Micromeritics ASAP 2460 Operator's Manual

Accelerated surface area and porosimetry system

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ASAP 2460

Accelerated Surface Area and Porosimetry System

Operator's Manual

V2.01

246-42800-01

Jan 2014

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Page 1 ASAP 2460 Accelerated Surface Area and Porosimetry System Operator’s Manual V2.01 246-42800-01 Jan 2014...
Page 2 Zip," and "MacZip" for its own source and binary releases. © Micromeritics Instrument Corporation 2013 - 2014. All rights reserved. Printed in the U.S.A. The software described in this manual is furnished under a license agreement and may be used or copied only in...
Page 3 MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its products other than the liability stated above. This warranty is in lieu of all other warranties, express or implied, including, but not limited to, the implied warranties of merchantability or fitness for use.
Page 5: Table Of Contents
ASAP 2460 Operator’s Manual Table of Contents TABLE OF CONTENTS 1. USING THE ANALYZER Introduction ..............1-1 Organization of the Operator’s Manual .
Page 6 Table of Contents ASAP 2460 Operator’s Manual Degas Conditions ............2-18 Analysis Conditions .
Page 7 ASAP 2460 Operator’s Manual Table of Contents Summary Report ............3-33 Isotherm Report Options .
Page 8 Table of Contents ASAP 2460 Operator’s Manual Save to File ............. . 4-34 Load from File .
Page 9 ASAP 2460 Operator’s Manual Table of Contents Checking and Cleaning the Analysis Port Dewars....... . 7-5 Replacing Analysis Port Filters .
Page 10 Table of Contents ASAP 2460 Operator’s Manual Equilibration ..............C-6 Thermal Transpiration Correction .
Page 11 ASAP 2460 Operator’s Manual Table of Contents Enter ............... D-2 E.
Page 12 Table of Contents ASAP 2460 Operator’s Manual viii 246-42800-01 - Nov 2013...
Page 13: Using The Analyzer
1. USING THE ANALYZER Introduction This manual provides details on program menu options and operating instructions. This chapter con- tains information on the ASAP 2460 system hardware and software components. Organization of the Operator’s Manual This operator’s manual is organized as follows:...
Page 14 Organization of the Operator’s Manual ASAP 2460 Operator’s Manual Chapter Description (continued) Appendix A FORMS Provides a sample information worksheet used to assist in obtaining a sample mass. Appendix B ERROR MESSAGES Provides a list of program error messages, causes, and actions.
Page 15: Conventions
ASAP 2460 Operator’s Manual Conventions Conventions This manual uses the following icons to identify notes of importance, warnings and cautions. Notes contain important information pertinent to the subject matter. Warnings contain information to help prevent actions that may cause personal injury.
Page 16: Equipment Description
Equipment Description ASAP 2460 Master Module and One Auxiliary Module The ASAP 2460 surface area analyzer is comprised of a Master Module, containing two analysis ports and application software for controlling the analyzer. Up to two Auxiliary Modules may be purchased, increasing the system from a two-port unit to a six-port unit.
Page 17: Gas Requirements
The system includes Isothermal Jackets, which were originally patented by Micromeritics, for the sam- ple tube. The Isothermal Jacket maintains a stable thermal profile along the full length of the sample and Psat tubes.
Page 18: Controls, Indicators, And Connectors
Controls, Indicators, and Connectors This section contains a description of the controls, indicators, and connectors located on the front and side panels of the ASAP 2460 system. Front Panel The front panel of the Master Module and Auxiliary Modules contains analysis stations and saturation pressure ports.
Page 19: Side Panel
ASAP 2460 Operator’s Manual Controls, Indicators, and Connectors Power indicator Sample port connector o port connector For installing the sample tube. Sample port connector For installing a (saturation pressure) tube. port connector Turns on and flashes green while the analyzer is Analyzer power indicator attempting to communicate with the computer.
