sci. USSR, 55, 331 (1947). TriStar II Plus Operator Manual 7 - 16 303-42800-01 (Rev M ) — Sep 2023...
Page 133 Accumulated error results in the calculation of a too large volume of (possibly nonexistent) small pores if the thickness curve used underestimates film thinning. TriStar II Plus Operator Manual 7 - 17 303-42800-01 (Rev M ) — Sep 2023...
Page 134: Report Features And Shortcuts
Tabular and graphical reports contain sample and analyzer statistics such as analysis date/- time, analysis conditions, etc. The headers contain notes of sample file changes occurring after analysis. TriStar II Plus Operator Manual 7 - 18 303-42800-01 (Rev M ) — Sep 2023...
Page 135 Copies the report header as text. Text is copied to the clipboard and Copy header as text then can be pasted into other documents. Opens a dialog box for editing the report title. Edit TriStar II Plus Operator Manual 7 - 19 303-42800-01 (Rev M ) — Sep 2023...
Page 136 Displays the selected or hidden report in the Reports list box. Show [button] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 7 - 20 303-42800-01 (Rev M ) — Sep 2023...
Page 137 Right-click in the report data. Select Table header font on the shortcut Table header font menu. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 7 - 21 303-42800-01 (Rev M ) — Sep 2023...
Page 138 Title. Edits the selected axis label. Title font. Modifies the font for the selected axis label. Deselect Use default font. Select new font attributes for report data. Enable Use TriStar II Plus Operator Manual 7 - 22 303-42800-01 (Rev M ) — Sep 2023...
Page 139: Graph Features And Shortcuts
Title. Changes the title of the selected curve. Use default thickness. Uses the default curve thickness. Deselect to enter a new thickness number in the Thickness text box. TriStar II Plus Operator Manual 7 - 23 303-42800-01 (Rev M ) — Sep 2023...
Page 140 Displays a list of all curves. Select the curve(s) to display. Show curve For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 7 - 24 303-42800-01 (Rev M ) — Sep 2023...
Page 141 A box will display in the area to be enlarged. To return to normal view, right-click in the graph and select Autoscale all axes. TriStar II Plus Operator Manual 7 - 25 303-42800-01 (Rev M ) — Sep 2023...
Page 142 Deselect this option to remove the grid [selection] lines. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 7 - 26 303-42800-01 (Rev M ) — Sep 2023...
Page 143: Graph And Sample Overlays
DFT Pore Size / Surface Energy Dollimore-Heal Adsorption / Desorption Horvath-Kawazoe M-P Method This feature is available only when using Advanced option presentation. Go to Options > Option Presentation > Advanced. TriStar II Plus Operator Manual 7 - 27 303-42800-01 (Rev M ) — Sep 2023...
Page 144: Generate Pore Size Distribution Graph Overlays
Copy/paste. Data can be copied from one sample file (source) and pasted into another sample file (target). Pore size distribution report overlays menu selections are: Copy data Paste data Edit Imported Data Display Imported Data TriStar II Plus Operator Manual 7 - 28 303-42800-01 (Rev M ) — Sep 2023...
Page 145 3. Select a sample file to overlay graphs on to. 4. Click Open (or double-click the file name). 5. Right-click in the graph area and select Edit imported data. TriStar II Plus Operator Manual 7 - 29 303-42800-01 (Rev M ) — Sep 2023...
Page 146 5. Click OK to close the window. 6. Click Preview on the Report Options tab. 7. Click Print in the reports toolbar section to display print options. TriStar II Plus Operator Manual 7 - 30 303-42800-01 (Rev M ) — Sep 2023...
Page 147: Overlay Multiple Sample Files
4. In the Selected Reports list box, highlight a report then click Edit. Use the following table to complete the process for the selected report. TriStar II Plus Operator Manual 7 - 31 303-42800-01 (Rev M ) — Sep 2023...
Page 148 6. On the Plot Overlay Sample Selection window, move up to 25 files from the Available Files box to the Selected Files box: 7. Click OK. 8. To view the report, click Preview. TriStar II Plus Operator Manual 7 - 32 303-42800-01 (Rev M ) — Sep 2023...
Page 149 Selects the status of files to be combined. Status [drop-down box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 7 - 33 303-42800-01 (Rev M ) — Sep 2023...
Page 150: Import Ascii Pore Distribution Data
4. Right-click on the graph and select Paste Data on the shortcut menu. 5. To hide or show imported data, right-click in the graph area and use the Display imported data option on the shortcut menu. TriStar II Plus Operator Manual 7 - 34 303-42800-01 (Rev M ) — Sep 2023...
Page 151: Report Examples
Report Examples EPORT XAMPLES BET R EPORT TriStar II Plus Operator Manual 7 - 35 303-42800-01 (Rev M ) — Sep 2023...
Page 152: Bet Surface Area Plot
7 About Reports BET S URFACE TriStar II Plus Operator Manual 7 - 36 303-42800-01 (Rev M ) — Sep 2023...
Page 153: Bjh Adsorptive Cumulative Pore Volume
BJH Adsorptive Cumulative Pore Volume BJH A DSORPTIVE UMULATIVE OLUME TriStar II Plus Operator Manual 7 - 37 303-42800-01 (Rev M ) — Sep 2023...
Page 154: Bjh Desorption Cumulative Pore Volume
7 About Reports BJH D ESORPTION UMULATIVE OLUME TriStar II Plus Operator Manual 7 - 38 303-42800-01 (Rev M ) — Sep 2023...
Page 155: Isotherm Linear Plot
Isotherm Linear Plot SOTHERM INEAR TriStar II Plus Operator Manual 7 - 39 303-42800-01 (Rev M ) — Sep 2023...
Page 156: Isotherm Log Report
7 About Reports SOTHERM EPORT TriStar II Plus Operator Manual 7 - 40 303-42800-01 (Rev M ) — Sep 2023...
