Micromeritics GEMINI VII Operator's Manual
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Micromeritics GEMINI VII Operator's Manual

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G
VII
EMINI
S
A
A
URFACE
REA
NALYZER
O
M
PERATOR
ANUAL
239-42828-01
May 2021
(Rev H )

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Summary of Contents for Micromeritics GEMINI VII

  • Page 1 ® EMINI URFACE NALYZER PERATOR ANUAL 239-42828-01 May 2021 (Rev H )
  • 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 - 2021. 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: Corporate Profile

    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, prestigious government, and academic institutions. Our world-class scientists and responsive support teams enable customer success by applying Micromeritics technology to the most demanding applications.

  • Page 5: Contact Us

    Norcross, GA / USA / 30093-2901 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 Learning Center Phone: 1-770-662-3607 www.Micro.edu Gemini VII Operator Manual 239-42828-01 (Rev H ) — May 2021...

  • Page 6: About This Manual

    Parts and Accessories Vacuum Pump Guide (PDF) All references to Gemini VII in this document encompass the Gemini VII models 2390a, 2390p, and 2390t unless otherwise noted. It also encompasses all references to the Gemini VII and Gemini VII Confirm environments unless otherwise noted.

  • Page 7: General Safety

    The Gemini VII sound level is below 80 dBA. Hearing protection is optional. The Gemini VII has a safety shield. Ensure it is in place when operating the instru- ment.
  • Page 8 General Safety NTENDED The Gemini VII series analyzers provide single and multipoint surface area and pore size measurements. Three models are available — the Gemini 2390a, 2390p, and 2390t. The Gemini 2390a and 2390p are enclosed in the same size cabinet. The only physical difference...
  • Page 9 EFUP (for example, battery modules) and so 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. Gemini VII Operator Manual 239-42828-01 (Rev H ) — May 2021...

  • Page 11: Table Of Contents

    Equipment Options and Upgrades 1 - 3 Gas Requirements and Purity 1 - 5 Cryogen Requirements 1 - 5 Specifications for the Gemini VII 1 - 6 2 About the Software 2 - 1 Menu Structure 2 - 1 Common Fields and Buttons...
  • Page 12 Perform an Empty Tube Analysis 5 - 14 Perform a Reference Material Analysis 5 - 16 Perform a QuickStart Analysis 5 - 18 Measure Saturation Pressure 5 - 19 Gemini VII Operator Manual 239-42828-01 (Rev H ) — May 2021...
  • Page 13 7 - 14 Dollimore-Heal Adsorption/Desorption Report 7 - 15 Dubinin Report 7 - 20 f-Ratio Method Report 7 - 25 Freundlich Report 7 - 27 Horvath-Kawazoe Report 7 - 29 Gemini VII Operator Manual 239-42828-01 (Rev H ) — May 2021...
  • Page 14 Enable Manual Control 10 - 14 Perform a Leak Test 10 - 15 Perform Reference Material Analysis 10 - 17 Perform an Empty Tube Analysis for Diagnostic Purposes 10 - 17 Gemini VII Operator Manual 239-42828-01 (Rev H ) — May 2021...
  • Page 15 D O-ring Compatibility D - 1 E Worksheets E - 1 Sample Data Worksheet for Gas Adsorption E - 2 Gemini VII 2390 EU Declaration of Conformity DoC - 1 Index Index - 1 Gemini VII Operator Manual xiii 239-42828-01 (Rev H ) — May 2021...

  • Page 17: Analyzer Components

    1 Analyzer Components NALYZER OMPONENTS Parts and accessories can be found online at www.Micromeritics.com. RONT OMPONENTS A. Dewar B. Sample safety shield C. Power indicator light D. Balance port and balance tube E. P port and tube F. Sample port and sample tube G.
  • Page 18 F. Keypad connection - used only wit keypad con- figurations G. Helium inlet port for helium gas supply H. Adsorptive gas inlet I. Vacuum pump connector Gemini VII Operator Manual 1 - 2 239-42828-01 (Rev H ) — May 2021...

  • Page 19: Equipment Options And Upgrades

    Dewar and the recirculating liquids. The Chiller Dewar Quick Start Guide [part number 025-42801-00] can be found on the Micromeritics web page (www.Micromeritics.com). The analyzer requires a vacuum pump for sample analysis. Vacuum...
  • Page 20 Needle valves are also provided for introducing the vacuum slowly to prevent fluidization of samples. The VacPrep is an independent unit and not controlled by the analyzer. Gemini VII Operator Manual 1 - 4 239-42828-01 (Rev H ) — May 2021...

  • Page 21: Gas Requirements And Purity

    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 can be found online at www.Micromeritics.com.
  • Page 22 1,000 mmHg pressure trans- ducer. Typically, oxygen, argon, carbon dioxide, butane, methane, and other light hydrocarbons will produce useful data above abso- lute pressures of a few mmHg. Gemini VII Operator Manual 1 - 6 239-42828-01 (Rev H ) — May 2021...

  • Page 23: Specifications For The Gemini Vii

    Sample capacity is approx- imately 2.0 cm Standard Tube Gemini VII 2390t. 0.95 cm (3/8 in.) OD × 20.5 cm (8.1 in.) long with 8.9 cm of volume. Sample capacity is approximately 2.0 Gemini VII 2390a and 2390p. 8 hours Dewar Gemini VII 2390t.
  • Page 24 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. Gemini VII Operator Manual 1 - 8 239-42828-01 (Rev H ) — May 2021...

  • Page 25: About The Software

    Use to manage open windows and display a list of open windows. A Window checkmark appears to the left of the active window. Provides access to the embedded operator manual, the Micromeritics web Help page (www.Micromeritics.com), and information about the application.

  • Page 26: Common Fields And Buttons

    Selects the report destination. Destination When working with report parameters, highlight the item in the Selected Edit Reports list box and click Edit to modify the report details. Gemini VII Operator Manual 2 - 2 239-42828-01 (Rev H ) — May 2021...
  • Page 27 The original file will remain unchanged. No ana- lysis data is added to the file. The only information added is sample information, material properties, liquid properties, analysis and report- ing parameters. Gemini VII Operator Manual 2 - 3 239-42828-01 (Rev H ) — May 2021...
  • Page 28 Operation. Displays the data from the current analysis. View Instrument Log. Displays recent analyses, calibrations, errors, or messages. Instrument Schematic. Displays a schematic of the analyzer system. Gemini VII Operator Manual 2 - 4 239-42828-01 (Rev H ) — May 2021...