Page 20: Back Panel
Controls, Indicators, and Connectors ASAP 2460 Operator’s Manual Gas inlet ports  Used to connect up to six analysis gas supplies to the analyzer. When measuring free space, any one of the ports (1 through 6) may be used for helium.
Page 21: Turning On The System
ASAP 2460 Operator’s Manual Turning On the System For connecting the vacuum pump to the analyzer. Vacuum pump port For connecting the analyzer to the computer. Ethernet connector For connecting a SmartPrep degassing unit to the analyzer. RS232 connector For turning the analyzer on and off. This switch also serves On/Off switch as the main breaker for the analyzer;...
Page 22: Reports
Reports ASAP 2460 Operator’s Manual Reports Report options can be specified when creating the sample information file. When an analysis is run, data gathered during the analysis process are compiled into the predefined reports. Reports can also be defined and generated after an analysis has been run. Each selected report is displayed on its own tab and reflects data collected during the analysis.
Page 23: Using The Software
ASAP 2460 Operator’s Manual Using the Software Using the Software The software screens shown in this manual represent a six-port ASAP 2460 system. The number of ports shown on the screens will differ according to the system configuration (from two to six ports).
Page 24: Files
Using the Software ASAP 2460 Operator’s Manual Shortcut Key(s) Function Accesses the online operator’s manual. Displays the File Selector screen. When in the File Selector screen, displays the file search box. When in the File Selector screen, opens the address bar.
Page 25: File Name Conventions
ASAP 2460 Operator’s Manual Using the Software File Status Description (continued) Sample information files that have been used in a degassing operation, but have Prepared not been used in an analysis. This status is applicable only if using the SmartPrep degasser.
Page 26: Libraries
ASCII Libraries The application software contains libraries of the Micromeritics application-specific files. The library is located within the File Selector window. The Library provides an easy way to locate and open appli- cation-specific files. For example, to locate and open a sample information file, click the Sample Information library folder on the left.
Page 27: Menu Structure
ASAP 2460 Operator’s Manual Using the Software Library Name Default Directory File extension 2460\Data .MTH Methods 2460\Param .RPO Report Options 2460\Data .SMP Sample Information 2460\Param .STB Sample Tube Menu Structure All program functions are located on menus accessed from the menu bar. Each menu contains com- mands and, in some cases, a submenu.
Page 28: Window Menu
Arranges the symbols for all minimized windows. Arrange Icons Help Menu The Help menu provides access to the online operator’s manual, the Micromeritics web page, tutorials, and information about the analyzer. Help Menu Option Description Provides access to the online operator’s manual.
Page 29: Setup Program
Using the Software Help Menu Option Description (continued) Provides access to instructional tutorials. Tutorials Provides a link to the Micromeritics web page: Micromeritics on the www.Micromeritics.com Provides an Internet link to additional 2460 information. ASAP 2460 on the Web Provides the analysis program version number.
Page 30 Using the Software ASAP 2460 Operator’s Manual 1-18 246-42800-01 - Aug 2013...
Page 31: Operational Procedures
ASAP 2460 Operator’s Manual Introduction 2. OPERATIONAL PROCEDURES Introduction This chapter contains information on: • working with Interactive Reports • editing the default method • creating sample files in Advanced, Basic, and Restricted formats • defining parameter files • manually entering data •...
Page 32 Working with Interactive Reports ASAP 2460 Operator’s Manual To view the plots in either Relative or Absolute pressure, click the Relative or Absolute option. The dropdown list at the bottom of the window shows Isotherm as the current choice. To view another report or to view the sample information file, click the dropdown arrow.
Page 33 ASAP 2460 Operator’s Manual Working with Interactive Reports For example, if BET Surface Area is selected, a window similar to the following displays: When data are edited, the changes are reflected immediately in the plots and the summary data displayed in the window. Some editing options are: •...