Page 157: T-Plot
TriStar II Plus Operator Manual 7 - 41 303-42800-01 (Rev M ) — Sep 2023...
Page 159: Selected Report Options
Calls for accessing the sample file data can be found in the Mic Module Python Calls section of this appendix. More advanced example python scripts are included in the analyzer software. TriStar II Plus Operator Manual 8 - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 160 9. On the Report Options tab, click Preview. The Python Reports will be included on the tabs across the top portion of the Reports window. TriStar II Plus Operator Manual 8 - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 161 Use to overlay samples as defined by the function. Overlay samples (if shown) [check box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 162: Alpha-S Method Report
It must have a two-column format with the relative pressures in the first column and the alpha-s values in the second column. Columns must be separated by a space or a tab. TriStar II Plus Operator Manual 8 - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 163 Tabular Report. Use to have a tabular report of data generated. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 164: Bet Surface Area Report
Use Interpolation option. Exclude All. Select to exclude all pressure points in the table. TriStar II Plus Operator Manual 8 - 6 303-42800-01 (Rev M ) — Sep 2023...
Page 165 Tabular report. Use to have a table of measured and calculated values generated. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 7 303-42800-01 (Rev M ) — Sep 2023...
Page 166: Bjh Adsorption/Desorption Report
Displays the Adsorptive Options window. The recommended adsorpt- Adsorptive [button] ives and their values are shown. Up to eight adsorptive and adsorbate property factor combinations may be specified. TriStar II Plus Operator Manual 8 - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 167 BJH pore volume. Enter the fraction of pores open at both ends to compensate for this error. TriStar II Plus Operator Manual 8 - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 168 One predefined curve is shipped with the analysis program and is found in the Reference directory. TriStar II Plus Operator Manual 8 - 10 303-42800-01 (Rev M ) — Sep 2023...
Page 169 Columns must be separated by a space or a tab. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 11 303-42800-01 (Rev M ) — Sep 2023...
Page 170 Overlay. Select an option to overlay onto the current report. Y-Axis [group box] Variable. Select a variable. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 12 303-42800-01 (Rev M ) — Sep 2023...
Page 171 Enabled only when Fixed pore size table is selected. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 13 303-42800-01 (Rev M ) — Sep 2023...
Page 172: Dft Pore Size Report
Lists the models that meet the specified criteria and match the Model [drop-down box] adsorbate and temperature of the sample data. If no models appear, no models meet the selected criteria. One model must be selected. TriStar II Plus Operator Manual 8 - 14 303-42800-01 (Rev M ) — Sep 2023...
Page 173 Edit. The Log Goodness of Fit and Goodness [group box] of Fit graphs cannot be edited. Autoscale Options. Use to autoscale the x-axis and/or y-axes. TriStar II Plus Operator Manual 8 - 15 303-42800-01 (Rev M ) — Sep 2023...
Page 174 DFT calculation used by earlier versions of the application is produced. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 16 303-42800-01 (Rev M ) — Sep 2023...
Page 175: Dft Surface Energy Report
The DFT Surface Energy report contains the results of surface energy distribution analyses. DFT Surface Energy Report Options fields and buttons are identical to the DFT Pore Size Report Options. TriStar II Plus Operator Manual 8 - 17 303-42800-01 (Rev M ) — Sep 2023...
Page 176: Dollimore-Heal Adsorption/Desorption Report
Displays the Adsorptive Options window. The recommended adsorpt- Adsorptive [button] ives and their values are shown. Up to eight adsorptive and adsorbate property factor combinations may be specified. TriStar II Plus Operator Manual 8 - 18 303-42800-01 (Rev M ) — Sep 2023...
Page 177 One predefined curve is shipped with the analysis program and is found in the Reference directory. TriStar II Plus Operator Manual 8 - 19 303-42800-01 (Rev M ) — Sep 2023...
Page 178 Columns must be separated by a space or a tab. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 20 303-42800-01 (Rev M ) — Sep 2023...
Page 179 Edit. The fields and buttons for these reports are identical to the BJH Plot Report Options. Dollimore-Heal Tabular Report Options Dollimore-Heal Tabular Report Options are identical to the BJH Tabular Report Options. TriStar II Plus Operator Manual 8 - 21 303-42800-01 (Rev M ) — Sep 2023...
Page 180: Dubinin Report
Enter the minimum and maximum limits for Radushkevich or Astak- Fitted Relative hov relative pressures included in the line fit. Pressure Range [group box] TriStar II Plus Operator Manual 8 - 22 303-42800-01 (Rev M ) — Sep 2023...
Page 181 Select the reports to generate. Highlight the report, then click Edit Select Reports modify report options. [group box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 23 303-42800-01 (Rev M ) — Sep 2023...
Page 182 Select to plot points on the graph. Plot curve / Plot points [selection] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 24 303-42800-01 (Rev M ) — Sep 2023...