  • Page 29: File Status

    Saves the relative pressures and resulting quantities adsorbed as an ASCII text file. These data are derived by dividing the isotherm by the quantity adsorbed at 0.4 relative pressure. Gemini VII Operator Manual 2 - 5 239-42828-01 (Rev H ) — May 2021...
  • Page 30 The density conversion factor in the adsorptive properties file is used to convert quantity adsorbed to volume of condensed adsorptive. Gemini VII Operator Manual 2 - 6 239-42828-01 (Rev H ) — May 2021...

  • Page 31: 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. Gemini VII Operator Manual 2 - 7 239-42828-01 (Rev H ) — May 2021...
  • Page 32 Opens the File Selector window listing sample information files. Shift + F2 Opens the shortcut menu of either the selected component on the analyzer Shift + F9 schematic when manual control is enabled or onscreen reports. Gemini VII Operator Manual 2 - 8 239-42828-01 (Rev H ) — May 2021...

  • Page 33: 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. Gemini VII Operator Manual 2 - 9 239-42828-01 (Rev H ) — May 2021...
  • Page 34 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. Gemini VII Operator Manual 2 - 10 239-42828-01 (Rev H ) — May 2021...

  • Page 35: 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. Gemini VII Operator Manual 2 - 11 239-42828-01 (Rev H ) — May 2021...

  • Page 36: Methods

    The Method drop-down list displays only those methods applicable to the open sample file type. Developer Group view in a CFR21 environment Default Method Examples Default Method Examples Gemini VII Operator Manual 2 - 12 239-42828-01 (Rev H ) — May 2021...
  • Page 37 Specify a default numeric string to be used as a prefix in the Sample Sequence Number field when a new sample file is created. This number increments with [text box] each sample file created. Gemini VII Operator Manual 2 - 13 239-42828-01 (Rev H ) — May 2021...

  • Page 38: Configure The Analyzer

    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. Gemini VII Operator Manual 2 - 14 239-42828-01 (Rev H ) — May 2021...

  • Page 39: Unit Configuration

    Click to display the Unit IP Setup window. Use to change the IP Change IP [button] address and subnet mask assigned during installation. Do not edit these fields unless instructed by a Micromeritics Service Rep- resentative. Restores the controller to factory defaults.

  • Page 40: Instrument Status

    Select the logs to display. Analysis/ Calibration/ Message [check box] For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 2 - 16 239-42828-01 (Rev H ) — May 2021...

  • Page 41: Show Instrument Schematic

    Open Valve. Green indicates an open valve. Closed Valve. Yellow indicates a closed valve. When manual control is disabled, closed valves appear white. Servo Valve. Closed. Servo Valve. Open. Gemini VII Operator Manual 2 - 17 239-42828-01 (Rev H ) — May 2021...
  • Page 42 The reading for the sample pressure transducer is displayed just below the analysis servo valve and valve 5-s. Balance volume adjustment. Can be adjusted by a Micromeritics Service Representative. Pressure relief valve. Prevents excessive pressure build-up in the event of abnormal operation.
  • Page 43 (or right click and select Stop from the menu). Lower. Select Lower and press the keyboard space bar to lower the elevator. Stop. Stops the elevator from moving. Gemini VII Operator Manual 2 - 19 239-42828-01 (Rev H ) — May 2021...

  • Page 44: Show Status

    Use to show the current status for each port. If multiple units are attached to the computer, select Show Status on each Unit [n] menu. The status for all units displays. Gemini VII Operator Manual 2 - 20 239-42828-01 (Rev H ) — May 2021...

  • Page 45: Export Files

    The IP address for the computer and the IP address specified in the setup program must match. The IP address must be 192.168.77.100. Gemini VII Operator Manual 2 - 21 239-42828-01 (Rev H ) — May 2021...

  • Page 46: Software Updates

    Micromeritics application are installed properly. 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). When performing a software update, existing data files are not overwritten. There are three types of subsequent installation: Later version than the current installation.

  • Page 47: Software Uninstall

    The software can be uninstalled two ways. Either method removes only the files required to run the software - not he analysis files. Click the Windows Start icon. Scroll to the Micromeritics entry. Select the Uninstall [analyzer] option, then follow the prompts.
  • Page 48 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 49: 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 50 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. Gemini VII Operator Manual 2 - 26 239-42828-01 (Rev H ) — May 2021...

  • Page 51: Option Presentation For 21Cfr11 Environments

    Lists the current user, successful and failed application user login attempts, and contains a description of all the changes made to sample files. Contains an audit trail of all system initializations, user login attempts, and sample analyses. Gemini VII Operator Manual 2 - 27 239-42828-01 (Rev H ) — May 2021...

  • Page 52: 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 53: Sample Files

    To change the view for the selected window, use the drop-down list at the bottom of the sample file editor. Gemini VII Operator Manual 3 - 1 239-42828-01 (Rev H ) — May 2021...

  • Page 54: Create Sample Files

    The Degas Conditions tab displays only if enabled in Options > Option Presentation > Show Degas Conditions Advanced or Developer view Basic or Analyst view Gemini VII Operator Manual 3 - 2 239-42828-01 (Rev H ) — May 2021...
  • Page 55 If Manually entered is selected, the Isotherm Report becomes available in the Basic/Advanced drop-down list for pasting or importing data into the file. Manually Enter Data on page 3 - Gemini VII Operator Manual 3 - 3 239-42828-01 (Rev H ) — May 2021...
  • Page 56 Common Fields and But- tons on page 2 - * This field label may have been renamed or may not display if modified in Options > Default Methods. Gemini VII Operator Manual 3 - 4 239-42828-01 (Rev H ) — May 2021...

  • Page 57: Open A Sample File

    Preparing 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 Gemini VII Operator Manual 3 - 5 239-42828-01 (Rev H ) — May 2021...
  • Page 58 Advanced or Basic 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. Gemini VII Operator Manual 3 - 6 239-42828-01 (Rev H ) — May 2021...