Page 34: Editing The Default Method
Editing the Default Method ASAP 2460 Operator’s Manual Editing the Default Method Sample files include the information required by the analyzer to perform analyses and collect data. A method is a template for sample files that contains the parameters to be used for an analysis. The anal- ysis software contains a default method.
Page 35 ASAP 2460 Operator’s Manual Editing the Default Method In the Sample file name text box, enter an optional default file name. This information will be appended to the sequence number as a part of the file name and will also display in the Sample text box when a sample file is created.
Page 36: Creating Methods
Creating Methods ASAP 2460 Operator’s Manual Creating Methods In addition to the default method, you can create methods to be used when creating a new sample file as described below. Go to File > New and create a new Sample Information file.
Page 37 ASAP 2460 Operator’s Manual Creating Methods On the Method tab, if files created using this Method are to be saved in a file directory other than the default, select the Use separate sample file directory checkbox and click the Browse icon to select a directory.
Page 38: Defining Sample Information Files
Defining Sample Information Files ASAP 2460 Operator’s Manual Defining Sample Information Files A sample information file must be created for each analysis. This file can be created prior to or at the time of analysis. The sample information file identifies the sample, guides the analysis, and specifies report options.
Page 39 ASAP 2460 Operator’s Manual Defining Sample Information Files Ensure that the Advanced option is checked in the Options > Option Presentation menu. Go to File > New Sample. Some text boxes may have different field labels if renamed or may not display if omitted in the Default Method.
Page 40 Defining Sample Information Files ASAP 2460 Operator’s Manual In the Mass group box, indicate if mass is to be manually entered by the operator (Enter) or calculated by the system (Calculate). Refer to box, page 3-12. Mass group In the Type of Data group box, indicate if the data is to be automatically collected by the system or manually entered by the operator.
Page 41: Basic Or Restricted Format
ASAP 2460 Operator’s Manual Defining Sample Information Files Basic or Restricted Format The Basic and Restricted formats use predefined parameter files to create a sample information file. Refer to Files, page 3-10. Sample Information • When using the Basic format, switch to the Advanced format to edit parameter file values.
Page 42: Opening Sample Information Files
Defining Sample Information Files ASAP 2460 Operator’s Manual Click the dropdown arrows to select default parameter files for Degas conditions, Analysis conditions, and Report options. To auto-populate fields from another .SMP file, click the Replace All button and select a .SMP file that contains the desired parameters.
Page 43: Opening Files With A Status Of Complete, Analyzing, Or Entered
ASAP 2460 Operator’s Manual Defining Sample Information Files Opening Files with a Status of Complete, Analyzing, or Entered Go to File > Open or use the F2 keyboard shortcut. From the Sample Information library folder, select a .SMP file with a status of Complete, Analyzing, or Entered and click Open (or double click the file name).
Page 44: Opening Files With A Status Of Preparing, Prepared, Or No Analysis
Defining Sample Information Files ASAP 2460 Operator’s Manual Opening Files with a Status of Preparing, Prepared, or No Analysis Go to File > Open or use the F2 keyboard shortcut. To sort the file list by status, click the Mic Status column header.
Page 45 ASAP 2460 Operator’s Manual Defining Sample Information Files The Sample Description window displays in the specified format (Advanced, Basic, or Restricted). The following window is shown in Advanced format. 246-42800-01 - Aug 2013 2-15...
Page 46: Defining Parameter Files
Defining Parameter Files ASAP 2460 Operator’s Manual Defining Parameter Files The following file types can exist as part of the sample information file as well as individual parameter files: • Sample Tube Files .STB file extension • Degas Conditions .DEG file extension •...
Page 47 ASAP 2460 Operator’s Manual Defining Parameter Files Enter a description in the Sample Tube field. This description displays in the Sample tube dropdown list on the Sample Description tab. In the Blank Tube Properties group box, enter the warm free space and the cold free space.