Page 183 /p )^n. The value for [n] is the optimized exponent if Optimize exponent is selected on the Dubinin Report Options window. If not, then the value for [n] is the entered exponent value. TriStar II Plus Operator Manual 8 - 25...
Page 184 Use to overlay sample files on the plot. Overlay samples [check box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 26 303-42800-01 (Rev M ) — Sep 2023...
Page 185: F-Ratio Method Report
Browse to select a sample file to use as a reference for the isotherm. Reference isotherm Select a file containing an isotherm measured from a non-porous [group box] sample of the same material as the current sample. TriStar II Plus Operator Manual 8 - 27 303-42800-01 (Rev M ) — Sep 2023...
Page 186 Overlay samples. Use to overlay sample files on the f-plot. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 28 303-42800-01 (Rev M ) — Sep 2023...
Page 187: Freundlich Report
Exclude. Exclude All. Select to exclude all pressure points in the table. Include All. Select to include all pressure points in the table. TriStar II Plus Operator Manual 8 - 29 303-42800-01 (Rev M ) — Sep 2023...
Page 188 Use to have a report of the pressure points generated. Tabular report [selection] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 30 303-42800-01 (Rev M ) — Sep 2023...
Page 189: Horvath-Kawazoe Report
Select the option that best represents the physical geometry of the Pore Geometry micropores in the sample material. When Sphere is selected, options [group box] in the Interaction Parameter group box are disabled. TriStar II Plus Operator Manual 8 - 31 303-42800-01 (Rev M ) — Sep 2023...
Page 190 Density. Enter the density per unit area of the adsorptive. * Diameter. Enter the diameter of the gas phase atom. Diameter at zero energy. Enter the diameter of an atom at zero TriStar II Plus Operator Manual 8 - 32 303-42800-01 (Rev M ) — Sep 2023...
Page 191 [selection] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 33 303-42800-01 (Rev M ) — Sep 2023...
Page 192 Options window, then click Edit. Select the data types to include in the report. Column [n] indicates the column order and data contents for the report. TriStar II Plus Operator Manual 8 - 34 303-42800-01 (Rev M ) — Sep 2023...
Page 193: Isotherm Report
) STP or mmol/g per other Surface Area (cm ) STP or mmol/m Select each option to include on the final report. Click the Options Selected Reports TriStar II Plus Operator Manual 8 - 35 303-42800-01 (Rev M ) — Sep 2023...
Page 194 Weight %. Enter the mass percentage when plotting pressure composition. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 36 303-42800-01 (Rev M ) — Sep 2023...
Page 195: Langmuir Report
Calculation pressure range. Enter the minimum and maximum pressures to be used in the pressure table. To exclude a point from the calculations used to generate the report, select Exclude. TriStar II Plus Operator Manual 8 - 37 303-42800-01 (Rev M ) — Sep 2023...
Page 196 Overlay samples. Use to overlay sample files on the Langmuir transform plot. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 38 303-42800-01 (Rev M ) — Sep 2023...
Page 197: Mp-Method Report
Exclude. Exclude All. Select to exclude all pressure points in the table. Include All. Select to include all pressure points in the table. TriStar II Plus Operator Manual 8 - 39 303-42800-01 (Rev M ) — Sep 2023...
Page 198 Thickness Curve equation for the selected curve. [group box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 40 303-42800-01 (Rev M ) — Sep 2023...
Page 199 Overlay. Select an option to overlay on the current report. Variable. Select a variable. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 41 303-42800-01 (Rev M ) — Sep 2023...
Page 200 The MP Method reports hydraulic radius only. If Pore size in diameter is selected on the Unit Selection window, pore size in radius will be reported. TriStar II Plus Operator Manual 8 - 42 303-42800-01 (Rev M ) — Sep 2023...
Page 201: Nldft Advanced Psd Report
More accurate means getting the pore distribution at smaller pore sizes (a few Angstroms) as well as larger pore sizes (one thousand Angstroms). TriStar II Plus Operator Manual 8 - 43 303-42800-01 (Rev M ) — Sep 2023...
Page 202 Use to select the second sample file. Select Reports [group box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 44 303-42800-01 (Rev M ) — Sep 2023...
Page 203 Data are automatically calculated for both sample files. c. Click Edit to make any necessary modifications to the second sample file. TriStar II Plus Operator Manual 8 - 45 303-42800-01 (Rev M ) — Sep 2023...
Page 204 8 Selected Report Options TriStar II Plus Operator Manual 8 - 46 303-42800-01 (Rev M ) — Sep 2023...
Page 205: Options Report
Lists the conditions used to perform the analysis such as: Adsorptive properties Analysis conditions Analysis method Degas conditions Free space Saturation pressure (P ) and temperature Options reports cannot be edited. TriStar II Plus Operator Manual 8 - 47 303-42800-01 (Rev M ) — Sep 2023...
Page 206: Sample Audit Trail Report
UDIT RAIL EPORT For 21CFR11 environments only. This report lists all changes and comments that have been applied to sample files with a Complete status. TriStar II Plus Operator Manual 8 - 48 303-42800-01 (Rev M ) — Sep 2023...
Page 207: Summary Report
Pass/Fail [n]. Click to display the Pass/Fail Options window for selection of pass/fail criteria. S A: Single-point BET. Use to enable Pass/Fail [n] in the Item [n] group box. TriStar II Plus Operator Manual 8 - 49 303-42800-01 (Rev M ) — Sep 2023...