  • Page 59: Manually Enter Data

    4. On the Sample Description tab, select Manually entered in the Type of Data group box. 5. In the view selector drop-down list at the bottom of the window, click Advanced, then select Isotherm. Gemini VII Operator Manual 3 - 7 239-42828-01 (Rev H ) — May 2021...
  • Page 60 3 Sample Files 6. Ensure that all parameter fields are set appropriately, then click Paste. Gemini VII Operator Manual 3 - 8 239-42828-01 (Rev H ) — May 2021...
  • Page 61 Relative Pressure Quantity Adsorbed (cm3/g STP) 0.996251 403.793 0.86016 389.626 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 Gemini VII Operator Manual 3 - 9 239-42828-01 (Rev H ) — May 2021...
  • Page 62 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. Gemini VII Operator Manual 3 - 10 239-42828-01 (Rev H ) — May 2021...

  • Page 63: 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 Gemini VII Operator Manual 4 - 1 239-42828-01 (Rev H ) — May 2021...

  • Page 64: Adsorptive Properties

    This value is used for a calculated free space. [text box] For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 4 - 2 239-42828-01 (Rev H ) — May 2021...

  • Page 65: Analysis Conditions

    Use to browse for an Analysis Conditions file that contains analysis con- Analysis conditions dition parameters to be used in the analysis. [drop-down box] Gemini VII Operator Manual 4 - 3 239-42828-01 (Rev H ) — May 2021...
  • Page 66 Calculate. Select to have the free-space calculated using the value entered for Volume Correction (entered on the Unit [n] > Unit Configuration window) and the non-ideality factor (entered on the Adsorptive Properties window). Gemini VII Operator Manual 4 - 4 239-42828-01 (Rev H ) — May 2021...
  • Page 67 (models p and t only). Select if is to be ° p° measured for each point. Bath temperature. Calculates using the entered bath temperature. p° Gemini VII Operator Manual 4 - 5 239-42828-01 (Rev H ) — May 2021...
  • Page 68 For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 4 - 6 239-42828-01 (Rev H ) — May 2021...

  • Page 69: 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). Degas Conditions...
  • Page 70 Vacuum level. Evacuation time starts when the vacuum level is reached. For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 4 - 8 239-42828-01 (Rev H ) — May 2021...

  • Page 71: Report Options

    Or, click the Report Options tab when in Advanced option presentation. About Reports on page 6 - 1 Selected Report Options on page 7 - 1 The Calculations document can be found on the Micromeritics web page (www.Micromeritics.com). Additional reports are available using the Reports menu.
  • Page 72 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 But- tons on page 2 - Gemini VII Operator Manual 4 - 10 239-42828-01 (Rev H ) — May 2021...

  • Page 73: 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 Gemini VII Operator Manual 5 - 1 239-42828-01 (Rev H ) — May 2021...
  • Page 74 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. Gemini VII Operator Manual 5 - 2 239-42828-01 (Rev H ) — May 2021...

  • Page 75: 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. Gemini VII Operator Manual 5 - 3 239-42828-01 (Rev H ) — May 2021...
  • Page 76 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. Gemini VII Operator Manual 5 - 4 239-42828-01 (Rev H ) — May 2021...
  • Page 77 11. Rinse the sample tube closure with isopropyl alcohol, then wipe the sample tube closure dry with a clean, lint-free cloth. 12. Label the sample tube and stopper for identification. 13. Replace the rubber stopper. Gemini VII Operator Manual 5 - 5 239-42828-01 (Rev H ) — May 2021...

  • Page 78: Determine The Sample Mass

    7. Remove either the rubber stopper from the sample tube. 8. Use the sample tube funnel (provided in the accessories kit) and pour the sample from the weighing container into the sample tube. Gemini VII Operator Manual 5 - 6 239-42828-01 (Rev H ) — May 2021...
  • Page 79 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. Gemini VII Operator Manual 5 - 7 239-42828-01 (Rev H ) — May 2021...

  • Page 80: Degas The Sample

    Start Degas, then degas the sample using menu commands and information entered on the Degas Conditions tab. The Smart VacPrep Operator Manual can be found on the Micromeritics web page (www.Micromeritics.com). After the sample has been weighed, use a degassing unit to remove any contaminants which may have adsorbed to the surface or pores.

  • Page 81: Sample Tube Installation

    It is not necessary to remove and replace the balance tube between analyses unless it has been contaminated or if using a different size sample tube. Gemini VII Operator Manual 5 - 9 239-42828-01 (Rev H ) — May 2021...
  • Page 82 5 Perform an Analysis 5. Place the Dewar cover under the sample and balance tubes and slide upward until it is 7.5 cm (3 in.) from connector nuts. Gemini VII Operator Manual 5 - 10 239-42828-01 (Rev H ) — May 2021...

  • Page 83: Fill And Install The Dewar

    4. Place the Dewar on the elevator. A Dewar support is not necessary for the larger Dewar used with the Gemini 2390t. Place the Dewar directly on the elevator. 5. Close the safety shield on the front of the analyzer. Gemini VII Operator Manual 5 - 11 239-42828-01 (Rev H ) — May 2021...
  • Page 84 [drop-down box] Click to start the analysis. Start [button] For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 5 - 12 239-42828-01 (Rev H ) — May 2021...

  • Page 85: Perform A Sample Analysis

    Displays the last point pressure and relative pressure for each port. Status window For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 5 - 13 239-42828-01 (Rev H ) — May 2021...

  • Page 86: 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. Gemini VII Operator Manual 5 - 14 239-42828-01 (Rev H ) — May 2021...
  • Page 87 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. Gemini VII Operator Manual 5 - 15 239-42828-01 (Rev H ) — May 2021...

  • Page 88: Perform A Reference Material Analysis

    9. Fill the Dewar with liquid nitrogen to about 5 cm (2 in.) from the top. Allow the Dewar to equi- librate to ambient conditions (approximately 30 minutes). 10. Close the sample compartment door. 11. Go to Unit [n] > Start Analysis. Gemini VII Operator Manual 5 - 16 239-42828-01 (Rev H ) — May 2021...
  • Page 89 The gas lines are not clean. Helium must be 99.995% pure. The measured free space is too high. This indicates the helium may not be pure enough. Gemini VII Operator Manual 5 - 17 239-42828-01 (Rev H ) — May 2021...