Page 48: Degas Conditions
Defining Parameter Files ASAP 2460 Operator’s Manual Degas Conditions Degas Conditions files contain degassing information for sample preparation. Degassing is a required step in preparation for the analysis; however, the Degas Conditions tab is only applicable if using the SmartPrep Degasser. This section contains degassing instructions that will be sent to the SmartPrep Degasser equipment.
Page 49: Analysis Conditions
ASAP 2460 Operator’s Manual Defining Parameter Files To overwrite degas conditions with parameters from another Degas Conditions file, click the Degas Conditions dropdown arrow and select a file from the list or click Browse, then locate and select the .DEG file containing the new parameters and click Open.
Page 50 Defining Parameter Files ASAP 2460 Operator’s Manual Click OK when prompted to create a new file. To overwrite run conditions with parameters from another Analysis Conditions file, click the Description dropdown arrow and select a file from the list or click Browse, then locate and select the .ANC file containing the new parameters and click Open.
Page 51: Adsorptive Properties
ASAP 2460 Operator’s Manual Defining Parameter Files Adsorptive Properties Adsorptive properties provide the adsorptive (analysis gas) characteristics for the analysis. Go to File > Open. Select the Adsorptive Properties library folder and enter a file name in the File name field.
Page 52 Defining Parameter Files ASAP 2460 Operator’s Manual Enter the mnemonic for the Adsorptive gas (for example, N2) in the Mnemonic text box. Click Psat vs T to edit the Psat vs Temperature table. Edit any other field(s) on this dialog as required, then click Enter the appropriate information (or accept the defaults) in the following fields.
Page 53: Report Options
ASAP 2460 Operator’s Manual Defining Parameter Files Report Options Report Options files specify the type of reports that will be generated from an analysis or from manu- ally entered data. They also contain report details, for example, axis scale, axis range, and column headings.
Page 54 Defining Parameter Files ASAP 2460 Operator’s Manual Click OK when prompted to create a new file. To overwrite report options with parameters from another Report Options file, either click the Report Options dropdown arrow and select a file from the list or click Browse, then locate and select the .RPO file containing the new parameters and click Open.
Page 55: Importing Manually Entered Isotherm Data From The Interactive Isotherm Window
ASAP 2460 Operator’s Manual Defining Parameter Files Importing Manually Entered Isotherm Data from the Interactive Isotherm Window When importing isotherm data from an external ASCII text file using the Import button on the interac- tive isotherm window, the ASCII text file must follow these rules: ASCII text file format rules •...
Page 56: Copying / Pasting Manually Entered Isotherm Data
Defining Parameter Files ASAP 2460 Operator’s Manual Resize the isotherm window until the Import button displays. Import button Ensure that all parameter fields are set appropriately then click Import. On the File Selector window, locate and select the .TXT file and click Open. The isotherm data from the original sample file is imported and displays in the new sample file.
Page 57 ASAP 2460 Operator’s Manual Defining Parameter Files Right click in the graph area of the interactive reports window and select Copy Data. This will copy the data from the active file to the clipboard. Right click in the graph area and...
Page 58: Preparing For Analysis
Sample tubes and filler rods must be clean and dry before samples are added and weighed. The follow- ing table indicates which materials are supplied by Micromeritics and which are supplied by the user. The procedures in the following the table are recommended.
Page 59 ASAP 2460 Operator’s Manual Preparing for Analysis Fill the sample tubes with warm water and place them in the ultrasonic cleaning unit. Then place the filler rods in the unit. Turn on the ultrasonic cleaning unit for approximately fifteen minutes.
Page 60: Determining The Sample Mass
Preparing for Analysis ASAP 2460 Operator’s Manual Remove the sample tubes and filler rods from the oven and allow to cool. 10. Blow out the sample tubes with oil-free compressed air. 11. Label the sample tube and stopper for identification.
Page 61: Degassing The Sample
[C] Sample mass (Before Degas). Degassing the Sample After the sample has been weighed, use a degassing unit to remove any contaminants which may have adsorbed on the surface or in pores. Appropriate degassing units are available from Micromeritics. Refer to INFORMATION, page for ordering information.