Page 208 Selects (or deselects) all options. Select All / Deselect All [button] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 50 303-42800-01 (Rev M ) — Sep 2023...
Page 209: T-Plot Report
Exclude. Exclude All. Select to exclude all pressure points in the table. Include All. Select to include all pressure points in the table. TriStar II Plus Operator Manual 8 - 51 303-42800-01 (Rev M ) — Sep 2023...
Page 210 One predefined curve is shipped with the analysis program and is found in the Reference directory. TriStar II Plus Operator Manual 8 - 52 303-42800-01 (Rev M ) — Sep 2023...
Page 211 Overlay samples. Use to overlay sample files on the t-plot. For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 53 303-42800-01 (Rev M ) — Sep 2023...
Page 212: Temkin Report
Exclude. Exclude All. Select to exclude all pressure points in the table. Include All. Select to include all pressure points in the table. TriStar II Plus Operator Manual 8 - 54 303-42800-01 (Rev M ) — Sep 2023...
Page 213 Select and enter the monolayer capacity of the sample. Specify monolayer capacity [check box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 8 - 55 303-42800-01 (Rev M ) — Sep 2023...
Page 214: Validation Report
If the data for any reports selected for validation are determined to be out of range, a warning will display and suggestions are given for corrective action. TriStar II Plus Operator Manual 8 - 56 303-42800-01 (Rev M ) — Sep 2023...
Page 215: Diagnostics
Use to display diagnostic readings, start diagnostic tests, and open saved diagnostic reports. Each test generates a file to the default directory name and path of ...\...\Service\userdiag unless another directory name was specified. These reports can be sent to a Micromeritics Service Representative for examination.
Page 216 Select the diagnostic test to be performed. Test [drop-down box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual 9 - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 217: Calibration
Disabled calibration menu options can be accessed only with the assistance of an authorized Micromeritics Service Representative. Calibrations can be saved to a file and reloaded later. To review calibration details of the analyzer, go to Unit [n] > Unit Configuration.
Page 218: Match Transducers
1. Ensure that all applicable transducers are selected. 2. Click Start. The window closes when the operation is complete. 3. Click when the process is complete. TriStar II Plus Operator Manual 10 - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 219: Pressure Offset
The current pressure readings and operation status messages display. When the calibration is complete, a confirmation message is displayed with the event log message for the pressure transducer offset calibration. Click OK. TriStar II Plus Operator Manual 10 - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 220: Servo Valve
Ensure the pressure transducer has been calibrated before performing this pro- cedure. Go to Unit [n] > Unit Configuration and view the calibration information. Contact your Micromeritics Service Representative if calibration dates are not listed. Click Start. The window closes when the calibration is complete.
Page 221: Load Calibration From File
[SN]last.cal. The backup file is overwritten each time a new one is created. Changing the calibration may affect the analyzer’s performance. TriStar II Plus Operator Manual 10 - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 223: Troubleshooting
When unexpected results occur, some common operational problems not indicated on the window and their respective causes and solutions are provided. The following can be found on the Micromeritics web page (www.micromeritics.com). Error Messages document (PDF) Parts and Accessories Smart VacPrep Operator Manual (PDF)
Page 224 Action D: Install plug or empty sample tube. Cause E: Gas inlet valve open while vacuum valve open. Action E: With manual control enabled, use the instrument schematic to close gas inlet valve. TriStar II Plus Operator Manual 11 - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 225: Power
Power OWER The TriStar II Plus is designed to operate with universal input power supply (100-240 VAC, 50/60 Hz, 150 VA). Noise-free power of the correct voltage and frequency, with a safety earth ground, should be available through a standard wall receptacle. The power outlet should be able to supply 15 amps @ 100 or 115 VAC ±10% or 7.5 amps @ 230 VAC ±10%.
Page 226: Guidelines For Connecting Gases
This will help avoid confusion when maintenance is required. Label the gas line at the analyzer inlet for proper identification and maintenance. TriStar II Plus Operator Manual 11 - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 227: Replace A Gas Cylinder
C. Low pressure gauge D. High pressure gauge E. Gas cylinder shut-off valve F. Regulator connecter nut G. Regulator control knob H. Brass reducer fitting TriStar II Plus Operator Manual 11 - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 228 7. Replace the protective cap on the depleted cylinder. Disconnect the retaining strap and move the cylinder to an appropriate location. TriStar II Plus Operator Manual 11 - 6 303-42800-01 (Rev M ) — Sep 2023...
Page 229 See the Regulator Pressure Settings table in Connect a Gas Cylinder. b. Open the regulator Shut-off valve. c. Open the gas cylinder Shut-off valve and flow gas for 10 to 30 seconds. TriStar II Plus Operator Manual 11 - 7 303-42800-01 (Rev M ) — Sep 2023...