  • Page 90: Perform A Quickstart Analysis

    [drop-down box] selected for analysis conditions. For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 5 - 18 239-42828-01 (Rev H ) — May 2021...

  • Page 91: Measure Saturation Pressure

    Click Start. After analysis, go to Unit [n] > Unit Configuration. The recorded value now displays in the Last Measured Po field. Gemini VII Operator Manual 5 - 19 239-42828-01 (Rev H ) — May 2021...

  • Page 93: 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. Gemini VII Operator Manual 6 - 1 239-42828-01 (Rev H ) — May 2021...

  • Page 94: 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. Gemini VII Operator Manual 6 - 2 239-42828-01 (Rev H ) — May 2021...

  • Page 95: Regression Report

    Report [button] 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. Gemini VII Operator Manual 6 - 3 239-42828-01 (Rev H ) — May 2021...
  • Page 96 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 But- tons on page 2 - Gemini VII Operator Manual 6 - 4 239-42828-01 (Rev H ) — May 2021...

  • Page 97: 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. Gemini VII Operator Manual 6 - 5 239-42828-01 (Rev H ) — May 2021...
  • Page 98 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] Gemini VII Operator Manual 6 - 6 239-42828-01 (Rev H ) — May 2021...
  • Page 99 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 But- tons on page 2 - Gemini VII Operator Manual 6 - 7 239-42828-01 (Rev H ) — May 2021...

  • Page 100: 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] Gemini VII Operator Manual 6 - 8 239-42828-01 (Rev H ) — May 2021...
  • Page 101 Tabular report numeric values contributed by each sample. [check box] For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 6 - 9 239-42828-01 (Rev H ) — May 2021...

  • Page 102: 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. 6. Click Save. Gemini VII Operator Manual 6 - 10 239-42828-01 (Rev H ) — May 2021...

  • Page 103: 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. Gemini VII Operator Manual 6 - 11 239-42828-01 (Rev H ) — May 2021...

  • Page 104: 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 105 A problem with either ambient or analysis free space values may indicate a free space measurement error and affect all calculations of quantity adsorbed. Gemini VII Operator Manual 6 - 13 239-42828-01 (Rev H ) — May 2021...
  • Page 106 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). Gemini VII Operator Manual 6 - 14 239-42828-01 (Rev H ) — May 2021...
  • Page 107 McClellan, A.L., and Harnsberger, H.F., Journal of Colloid and Interface Science, 23, 577 (1967). Thomson, W., Phil. Mag. S., 42, 448 (1871). Gemini VII Operator Manual 6 - 15 239-42828-01 (Rev H ) — May 2021...
  • Page 108 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). Gemini VII Operator Manual 6 - 16 239-42828-01 (Rev H ) — May 2021...
  • Page 109 Accumulated error results in the calculation of a too large volume of (possibly nonexistent) small pores if the thickness curve used underestimates film thinning. Gemini VII Operator Manual 6 - 17 239-42828-01 (Rev H ) — May 2021...

  • Page 110: 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. Gemini VII Operator Manual 6 - 18 239-42828-01 (Rev H ) — May 2021...
  • Page 111 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 Gemini VII Operator Manual 6 - 19 239-42828-01 (Rev H ) — May 2021...
  • Page 112 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 But- tons on page 2 - Gemini VII Operator Manual 6 - 20 239-42828-01 (Rev H ) — May 2021...
  • Page 113 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 But- tons on page 2 - Gemini VII Operator Manual 6 - 21 239-42828-01 (Rev H ) — May 2021...
  • Page 114 Scale font. Modifies the font for the scale label. Deselect Use default font to enable font options. Title. Edits the selected axis label. Title font. Modifies the font for the selected axis label. Deselect Use Gemini VII Operator Manual 6 - 22 239-42828-01 (Rev H ) — May 2021...

  • Page 115: 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. Gemini VII Operator Manual 6 - 23 239-42828-01 (Rev H ) — May 2021...
  • Page 116 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 But- tons on page 2 - Gemini VII Operator Manual 6 - 24 239-42828-01 (Rev H ) — May 2021...
  • Page 117 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. Gemini VII Operator Manual 6 - 25 239-42828-01 (Rev H ) — May 2021...
  • Page 118 Deselect this option to remove the grid [selection] lines. For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 6 - 26 239-42828-01 (Rev H ) — May 2021...

  • Page 119: 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. Gemini VII Operator Manual 6 - 27 239-42828-01 (Rev H ) — May 2021...

  • Page 120: Overlay Multiple Sample Files

    3. Click the Report Options tab. 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. Gemini VII Operator Manual 6 - 28 239-42828-01 (Rev H ) — May 2021...
  • Page 121 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. Gemini VII Operator Manual 6 - 29 239-42828-01 (Rev H ) — May 2021...
  • Page 122 Select the status of files to be combined. Status [drop-down box] For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 6 - 30 239-42828-01 (Rev H ) — May 2021...

  • Page 123: Report Examples

    Report Examples EPORT XAMPLES BJH A DSORPTION EPORT Gemini VII Operator Manual 6 - 31 239-42828-01 (Rev H ) — May 2021...

  • Page 124: Horvath-Kawazoe Report

    6 About Reports ORVATH AWAZOE EPORT Gemini VII Operator Manual 6 - 32 239-42828-01 (Rev H ) — May 2021...

  • Page 125: Isotherm Linear Plot Report

    Isotherm Linear Plot Report SOTHERM INEAR EPORT Gemini VII Operator Manual 6 - 33 239-42828-01 (Rev H ) — May 2021...

  • Page 126: Sample Log Report

    6 About Reports AMPLE EPORT Gemini VII Operator Manual 6 - 34 239-42828-01 (Rev H ) — May 2021...

  • Page 127: T-Plot Report

    Report EPORT Gemini VII Operator Manual 6 - 35 239-42828-01 (Rev H ) — May 2021...

  • Page 128: Validation Report

    6 About Reports ALIDATION EPORT Gemini VII Operator Manual 6 - 36 239-42828-01 (Rev H ) — May 2021...

  • Page 129: Selected Report Options

    To edit reports, open the Sample file then select the Report Options tab. Highlight the report name in the Selected Reports list box and click Edit. Gemini VII Operator Manual 7 - 1 239-42828-01 (Rev H ) — May 2021...