Page 62 Preparing for Analysis ASAP 2460 Operator’s Manual After degassing is complete, perform the following steps: Weigh the sample tube set containing the sample and record the weight on the Sample Data Worksheet as [B] Sample tube set plus sample mass (After Degas).
Page 63: Installing Sample Tubes
ASAP 2460 Operator’s Manual Installing Sample Tubes Installing Sample Tubes Remove the closure from the sample tube. If a filler rod is used, slide the filler rod slowly into the sample tube. Slide an isothermal jacket down over the sample tube stem until it touches the sample tube bulb.
Page 64: Filling Dewars
Filling Dewars ASAP 2460 Operator’s Manual Filling Dewars Precautions Always handle dewars with care. Any product incorporating a vacuum is a potential safety hazard and should be treated with caution. We recommend the following be observed when handling dewars containing liquefied gases: •...
Page 65: Filling An Analysis Dewar
ASAP 2460 Operator’s Manual Filling Dewars Filling an Analysis Dewar Fill the analysis dewar with the analysis bath fluid to about 5 cm (2 inches) from the top.  Incorrect fluid levels can lead to measurement errors. Do not overfill the dewar.
Page 66 Filling Dewars ASAP 2460 Operator’s Manual Insert the dipstick into the Dewar and check the level of the analysis bath liquid. Condensation should not exceed the Level Indicator mark. Level indicator mark Wetness or frozen  condensation indicates bath liquid...
Page 67 ASAP 2460 Operator’s Manual Filling Dewars Place the dewar on the elevator under the sample tube.  246-42800-01 - Aug 2013 2-37...
Page 68 Filling Dewars ASAP 2460 Operator’s Manual Attach the safety shield to the two hooks on the front panel to enclose the sample tube and dewar. Begin the analysis as described in the next topic. 2-38 246-42800-01 - Aug 2013...
Page 69: Performing An Analysis
ASAP 2460 Operator’s Manual Performing an Analysis Performing an Analysis Analyses may be performed in one of these modes: • Standard • Krypton • High Throughput • Micropore Before beginning an analysis, make sure the tank pressure for the gas regulator is at least 200 psig.
Page 70 Performing an Analysis ASAP 2460 Operator’s Manual Select Unit > Start Analysis. Select the port to be used for analysis. Click Browse and select a sample information file or click New to create a new sample information file. Verify the information populated into the sample identification, Density, Mass, Sample + Tube, and Empty Tube fields.
Page 71 ASAP 2460 Operator’s Manual Performing an Analysis Click Start to start the analysis. A window displays data as they are collected. A short delay is encountered before the port status at the bottom of the window changes from the Idle state.
Page 72: Krypton Analysis
Performing an Analysis ASAP 2460 Operator’s Manual Krypton Analysis Krypton analyses are available only if the Krypton option is installed on the analyzer. Use the following guidelines for performing krypton analyses: • All ports must be idle in order to start an analysis.
Page 73 ASAP 2460 Operator’s Manual Performing an Analysis Select Unit > Start Krypton Analysis. The Krypton Analysis window is displayed. For each port to be used, either click Browse and select a sample information file or click New to create a new sample information file.
Page 74: High Throughput Analysis
Performing an Analysis ASAP 2460 Operator’s Manual Click Start to start the analysis. A window displays data as they are collected. A short delay is encountered before the port status at the bottom of the window changes from the Idle state.
Page 75 ASAP 2460 Operator’s Manual Performing an Analysis Select Unit > Start High Throughput Analysis. The High Throughput Analysis dialog is displayed. Perform steps 3 through 9 in the topic Analysis, page 2-42. Krypton 246-42800-01 - Aug 2013 2-45...
Page 76: Micropore Analysis
Performing an Analysis ASAP 2460 Operator’s Manual Micropore Analysis Micropore analyses are available only if the Micropore option is installed on the analyzer. In Micropore mode, up to six analyses are started together. Once a set is started, no other samples can be started until the set is complete.