Page 230 Close the gas cylinder Shut-off valve. e. Close the gas cylinder valve. 7. If the gas line to the instrument inlet was previously disconnected, reconnect it now. TriStar II Plus Operator Manual 11 - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 231: Clean And Verify The Gas Line
3. Select the Report after test option then select Preview. Click Start. 4. From the View drop-down list, select either Operation, Instrument Log, or Instrument TriStar II Plus Operator Manual 11 - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 232 User will be needed in 30 minutes to close the isolation valve. Click to begin auto- mated testing. 6. Click when the test is complete. The test reports display. TriStar II Plus Operator Manual 11 - 10 303-42800-01 (Rev M ) — Sep 2023...
Page 233: Enable Manual Control
When this option is enabled, a checkmark appears to the left of Unit [n] > Enable Manual Control. If the analyzer schematic is not immediately visible, go to Unit [n] > Show Instrument Schematic. TriStar II Plus Operator Manual 11 - 11 303-42800-01 (Rev M ) — Sep 2023...
Page 234: Perform A Leak Test
Unit [n] > Diagnostics > Start Diagnostic Test A Micromeritics Service Representative may request that a leak test be performed to determine if there is a system leak and may also require a copy of the report generated by this test.
Page 235 Perform a Leak Test A. Suspend/Resume/ Skip/Play buttons B. Port report buttons C. Live graph settings TriStar II Plus Operator Manual 11 - 13 303-42800-01 (Rev M ) — Sep 2023...
Page 236: Preventive Maintenance
** For oil-free pumps only: After 12 to 18 months of operation, the diaphragm(s) 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(s) be replaced by a Micromeritics Service Representative every 12 months.
Page 237: Check And Clean The Dewar
Do not pour liquid nitrogen directly into a sink. Doing so may cause drain pipes to burst. 3. Rinse the Dewar with warm water to melt any remaining ice accumulation which may remain. Dry thoroughly. 4. Replace the Dewar. TriStar II Plus Operator Manual 11 - 15 303-42800-01 (Rev M ) — Sep 2023...
Page 238: Clean The Instrument
SSEMBLY 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 Representative for disposition. Should lubrication become necessary, apply a light coat of Teflon Magnalube-G grease [Micromeritics part number 004-16163-00] to the elevator screw.
Page 239: Power Instrument On And Off
No. The program remains open and the analysis continues to run. 2. Computer, monitor, and printer. 3. Analyzer. 4. External vacuum pump. TriStar II Plus Operator Manual 11 - 17 303-42800-01 (Rev M ) — Sep 2023...
Page 240: Sample Port Frit Replacement
5. Replace the filter and O-ring. Carefully reassemble the sample tube fitting and reinstall on the sample port. Tighten by hand, then with a wrench to prevent leaks. TriStar II Plus Operator Manual 11 - 18 303-42800-01 (Rev M ) — Sep 2023...
Page 241: Sample Tube O-Ring Replacement
A. O-ring B. Ferrule C. Connector nut 4. Remove the O-ring from the top of the sample tube and replace it with a new one. TriStar II Plus Operator Manual 11 - 19 303-42800-01 (Rev M ) — Sep 2023...
Page 242: Recover From A Power Failure
Any data collected during the analysis will still be present, but the analysis should be restarted in order to produce complete results. TriStar II Plus Operator Manual 11 - 20 303-42800-01 (Rev M ) — Sep 2023...
Page 243: Service Test Mode
Options > Service Test Mode Service Test Mode is a password protected option used to perform certain service tests with the assistance of a trained Micromeritics Service Representative. This password is supplied by your Micromeritics Service Representative. If a menu item is grayed out, it is usually an indication that Service Test Mode is required.
Page 245 Calls for accessing the sample file data can be found in the Mic Module Python Calls section of this appendix. More advanced example python scripts are included in the analyzer software. TriStar II Plus Operator Manual A - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 246: Advanced Reports A
9. On the Report Options tab, click Preview. The Python Reports will be included on the tabs across the top portion of the Reports window. TriStar II Plus Operator Manual A - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 247 Use to overlay samples as defined by the function. Overlay samples (if shown) [check box] For fields and buttons not listed in this table, see Common Fields and Buttons on page 2 - TriStar II Plus Operator Manual A - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 248: Scripts A
Exclude All. Select to exclude all pressure points in the table. Include All. Select to include all pressure points in the table. OK. Saves and closes the active window. TriStar II Plus Operator Manual A - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 249 Removes the script from the Available Scripts box but does not affect Remove [button] original .py text file. Replaces the contents of the selected script however, the script Replace [button] name remains the same. TriStar II Plus Operator Manual A - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 250: Python Reports A
Graph', 'X', 'F(X)' myx = np.array( [0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, mic.graph.add( 'X2', myx, myx*myx, marker='o' mic.graph.add( 'sin(X)', myx, np.sin(myx), marker='^' The results are: TriStar II Plus Operator Manual A - 6 303-42800-01 (Rev M ) — Sep 2023...