  • Page 130: 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. Gemini VII Operator Manual 7 - 2 239-42828-01 (Rev H ) — May 2021...
  • Page 131 Tabular Report. Use to have a tabular report of data generated. For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 7 - 3 239-42828-01 (Rev H ) — May 2021...

  • Page 132: Bet Surface Area Report

    Use Interpolation option. Exclude All. Select to exclude all pressure points in the table. Gemini VII Operator Manual 7 - 4 239-42828-01 (Rev H ) — May 2021...
  • Page 133 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 But- tons on page 2 - Gemini VII Operator Manual 7 - 5 239-42828-01 (Rev H ) — May 2021...

  • Page 134: 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. Gemini VII Operator Manual 7 - 6 239-42828-01 (Rev H ) — May 2021...
  • Page 135 BJH pore volume. Enter the fraction of pores open at both ends to compensate for this error. Gemini VII Operator Manual 7 - 7 239-42828-01 (Rev H ) — May 2021...
  • Page 136 One predefined curve is shipped with the analysis program and is found in the Reference directory. Gemini VII Operator Manual 7 - 8 239-42828-01 (Rev H ) — May 2021...
  • Page 137 Columns must be separated by a space or a tab. For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 7 - 9 239-42828-01 (Rev H ) — May 2021...
  • Page 138 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 But- tons on page 2 - Gemini VII Operator Manual 7 - 10 239-42828-01 (Rev H ) — May 2021...
  • Page 139 Enabled only when Fixed pore size table is selected. For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 7 - 11 239-42828-01 (Rev H ) — May 2021...

  • Page 140: Dft Pore Size 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. Gemini VII Operator Manual 7 - 12 239-42828-01 (Rev H ) — May 2021...
  • Page 141 Shows the pore size. y-axis. Shows the area. Overlay. Select an overlay for the report. Plot Type. Select the method for data display. Gemini VII Operator Manual 7 - 13 239-42828-01 (Rev H ) — May 2021...

  • Page 142: 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. Gemini VII Operator Manual 7 - 14 239-42828-01 (Rev H ) — May 2021...

  • Page 143: 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. Gemini VII Operator Manual 7 - 15 239-42828-01 (Rev H ) — May 2021...
  • Page 144 One predefined curve is shipped with the analysis program and is found in the Reference directory. Gemini VII Operator Manual 7 - 16 239-42828-01 (Rev H ) — May 2021...
  • Page 145 Columns must be separated by a space or a tab. For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 7 - 17 239-42828-01 (Rev H ) — May 2021...
  • Page 146 Highlight any plot option in the Selected Reports list box in the Dollimore-Heal Report Options window, then click Edit. The fields and buttons for these reports are identical to the BJH Plot Report Options. Gemini VII Operator Manual 7 - 18 239-42828-01 (Rev H ) — May 2021...
  • Page 147 Dollimore-Heal Adsorption/Desorption Report OLLIMORE ABULAR EPORT PTIONS BJH Tabular Report on page 7 - 11 Dollimore-Heal Tabular Report Options are identical to the BJH Tabular Report Options. Gemini VII Operator Manual 7 - 19 239-42828-01 (Rev H ) — May 2021...

  • Page 148: 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] Gemini VII Operator Manual 7 - 20 239-42828-01 (Rev H ) — May 2021...
  • Page 149 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 But- tons on page 2 - Gemini VII Operator Manual 7 - 21 239-42828-01 (Rev H ) — May 2021...
  • Page 150 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 But- tons on page 2 - Gemini VII Operator Manual 7 - 22 239-42828-01 (Rev H ) — May 2021...
  • Page 151 /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. Gemini VII Operator Manual 7 - 23...
  • Page 152 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 But- tons on page 2 - Gemini VII Operator Manual 7 - 24 239-42828-01 (Rev H ) — May 2021...

  • Page 153: F-Ratio 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. Gemini VII Operator Manual 7 - 25 239-42828-01 (Rev H ) — May 2021...
  • Page 154 Overlay samples. Use to overlay sample files on the f-plot. For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 7 - 26 239-42828-01 (Rev H ) — May 2021...

  • Page 155: 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. Gemini VII Operator Manual 7 - 27 239-42828-01 (Rev H ) — May 2021...
  • Page 156 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 But- tons on page 2 - Gemini VII Operator Manual 7 - 28 239-42828-01 (Rev H ) — May 2021...

  • Page 157: 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. Gemini VII Operator Manual 7 - 29 239-42828-01 (Rev H ) — May 2021...
  • Page 158 Density. Enter the density per unit area of the adsorptive. * Diameter. Enter the diameter of the gas phase atom. Gemini VII Operator Manual 7 - 30 239-42828-01 (Rev H ) — May 2021...
  • Page 159 [selection] For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 7 - 31 239-42828-01 (Rev H ) — May 2021...
  • Page 160 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. Gemini VII Operator Manual 7 - 32 239-42828-01 (Rev H ) — May 2021...

  • Page 161: Isotherm Report

    Quantity Adsorbed [group box] per gram (cm /g) STP per BET Surface Area (cm ) STP or mmol/g per other Surface Area (cm ) STP or mmol/m Gemini VII Operator Manual 7 - 33 239-42828-01 (Rev H ) — May 2021...
  • Page 162 Weight %. Enter the mass percentage when plotting pressure composition. For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 7 - 34 239-42828-01 (Rev H ) — May 2021...

  • Page 163: 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. Gemini VII Operator Manual 7 - 35 239-42828-01 (Rev H ) — May 2021...
  • Page 164 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 But- tons on page 2 - Gemini VII Operator Manual 7 - 36 239-42828-01 (Rev H ) — May 2021...

  • Page 165: 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. Gemini VII Operator Manual 7 - 37 239-42828-01 (Rev H ) — May 2021...
  • Page 166 Thickness Curve equation for the selected curve. [group box] For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 7 - 38 239-42828-01 (Rev H ) — May 2021...
  • Page 167 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 But- tons on page 2 - Gemini VII Operator Manual 7 - 39 239-42828-01 (Rev H ) — May 2021...
  • Page 168 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. Gemini VII Operator Manual 7 - 40 239-42828-01 (Rev H ) — May 2021...

  • Page 169: 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. Gemini VII Operator Manual 7 - 41 239-42828-01 (Rev H ) — May 2021...