Page 77: Generating Reports
ASAP 2460 Operator’s Manual Generating Reports Generating Reports Select Reports > Start Report. Select a .SMP file from the library. The selected report name appears in the File name text box. To select more than one file, hold down the Ctrl key on the keyboard while selecting the files, or hold down the Shift key to select a range of files.
Page 78 Generating Reports ASAP 2460 Operator’s Manual If only one file was selected in Step 1, the Select Reports window displays. Verify the reports to generate and select additional reports if necessary. Click OK. If multiple files were selected, this window does not display.
Page 79: Listing Files
ASAP 2460 Operator’s Manual Listing Files Listing Files Provides the option to create a list of sample file information, for example, file name, date, time the file was created or last edited, file identification, and file status. Select File > List.
Page 80 Listing Files ASAP 2460 Operator’s Manual • File - select the destination directory. Enter a new file name in the File name field or accept the default. Select to save the file as a report system (.REP), a spreadsheet (.XLS), or an ASCII text (.TXT) file format.
Page 81: Exporting Files
ASAP 2460 Operator’s Manual Exporting Files Exporting Files Provides the option to export the contents of one or more sample files to either the screen, a printer, or to a file. Isotherm data can be exported as a .REP, .TXT, or .XLS file format. You can select the type of data to include or exclude during the export process.
Page 82 Exporting Files ASAP 2460 Operator’s Manual Types of data that can be included: • Options – Target pressures • Quantity adsorbed versus relative pressure • Quantity dosed, absolute pressure, elapsed time, free space, Psat measurements • Sample log • Labels...
Page 83: Generating Graph Overlays
ASAP 2460 Operator’s Manual Generating Graph Overlays Generating Graph Overlays Use the graph overlay function to compare multiple graph options. Graphical lines are differentiated by the use of varying colored symbols outlined on a legend. Overlays may be generated in two ways: •...
Page 84 Generating Graph Overlays ASAP 2460 Operator’s Manual Click the Report Options tab at the top of the window. Refer to the following table for instructions for the selected report. Highlight the report to overlay, then click Edit. If overlaying this type of Then...
Page 85 ASAP 2460 Operator’s Manual Generating Graph Overlays If overlaying this type of Then... (continued) report... a.) In the Selected Reports list box, highlight one of the report • BET Surface Area options shown on the left and click Edit. • Langmuir Surface Area •...
Page 86 Generating Graph Overlays ASAP 2460 Operator’s Manual On the Plot Overlay Sample Selection window, use one of the following options to move up to 25 files from the Available Files box to the Selected Files box. • Double click a file name in the Available Files box to move the file to the Selected Files box.
Page 87 ASAP 2460 Operator’s Manual Generating Graph Overlays The report screen displays with tabs across the top of the screen. Click each tab to view the reports. Refer to Bar, page 5-17. Report Tool 246-42800-01 - Aug 2013 2-57...
Page 88: Multiple Graph Overlays
Generating Graph Overlays ASAP 2460 Operator’s Manual Multiple Graph Overlays The overlay process allows the importing of pore-size distribution data from an ASCII text file. The ASCII text file must follow the format rules outlined below. Multiple graph overlays can only be generated for: •...
Page 89 ASAP 2460 Operator’s Manual Generating Graph Overlays To import the ASCII text file to generate graph overlays: The following steps use BJH Adsorption as an example. Screen appearance will vary depending on the selected report. Go to File > Open. Select a sample file to overlay graphs of other samples. To select more than one file, hold down the Ctrl key on the keyboard while selecting the files, or hold down the Shift key to select a range of files.
Page 90 Generating Graph Overlays ASAP 2460 Operator’s Manual b.) If the ASCII text file does not display on the Select Imported Overlays window, click Import. Locate the file, then click Open. Header information from the ASCII text file will then appear in the Select Imported Overlays window. If an error message appears instead, verify that the .TXT file format (listed above) is correct.