Page 251 ["Label 1:", "Label 2:", "Label 3:"], ["val1", "val2", "val3"] ) mic.summary.add( "Summary B", ["Label 4:", "Label 5:", "Label 6:"], ["val4", "val5", "val6"] ) The result is: TriStar II Plus Operator Manual A - 7 303-42800-01 (Rev M ) — Sep 2023...
Page 252 = x2 = x3 = 3.14159/2 mic.table.addtable( "My Set B" mic.table.addcolumn( "X", ['{:8.3f}'.format(x1), '{:8.3f}'.format(x2), '{:8.3f}'.format(x3)] ) mic.table.addcolumn( "sin(X)", ['{:8.3f}'.format(np.sin(x1)), '{:8.3f}'.format(np.sin(x2)), '{:8.3f}'.format(np.sin(x3))] ) mic.table.addcolumn( "cos(X)", ['{:8.3f}'.format(np.cos(x1)), '{:8.3f}'.format(np.cos(x2)), '{:8.3f}'.format(np.cos(x3))] ) TriStar II Plus Operator Manual A - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 253 Python Reports The result is: TriStar II Plus Operator Manual A - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 254: Acquire Basic Information A
= mic.sample_information('sample density') mic.summary( "Sample Information" mic.summary.add( "Sample Information", [ "Number of adsorption points:", "Warm free space:", "Cold free space:", "Sample mass:", "Description:", "Analysis temperature:", "Sample density:" TriStar II Plus Operator Manual A - 10 303-42800-01 (Rev M ) — Sep 2023...
Page 255 '{:8.3f}'.format(mol_weight), analysis_gas ] ) Note the calls to mic.isotherm and mic.adsorptive_data above are each returning results as a list with elements of varying return type. TriStar II Plus Operator Manual A - 11 303-42800-01 (Rev M ) — Sep 2023...
Page 256: Acquire Report Results A
"T-plot external surface area:", "T-plot micropore volume:" [ '{:10.5f}'.format(sa) + m²/g', '{:10.5f}'.format(c), '{:10.5f}'.format(vm) + cm³/g', '{:10.5f}'.format(esa) + m²/g', '{:10.5f}'.format(vol) + ' cm³/g' The result is: TriStar II Plus Operator Manual A - 12 303-42800-01 (Rev M ) — Sep 2023...
Page 257 (np.isnan(xdat[0]) np.isnan(ydat[0])): # NaN indicates BJH calculation error. mic.graph( 'BJH Adsorption/Desorption', 'Pore Diameter (Å)', 'Incremental Volume (cm³/g)' mic.graph.add( desc, xdat, ydat ) The result is: TriStar II Plus Operator Manual A - 13 303-42800-01 (Rev M ) — Sep 2023...
Page 258: Acquire Overlay Sample Data A
1', p1, q1 ) mic.graph.add( 'Overlay Isotherm 2', p2, q2 ) mic.summary( "A Summary Report" mic.summary.add( "Two samples", [ "Primary sample:", "Overlay sample 1:", "Overlay sample 2:" [ desc, desc1, desc2 ] ) TriStar II Plus Operator Manual A - 14 303-42800-01 (Rev M ) — Sep 2023...
Page 259 Sample files to overlay must be selected, and The Overlay samples checkbox on the Advanced Report Options window must be selected. TriStar II Plus Operator Manual A - 15 303-42800-01 (Rev M ) — Sep 2023...
Page 260: Enable The Use Of Overlay Data A
6. Select the Overlay samples checkbox to the right of the selected report. 7. Click OK. 8. Run the script using the instructions found in Scripts on page A - TriStar II Plus Operator Manual A - 16 303-42800-01 (Rev M ) — Sep 2023...
Page 261 header --- column header; must be a string convertible) values --- column values; must be a list of strings con- vertible) align --- column alignment; 'r', 'l', right, left, center justified TriStar II Plus Operator Manual A - 17 303-42800-01 (Rev M ) — Sep 2023...
Page 262 A Advanced Reports - Python Module Create a New Tabular Report mic.table( title='User Table' Keyword arguments: title --- the tabular report title (default = 'User Table') TriStar II Plus Operator Manual A - 18 303-42800-01 (Rev M ) — Sep 2023...
Page 263 values --- column of values; must be a list of strings convertible) the same length labels Create a New Summary Report mic.summary( title='User Summary' Keyword arguments: title --- the summary title TriStar II Plus Operator Manual A - 19 303-42800-01 (Rev M ) — Sep 2023...
Page 264 '-.' : dash dot '-..' : dash dot dot marker --- marker shape; (default = 'a') '+' : plus : circle 'x' : cross '^' : up triangle 'v' : down triangle TriStar II Plus Operator Manual A - 20 303-42800-01 (Rev M ) — Sep 2023...
Page 265 Add a curve to the last created graphical report using the second y-axis. The arguments to this call are the same to mic.- graph.add. TriStar II Plus Operator Manual A - 21 303-42800-01 (Rev M ) — Sep 2023...
Page 266 yyrange --- None, two values giving the min range of the axis. xbars_id --- None, the id of an xbar control created via the mic.control() object TriStar II Plus Operator Manual A - 22 303-42800-01 (Rev M ) — Sep 2023...
Page 267 p, qads, n_ads, warm_fs, cold_fs, mass, desc = mic.isotherm ('rel') p --- array of pressure (relative absolute) qads --- array of cumulative quantity adsorbed TriStar II Plus Operator Manual A - 23 303-42800-01 (Rev M ) — Sep 2023...
Page 268 A Advanced Reports - Python Module num_ads --- number of points the adsorption curve warm_fs --- warm free-space cold_fs --- cold free-space mass --- sample mass desc --- sample description TriStar II Plus Operator Manual A - 24 303-42800-01 (Rev M ) — Sep 2023...
Page 269 (ambient) free-space; overlay unavail- able cold_fs --- cold (analysis) free-space; overlay unavail- able mass --- sample mass; overlay unavailable desc --- sample description; empty-string overlay unavailable TriStar II Plus Operator Manual A - 25 303-42800-01 (Rev M ) — Sep 2023...
Page 270 (nm^2) hsd --- hard sphere diameter (angstroms) dcf --- density conversion factor (dimensionless) mol_weight --- molecular weight analysis_gas --- mnemonic the analysis gas species (e.g., 'CO', 'H2') TriStar II Plus Operator Manual A - 26 303-42800-01 (Rev M ) — Sep 2023...