  • Page 170: Sample Audit Trail Report

    This report provides information on: Manual control operations performed during analysis. Information entered using Add Log Entry on the sample file editor. Warnings and/or errors which occurred during analysis. Gemini VII Operator Manual 7 - 42 239-42828-01 (Rev H ) — May 2021...

  • Page 171: Summary Report

    A range can be left open by not selecting the limit. In the text box to the right of Upper / Lower, enter operator instructions to be displayed if a failure is encountered. Gemini VII Operator Manual 7 - 43 239-42828-01 (Rev H ) — May 2021...
  • Page 172 Selects (or deselects) all options. Select All / Deselect All [button] For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 7 - 44 239-42828-01 (Rev H ) — May 2021...

  • Page 173: 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. Gemini VII Operator Manual 7 - 45 239-42828-01 (Rev H ) — May 2021...
  • Page 174 One predefined curve is shipped with the analysis program and is found in the Reference directory. Gemini VII Operator Manual 7 - 46 239-42828-01 (Rev H ) — May 2021...
  • Page 175 Overlay samples. Use to overlay sample files on the t-plot. For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 7 - 47 239-42828-01 (Rev H ) — May 2021...

  • Page 176: 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. Gemini VII Operator Manual 7 - 48 239-42828-01 (Rev H ) — May 2021...
  • Page 177 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 But- tons on page 2 - Gemini VII Operator Manual 7 - 49 239-42828-01 (Rev H ) — May 2021...

  • Page 178: 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. Gemini VII Operator Manual 7 - 50 239-42828-01 (Rev H ) — May 2021...

  • Page 179: 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 180 Select the diagnostic test to be performed. Test [drop-down box] For fields and buttons not listed in this table, see Common Fields and But- tons on page 2 - Gemini VII Operator Manual 8 - 2 239-42828-01 (Rev H ) — May 2021...

  • Page 181: 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 182: Balance 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. Click...

  • Page 183: Match Transducers

    1. Install a blank sample tube or small plug on each port. 2. Click Start. The window closes when the operation is complete. Click when the process is complete. Gemini VII Operator Manual 9 - 3 239-42828-01 (Rev H ) — May 2021...

  • Page 184: Zero Pressure

    2. Ensure that all applicable transducers are selected, then click Start. Click when the pro- cess is complete. The current pressure readings and operation status messages display. Gemini VII Operator Manual 9 - 4 239-42828-01 (Rev H ) — May 2021...

  • Page 185: Sample 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 186: Load Calibration From File

    The default file naming convention for calibration files can be used or the file name can be changed. The default file name of 0217-2013-04-25.CAL is interpreted as: 0217 Analyzer serial number 2013-04-25 Date the calibration file was saved .CAL File name extension Gemini VII Operator Manual 9 - 6 239-42828-01 (Rev H ) — May 2021...

  • Page 187: 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 188 Perform a Reference Material Analysis on page 5 - 16 . Print the results. 3. Contact your Micromeritics Service Representative. Specified pressure not reached. Cause A: Sample or balance tube not properly attached. Action A: Reattach sample and balance tubes. Ensure both are securely attached to ports.
  • Page 189 Action D: Have electrician check cord using a test meter. Replace the cord if defective. Cause E: Loose internal connection or broken wire. Action E: Call a Micromeritics Service Representative for repair or replacement inform- ation. Valves cannot be operated.

  • Page 190: Parts And Accessories

    Parts and accessories can be found online at www.Micromeritics.com. OWER The Gemini VII 2390 is designed to operate with a universal input power supply (100-240VAC) at 50/60Hz. Noise-free power of the correct voltage and frequency, with a safety earth ground, should be available through a standard wall receptacle.

  • Page 191: Safe Servicing

    Safe Servicing ERVICING Do not modify this instrument without the authorization of a Micromeritics service per- sonnel. To ensure safe servicing and continued safety of the instrument after servicing, service personnel should be aware of the following risks: Product specific risks that may affect service personnel: Electrical.

  • Page 192: Guidelines For Connecting Gases

    Do not use flexible gas lines. Some flexible lines may appear to be appropriate, such as those with a herringbone covering, but the line may be coated internally with a polymer. Gemini VII Operator Manual 10 - 6 239-42828-01 (Rev H ) — May 2021...
  • Page 193 500 psi (3500 kPa) on the high pressure gauge. Contaminants absorbed to the walls of the cylinder will desorb as the pressure decreases. Ensure the gas cylinder is closed before connecting to the analyzer. Gemini VII Operator Manual 10 - 7 239-42828-01 (Rev H ) — May 2021...

  • Page 194: Clean And Verify The Gas Line

    2. Select Report after test and select Preview as the destination. Resize the window if this option does not display. 3. Click Start. From the View drop-down list, select either Operation, Instrument Log, or Instru- ment Schematic. Gemini VII Operator Manual 10 - 8 239-42828-01 (Rev H ) — May 2021...
  • Page 195 If the Leak Rate field indicates Failed, a leak is indicated. Check the connections from the regulator shut-off valve to the gas cylinder shut-off valve. Tighten as necessary, then run the test again. Gemini VII Operator Manual 10 - 9 239-42828-01 (Rev H ) — May 2021...
  • Page 196 If running the test again, close the gas cylinder valve before starting the test. 9. Click Close to close the test report. Click Close again to close the test. Gemini VII Operator Manual 10 - 10 239-42828-01 (Rev H ) — May 2021...

  • Page 197: Replace A Gas Cylinder

    6. Use an appropriate wrench to loosen the nut at the regulator connector nut then remove the regulator from the cylinder. 7. Replace the protective cap on the depleted cylinder. Disconnect the retaining strap and move the cylinder to an appropriate location. Gemini VII Operator Manual 10 - 11 239-42828-01 (Rev H ) — May 2021...
  • Page 198 Turn the regulator Shut-off valve counter-clockwise to open. Allow gas to flow until both gauges read approximately zero. d. Close the regulator Shut-off valve to stop gas flow. Gemini VII Operator Manual 10 - 12 239-42828-01 (Rev H ) — May 2021...
  • Page 199 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. Gemini VII Operator Manual 10 - 13 239-42828-01 (Rev H ) — May 2021...

  • Page 200: 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. Gemini VII Operator Manual 10 - 14 239-42828-01 (Rev H ) — May 2021...