Page 91 ASAP 2460 Operator’s Manual Generating Graph Overlays From the Report Options window, in the Selected Reports list box, select a sub-report and click Edit. Select a sub- report Click Edit Click the dropdown arrow at the Variable field and select a variable to overlay. Then click the dropdown arrow of the Overlay field and select the Imported Data entry.
Page 92 Generating Graph Overlays ASAP 2460 Operator’s Manual To view the report, click the Preview button on the Sample Description window. If the sample file has been closed, go to Reports > Start Report. Select the file used in the previous steps and click Report. To select more than one file, hold down the Ctrl key on the keyboard while selecting the files, or hold down the Shift key to select a range of files.
Page 93 ASAP 2460 Operator’s Manual Generating Graph Overlays 246-42800-01 - Aug 2013 2-63...
Page 94 Generating Graph Overlays ASAP 2460 Operator’s Manual 2-64 246-42800-01 - Aug 2013...
Page 95: File Menu
ASAP 2460 Operator’s Manual Introduction 3. FILE MENU Introduction This chapter contains information specific to the File menu options used to create and open sample and parameter files. This chapter provides details of File menu options, commonly used functions and but- tons, and field descriptions.
Page 96 Common Fields and Buttons - File Menu Options ASAP 2460 Operator’s Manual Field or Button Description (continued) On report parameters screens, the From / To fields are enabled when Axis Range Autoscale options are not selected. Enter the starting and ending values for the x- and/or y-axes.
Page 97 ASAP 2460 Operator’s Manual Common Fields and Buttons - File Menu Options Field or Button Description (continued) File name text box Select a file from either the Name column or from the application Library. The file name displays in the File name text box. Click Open or double- click the file name to open the file.
Page 98: New Sample
New Sample ASAP 2460 Operator’s Manual New Sample Provides the option to create a new sample file or parameter file. Refer to Sample Information Files, page 3-10. 246-42800-01 - Aug 2013...
Page 99: Open
ASAP 2460 Operator’s Manual Open Open Provides access to the application Library. Refer to Libraries, page for information on Manage managing libraries.  Library • Sample Information files - the File name text box contains the next sequential sample information file name generated by the program.
Page 100: Save All
Save All ASAP 2460 Operator’s Manual file, go to File > Save As, select the Analysis Conditions folder in the application Library and enter a file name in the File name field. Click Save. Save All Saves all active windows under the current file names.
Page 101: Close
ASAP 2460 Operator’s Manual Close Close Closes the active window. If changes were made and not yet saved, a prompt displays providing the option to save the file. • Yes - saves the changes, then closes the window • No - closes the window without saving the changes •...
Page 102: Export
Exports isotherm data in a sample information file as a .REP, .TXT or .XLS file. When saved to a file, the data can be imported into other applications. Convert llows you to convert sample information files created with an ASAP 2400, ASAP 2405, or ASAP 2420 system to files compatible with the ASAP 2460 system. 246-42800-01 - Aug 2013...
Page 103: Exit
ASAP 2460 Operator’s Manual Exit Exit Exits the application program. If a file is open with unsaved changes, a prompt displays providing the option to save the changes and exit or to exit the program without saving the changes. • Yes - saves the changes, then closes the window •...
Page 104: Sample Information Files
Sample Information Files ASAP 2460 Operator’s Manual Sample Information Files File > New Sample Each analysis must be linked with a sample information file before the analysis can proceed. A sample information file can consist of parameter files, however, parameter files can also stand alone.
Page 105 ASAP 2460 Operator’s Manual Sample Information Files Field or Button Description (continued) Sample text box Enter a description of the sample. Enter identification information in the respective text boxes. Some text Operator / Submitter text boxes boxes may have been renamed or may not display if modified in Options >...