Page 271 sample_number --- Sample to retrieve 0 : current sample file (default) through : corresponding overlay sample file Usage: all_keywords = sample_information() mass = sample_information('sample mass') mass = sample_information('sample mass',0) TriStar II Plus Operator Manual A - 27 303-42800-01 (Rev M ) — Sep 2023...
Page 272 Report Result Description ----------- -------------- ----------- bet surface area Surface area (m^2/g) bet bet constant BET constant (dimen- sionless) bet monolayer capacity Monolayer capacity (cm^3/g) tplot external surface area External surface area (m^2/g) tplot micropore volume Micropore volume (cm^3/g) TriStar II Plus Operator Manual A - 28 303-42800-01 (Rev M ) — Sep 2023...
Page 273 porew --- array of pore dimension boundaries (angstroms); empty-array unavailable. incvol --- array of incremental pore volumes (cm^3/g); empty-array unavailable. desc --- Name of data set; empty-string unavailable. TriStar II Plus Operator Manual A - 29 303-42800-01 (Rev M ) — Sep 2023...
Page 274 porew --- array of pore dimension boundaries (angstroms); empty-array unavailable. incvol --- array of incremental pore volumes (cm^3/g); empty-array unavailable. desc --- Name of data set; empty-string unavailable. TriStar II Plus Operator Manual A - 30 303-42800-01 (Rev M ) — Sep 2023...
Page 275: B Dft Models
A graph that plots amount adsorbed versus equilibrium pressure is called an adsorption isotherm. TriStar II Plus Operator Manual B - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 276 10-14 seconds. Although the mathematics are simple, the number of calculations required for a system of even a few hundred particles is astronomical and challenges even the fastest computers. TriStar II Plus Operator Manual B - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 277 It can also be defined as the partial derivative of the grand potential energy with respect to density (or concentration). TriStar II Plus Operator Manual B - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 278 The area under the profile curve represents the amount adsorbed per unit area at this pressure. The positions of the maxima are separated by a distance determined by the size of the adsorptive atom. TriStar II Plus Operator Manual B - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 279 Inset d shows the profile converging on a density similar to that of bulk liquid argon in the center of the pore, indicating a phase transition. TriStar II Plus Operator Manual B - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 280 Figure 4 shows model isotherms for pores in the micropore size range. Note the logarithmic scale for pressure. Figure Model Isotherms in the Micropore Size Range of Pore Width Argon on Carbon at 87.3 K TriStar II Plus Operator Manual B - 6 303-42800-01 (Rev M ) — Sep 2023...
Page 281 Non-Local Density Functional Theory with Density-Dependent Weights N2 - Modified Density Functional Geometry: Free surface Substrate: Surface energy Method: Nitrogen at 77K TriStar II Plus Operator Manual B - 7 303-42800-01 (Rev M ) — Sep 2023...
Page 282 This model reports pore widths from 3.8 to 387 angstroms. TriStar II Plus Operator Manual B - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 283 This model was produced in the same manner as the N2 Modified Density Functional model listed earlier, except applicable to argon adsorbed at 87.3 K. TriStar II Plus Operator Manual B - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 284 N2 - Carbon Finite Pores, As=6, 2D-NLDFT Ar - Carbon Finite Pores, As=6, 2D-NLDFT Geometry: Finite Slit Substrate: Carbon Category: Porosity Method: Nitrogen at 77K; Argon at 87K TriStar II Plus Operator Manual B - 10 303-42800-01 (Rev M ) — Sep 2023...
Page 285 N2 - Carbon Cylinder, single-wall nanotube by NLDFT Ar - Argon Cylinder, single-wall nanotube by NLDFT Geometry: Cylinder Substrate: Carbon Category: Porosity Method: Nitrogen at 77 K; Argon at 87 K TriStar II Plus Operator Manual B - 11 303-42800-01 (Rev M ) — Sep 2023...
Page 286 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. TriStar II Plus Operator Manual B - 12 303-42800-01 (Rev M ) — Sep 2023...
Page 287: Models Based On Classical Theories B
(1) of the DFT Theory. The Calculations document can be found on the Micromeritics web page (www.micromeritics.com). Be aware that the deconvolution method only provides a fitting mechanism; it does not overcome any inherent shortcomings in the underlying theory.
Page 288 Method: Nitrogen 77 K The kernel function is calculated using the Halsey equation with standard parameters: The nitrogen properties used in the Kelvin equation are: TriStar II Plus Operator Manual B - 14 303-42800-01 (Rev M ) — Sep 2023...
Page 289 The calculation is the same as above except that cylindrical geometry is assumed. References: W. D. Harkins and G. Jura, J.A.C.S. 66, 1366 (1944). J. H. DeBoer et al., J. Colloid and Interface Sci. 21, 405 (1966). TriStar II Plus Operator Manual B - 15 303-42800-01 (Rev M ) — Sep 2023...
Page 290: Dft Model References B
Instrument Corp; presented at the International Symposium on the Effects of Sur- face Heterogeneity in Adsorption and Catalysts on Solids, Kazimierz Dolny, Poland (July 1992). TriStar II Plus Operator Manual B - 16 303-42800-01 (Rev M ) — Sep 2023...
Page 291 4. “The Determination of Surface Energetic Heterogeneity Using Model Isotherms Calculated by Density Functional Theory,” J.P. Olivier; presented at the Fifth International Conference on the Fundamentals of Adsorption, Pacific Grove, CA (1995). TriStar II Plus Operator Manual B - 17 303-42800-01 (Rev M ) — Sep 2023...