  • Page 201: Perform A Leak Test

    ERFORM A Unit [n] > Diagnostics 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. The test provides: Prompts on preparing the analyzer for the test.
  • Page 202 10 Troubleshooting A. Suspend/Resume/ Skip/Play buttons B. Port report buttons C. Live graph settings Gemini VII Operator Manual 10 - 16 239-42828-01 (Rev H ) — May 2021...

  • Page 203: Perform Reference Material Analysis

    2. Place the Dewar support on the elevator, then place a Dewar of water at ambient tem- perature on the Dewar support. (A Dewar support is not necessary for the larger Dewar used with the Gemini VII 2390t. Place the Dewar directly on the elevator.) 3. Go to Unit [n] > Empty Tube Analysis.
  • Page 204 10 Troubleshooting Tolerance in cm ±0.008 ±0.010 ±0.012 ±0.014 ±0.016 ±0.018 ±0.020 ±0.022 ±0.024 Gemini VII Operator Manual 10 - 18 239-42828-01 (Rev H ) — May 2021...

  • Page 205: 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 206: 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. Gemini VII Operator Manual 10 - 20 239-42828-01 (Rev H ) — May 2021...

  • Page 207: 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 208: 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 pump. 5. Smart VacPrep. Gemini VII Operator Manual 10 - 22 239-42828-01 (Rev H ) — May 2021...

  • Page 209: Sample Port Frit Replacement

    3. Use a wrench to remove the connecting nut from the sample port. Pry out the filter (frit) and O-ring. To avoid degassing problems, the frit should be clean and should not be touched with bare hands. Gemini VII Operator Manual 10 - 23 239-42828-01 (Rev H ) — May 2021...
  • Page 210 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. Gemini VII Operator Manual 10 - 24 239-42828-01 (Rev H ) — May 2021...

  • Page 211: Sample Tube O-Ring Replacement

    If the O-ring remains inside the sample port, use the O-ring removal tool from the accessory kit [tool part number 004-54618-00] or use a pair of tweezers or needle- nose pliers to remove it. Gemini VII Operator Manual 10 - 25 239-42828-01 (Rev H ) — May 2021...

  • Page 212: Recover From A Power Failure

    BASED ACUUM The Vacuum Pump Guide can be found on the Micromeritics web page (www.Micromeritics.com). Gemini VII Operator Manual 10 - 26 239-42828-01 (Rev H ) — May 2021...

  • Page 213: A Analyze Samples With A Total Surface Area Of 1.0M2 Or Less A

    (g/cm ); if density is unknown, refer to your labor- atory handbook. b. Determine the number (n) of glass beads needed to equal the sample volume: Gemini VII Operator Manual A - 1 239-42828-01 (Rev H ) — May 2021...
  • Page 214 10. Prepare the analysis Dewar and place it on the elevator. 11. Close the sample compartment door and start the analysis. Gemini VII Operator Manual A - 2 239-42828-01 (Rev H ) — May 2021...
  • Page 215 4. Attach the sample tube to the analysis port and the balance tube to the balance port. 5. Prepare the analysis Dewar and place it on the elevator. 6. Close the sample compartment door and start the analysis. Gemini VII Operator Manual A - 3 239-42828-01 (Rev H ) — May 2021...
  • Page 216 4. Attach the sample tube to the analysis port and the balance tube to the balance port. 5. Prepare the analysis Dewar and place it on the elevator. 6. Close the sample compartment door and start the analysis. Gemini VII Operator Manual A - 4 239-42828-01 (Rev H ) — May 2021...

  • Page 217: B Dft Models

    A graph that plots amount adsorbed versus equilibrium pressure is called an adsorption isotherm. Gemini VII Operator Manual B - 1 239-42828-01 (Rev H ) — May 2021...
  • Page 218 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. Gemini VII Operator Manual B - 2 239-42828-01 (Rev H ) — May 2021...
  • Page 219 It can also be defined as the partial derivative of the grand potential energy with respect to density (or concentration). Gemini VII Operator Manual B - 3 239-42828-01 (Rev H ) — May 2021...
  • Page 220 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. Gemini VII Operator Manual B - 4 239-42828-01 (Rev H ) — May 2021...
  • Page 221 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. Gemini VII Operator Manual B - 5 239-42828-01 (Rev H ) — May 2021...
  • Page 222 Figure 4 shows model isotherms for pores in the micropore size range. Note the logarithmic scale for pressure. Figure 4. Model Isotherms in the Micropore Size Range of Pore Width Argon on Carbon at 87.3 K Gemini VII Operator Manual B - 6 239-42828-01 (Rev H ) — May 2021...
  • Page 223 Non-Local Density Functional Theory with Density-Dependent Weights N2 - Modified Density Functional Geometry: Free surface Substrate: Surface energy Method: Nitrogen at 77K Gemini VII Operator Manual B - 7 239-42828-01 (Rev H ) — May 2021...
  • Page 224 This model reports pore widths from 3.8 to 387 angstroms. Gemini VII Operator Manual B - 8 239-42828-01 (Rev H ) — May 2021...
  • Page 225 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. N2 - Tarazona NLDFT, Esf = 30.0K Gemini VII Operator Manual B - 9 239-42828-01 (Rev H ) — May 2021...
  • Page 226 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 Gemini VII Operator Manual B - 10 239-42828-01 (Rev H ) — May 2021...
  • Page 227 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 Gemini VII Operator Manual B - 11 239-42828-01 (Rev H ) — May 2021...
  • Page 228 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. Gemini VII Operator Manual B - 12 239-42828-01 (Rev H ) — May 2021...
  • Page 229 This model is similar to the model above, but it more appropriate is for characterizing alkali metal exchanged zeolites. The reported pore size range is from 3.5 to 300 angstroms. Gemini VII Operator Manual B - 13 239-42828-01 (Rev H ) — May 2021...

  • Page 230: 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 231 G. Halsey, J. Chem. Phys 16, 931 (1948). Kelvin Equation with Harkins and Jura Thickness Curve N2 - Harkins and Jura Thickness Curve Geometry: Slit Substrate: Average Gemini VII Operator Manual B - 15 239-42828-01 (Rev H ) — May 2021...
  • Page 232 The kernel function is calculated using the Broekhoff-de Boer equation with standard parameters: The nitrogen properties used in the Kelvin equation are: Surface tension = 8.88 dynes cm Molar density = 0.02887g cm N2 - Broekhoff-de Boer Model Gemini VII Operator Manual B - 16 239-42828-01 (Rev H ) — May 2021...

  • Page 233: Dft Model References B

    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). Gemini VII Operator Manual B - 17 239-42828-01 (Rev H ) — May 2021...

  • Page 235: C Exported Data Example C

               Instrument type:    2390                         Original instrument type:    2390                                         Comments:                               Degas Conditions   Degas conditions:    Degas Conditions               Smart VacPrep evacuation      Backfill sample tube:    Automatic                    Evacuation rate:    0.67 kPa/s           Unrest. evacuation from:    0.67 kPa                        Vacuum level:    1.333224e-03 kPa   Gemini VII Operator Manual C - 1 239-42828-01 (Rev H ) — May 2021...
  • Page 236             Hold pressure:    13.3 kPa                           Heating Phase   Sample                     Ramp                prep:     Temperature      Rate      Time      Stage   (°C)  (°C/min)    (min)   ----        1             20          10       10          2            300          20       60   Analysis Conditions   Analysis conditions:    Carbon Run Conditions                 Pressure Table    Starting      Pressure       Ending         Pressure      Increment     Pressure     (p/p°)        (p/p°)        (p/p°)        0.000000000                 0.050000000     0.050000000                 0.075000000     0.075000000                 0.100000000     0.100000000                 0.125000000     0.125000000                 0.150000000   Gemini VII Operator Manual C - 2 239-42828-01 (Rev H ) — May 2021...
  • Page 237   0.300000000                 0.325000000     0.325000000                 0.350000000     0.350000000                 0.375000000     0.375000000                 0.400000000     0.400000000                 0.425000000     0.425000000                 0.450000000     0.450000000                 0.475000000     0.475000000                 0.500000000     0.500000000                 0.525000000     0.525000000                 0.550000000     0.550000000                 0.575000000     0.575000000                 0.600000000     0.600000000                 0.625000000     0.625000000                 0.650000000     0.650000000                 0.675000000     0.675000000                 0.700000000     0.700000000                 0.725000000     0.725000000                 0.750000000     0.750000000                 0.762500000     0.762500000                 0.775000000     0.775000000                 0.787500000     0.787500000                 0.800000000     0.800000000                 0.812500000     0.812500000                 0.825000000     0.825000000                 0.837500000     0.837500000                 0.850000000   Gemini VII Operator Manual C - 3 239-42828-01 (Rev H ) — May 2021...
  • Page 238   0.980000000                 0.990000000                Preparation   Evacuation rate:    40.00 kPa/min     Evacuation time:    2.00 min            Free Space   Calculated                            p° and Temperature            p° type:    Measured in Psat tube for each point     Temperature type:    Entered                                       Temperature:    77.150 K                               Gemini VII Operator Manual C - 4 239-42828-01 (Rev H ) — May 2021...
  • Page 239              Non-ideality factor:    0.0000620              Density conversion factor:    0.0015468       Report Options      Report options:    Carbon Black                             Show report title:    Yes                                           Report title:    Micromeritics Instrument Corporation          Show graphic:    Yes                                           Graphic file:    miclogo.emf                                 Graphic height:    0.250 in                                     Graphic width:    2.000 in                               Gemini VII Operator Manual C - 5 239-42828-01 (Rev H ) — May 2021...
  • Page 240     BJH Cum. Adsorption:    Yes                     BJH Cum. Desorption:    No                      D-H Cum. Adsorption:    No                      D-H Cum. Desorption:    No                              Pore Size   Average pore diameter:    Yes       BJH adsorption avg.:    Yes       BJH desorption avg.:    No        D-H adsorption avg.:    No    Gemini VII Operator Manual C - 6 239-42828-01 (Rev H ) — May 2021...
  • Page 241     Median pore width:    No         Dubinin-Radushkevich   Micropore surface area:    No         Monolayer capacity:    No             Dubinin-Astakhov      Micropore surface area:    No     Limiting micropore volume:    No                  MP-Method         Cumulative surface area:    No            Cumulative pore volume:    No     Average pore hydraulic radius:    No   Gemini VII Operator Manual C - 7 239-42828-01 (Rev H ) — May 2021...

  • Page 243: D O-Ring Compatibility D

    O-ring use, so rigid rules cannot be specified for these materials. Leak rate and ultimate vacuum levels may be used as indicators for O-ring performance. Gemini VII Operator Manual D - 1 239-42828-01 (Rev H ) — May 2021...

  • Page 245: E Worksheets E

    E Worksheets ORKSHEETS Worksheets in this section may be copied as needed. Sample Data Worksheet for Gas Adsorption on the next page Gemini VII Operator Manual E - 1 239-42828-01 (Rev H ) — May 2021...

  • Page 246: Sample Data Worksheet For Gas Adsorption

    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: Gemini VII Operator Manual E - 2 239-42828-01 (Rev H ) — May 2021...
  • Page 249 7 - 23 sample servo valve 9 - 5 transformed isotherm plot options 7 - 24 save to file 9 - 6 clean dewar 10 - 20 Gemini VII Operator Manual Index - 1 239-42828-01 (Rev H ) — May 2021...
  • Page 250 2 - 1 methods, about 2 - 12 heat of adsorption report 6 - 8 MicroActive reports 6 - 11 MP-Method plot report options 7 - 39 Gemini VII Operator Manual Index - 2 239-42828-01 (Rev H ) — May 2021...
  • Page 251 5 - 16, 10 - 17 Isotherm Linear Plot 6 - 33 references, DFT models B - 17 Langmuir 7 - 35 regression report 6 - 3 MicroActive 6 - 11 Gemini VII Operator Manual Index - 3 239-42828-01 (Rev H ) — May 2021...
  • Page 252 2 - 7 show instrument log 2 - 16 show instrument schematic 2 - 17 vacuum pump software oil-based 10 - 26 about 2 - 1 Gemini VII Operator Manual Index - 4 239-42828-01 (Rev H ) — May 2021...
  • Page 253 Index validation report example 6 - 36 validation, report options 7 - 50 warranty i worksheet, sample data E - 2 worksheets E - 1 Gemini VII Operator Manual Index - 5 239-42828-01 (Rev H ) — May 2021...

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