Page 293: C Free-Space Correction
Then the manifold is charged with helium, the pressure measured, and the valve opened allowing the helium to expand into the sample tube at ambient temperature. Again the pressure is measured. TriStar II Plus Operator Manual C - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 294 TriStar II Plus Operator Manual C - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 295 Micromeritics offers the following suggestions to assist in maintaining high-purity gases (particularly helium): Use metal gas lines only.
Page 296 6. Loosen the fitting at the instrument helium inlet until the low pressure side drops to approx- imately 3 psig (0.02 MPa), then tighten the fitting. TriStar II Plus Operator Manual D - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 297 8. Briefly open the gas cylinder valve, then use the Pressure Control knob to reset the reg- ulator output pressure to 15 psig. 9. After the pressure has stabilized (indicating there are no leaks), open the gas cylinder valve. TriStar II Plus Operator Manual D - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 298 Allow evacuation for a full 20 minutes. If evacuation time is too short, trapped air may remain in the lines. 5. Close valves 6, 7, and 10. TriStar II Plus Operator Manual D - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 299 Mass of sample tube set plus sample Mass of sample (step 2 minus step 1) Degas Information Degas apparatus Temperature (°C) Time (hours) Actual time started Actual time finished Degas Notes: TriStar II Plus Operator Manual E - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 300 Density: 1.000 g/cm³ Type of data: Automatically collected Instrument type: 3030 Original instrument type: 3030 Comments: Sample Tube Sample tube: Sample Tube Ambient free space: 1.0000 cm³ Analysis free space: 1.0000 cm³ TriStar II Plus Operator Manual F - 1 303-42800-01 (Rev M ) — Sep 2023...
Page 301 Evacuation rate: 0.67 kPa/s Unrest. evacuation from: 0.67 kPa Vacuum level: 1.333224e-03 kPa Evacuation time: 10 min Temperature ramp rate: 10.0 °C/min Target temperature: 30 °C Hold pressure: 13.3 kPa Heating Phase Sample Ramp TriStar II Plus Operator Manual F - 2 303-42800-01 (Rev M ) — Sep 2023...
Page 302 prep: Temperature Rate Time Stage (°C) (°C/min) (min) ---- 1 400 10 60 Analysis Conditions Analysis conditions: Run Conditions Isotherm collection: Target Pressure Pressure Table Starting Pressure Ending Pressure Increment Pressure (p/p°) (p/p°) (p/p°) 0.000000000 0.060000000 0.060000000 0.020000000 0.200000000 Preparation Fast evacuation: No Evacuation rate: 1.33 kPa/s TriStar II Plus Operator Manual F - 3 303-42800-01 (Rev M ) — Sep 2023...
Page 303 Evacuation time: 0.10 h Outgas test: Yes Outgas test duration: 180 s p° and Temperature p° type: Calculated from analysis temperature Temperature type: Entered Temperature: 77.300 K Dosing Use first pressure fixed dose: No TriStar II Plus Operator Manual F - 4 303-42800-01 (Rev M ) — Sep 2023...
Page 304 Minimum equilibration delay at p/p° >= 0.995: 1 s Sample Backfill Backfill at start of analysis: Yes Backfill at end of analysis: Yes Backfill gas: N2 Adsorptive Properties Adsorptive: krypton @ 77.35 K (Kr) Non-condensing adsorptive: No TriStar II Plus Operator Manual F - 5 303-42800-01 (Rev M ) — Sep 2023...
Page 305 Thermal conductivity: 1.00 Non-ideality factor: 0.0000300 Density conversion factor: 0.0012743 Dosing method: From Psat tube Psat vs. Temperature Table Saturation Pressure Temperature (kPa) (K) 1 0.2104 75.40 2 0.2341 75.85 3 0.2632 76.35 4 0.2988 76.90 5 0.3162 77.15 6 0.3309 77.35 7 0.3461 77.55 8 0.3701 77.85 TriStar II Plus Operator Manual F - 6 303-42800-01 (Rev M ) — Sep 2023...
Page 306 Graphic file: miclogo.emf Graphic height: 0.250 in Graphic width: 2.000 in Apply thermal transpiration correction: No Summary: Yes Surface Area Single-point BET: Yes Multi-point BET: Yes Langmuir: No t-Plot Micropore: No t-Plot External: No TriStar II Plus Operator Manual F - 7 303-42800-01 (Rev M ) — Sep 2023...
Page 307 BJH Cum. Desorption: No D-H Cum. Adsorption: No D-H Cum. Desorption: No Pore Size Average pore diameter: No BJH adsorption avg.: No BJH desorption avg.: No D-H adsorption avg.: No D-H desorption avg.: No TriStar II Plus Operator Manual F - 8 303-42800-01 (Rev M ) — Sep 2023...
Page 308 DFT Surface Energy: No Nanoparticle Size: No Horvath-Kawazoe Maximum pore volume: No Median pore width: No Dubinin-Radushkevich Micropore surface area: No Monolayer capacity: No Dubinin-Astakhov Micropore surface area: No Limiting micropore volume: No TriStar II Plus Operator Manual F - 9 303-42800-01 (Rev M ) — Sep 2023...
Page 309 High Range Value: 0.3000 m²/g High Range Message: Alumina 004/16816/00 Lot 152624-13 Upper Limit Low Range Value: 0.2200 m²/g Low Range Message: Alumina 004/16816/00 Lot 152624-13 Lower Limit Pass/Fail 3: No Pass/Fail 4: No TriStar II Plus Operator Manual F - 10 303-42800-01 (Rev M ) — Sep 2023...

Micromeritics TRISTAR II PLUS Operator's Manual

About this Manual

General Safety

1 Analyzer Components for Tristar II Plus

2 About the Software

3 Sample Files

4 Parameter Files

5 Degassing

6 Perform an Analysis

7 About Reports

8 Selected Report Options

9 Diagnostics

10 Calibration

11 Troubleshooting

B DFT Models

C Free-Space Correction

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