Page 106 Sample Information Files ASAP 2460 Operator’s Manual Field or Button Description (continued) • Use filler rod checkbox - select if a filler rod is to be used in the sample Sample Tube dropdown list tube. A filler rod reduces the stem free space volume resulting in (continued) reduction of free space error.
Page 107: Degas Conditions File
ASAP 2460 Operator’s Manual Degas Conditions File Field or Button Description (continued) Use to enter information to appear in the sample log report that cannot be Add Log Entry button recorded automatically through the application. Click the button again to enter multiple log entries.
Page 108 Degas Conditions File ASAP 2460 Operator’s Manual Field or Button Description Use to select for a .DEG file that contains degas condition parameters to be Degas Conditions dropdown list used in the analysis. Heating Phase table Enter up to five stages of degas conditions.
Page 109: Analysis Conditions Files
ASAP 2460 Operator’s Manual Analysis Conditions Files Analysis Conditions Files File > Open > Analysis Conditions (or click the Analysis Conditions tab when in Advanced format or use the F3 keyboard shortcut) The Analysis Conditions tab provides details for setting up the sample analysis conditions file.
Page 110 Analysis Conditions Files ASAP 2460 Operator’s Manual Field or Button Description (continued) • Adsorptive dropdown list- defaults to the adsorptive listed on the Adsorptive (continued) previous window. • Mnemonic - enter the mnemonic name for the adsorptive. • Non-condensing adsorptive - Select this option if this file is for a non- condensing gas (adsorptive).
Page 111 ASAP 2460 Operator’s Manual Analysis Conditions Files Field or Button Description (continued) Specify how isotherms are to be collected: Target Pressures or Dose Isotherm Collection group box Increments. Select to have isotherms collected by specifying target pressures. Select this Target Pressures option option to enable the Pressures and Options buttons.
Page 112 Analysis Conditions Files ASAP 2460 Operator’s Manual Field or Button Description (continued) Several analysis conditions files containing complete pressure tables are Target Pressures option (continued) included with the analysis program. When using these files, it is recommended to use the File > Save As option to save the file as a different name and edit the new file.
Page 113 ASAP 2460 Operator’s Manual Analysis Conditions Files Field or Button Description (continued) Target Pressures Options button • First Pressure Fixed Dose - Select this option to have the sample dosed with a specified amount of gas until the first pressure point is reached. This initial dosing quickly meets the adsorptive demand of the sample.
Page 114 Analysis Conditions Files ASAP 2460 Operator’s Manual Field or Button Description (continued) • Absolute / Relative pressure tolerance - values used to determine how Target Pressures Options button close the actual pressure must be to each target pressure from the (continued) pressure table.
Page 115 ASAP 2460 Operator’s Manual Analysis Conditions Files Field or Button Description (continued) • Equilibration delay - Enabled when Low pressure incremental dose Target Pressures Options button mode is selected. (continued) Minimum: Prevents premature equilibration caused by reduced percentage sensitivity to pressure changes at the lowest pressures.
Page 116 Analysis Conditions Files ASAP 2460 Operator’s Manual Field or Button Description (continued) • Low Pressure incremental dose mode - Choose this option when you Dose Increments option (continued) are performing an analysis of microporous materials. At low pressures on Type 1 isotherms, the pressure points are very closely spaced, making a useful pressure table difficult to define.
Page 117 ASAP 2460 Operator’s Manual Analysis Conditions Files Field or Button Description (continued) Preparation button • Fast evacuation - Select Fast evacuation when analyzing samples (such as pellets) that do not fluidize or shed particles under evacuation. • Evacuation rate / Unrestricted evac. from - enter the evacuation rate and the pressure at which unrestricted sample evacuation is to begin.
Page 118 Analysis Conditions Files ASAP 2460 Operator’s Manual Field or Button Description (continued) Free Space button Click to enter the type of free space measurement. Free Space button • Measure - select to measure the free space automatically over the (continued) sample prior to data collection.
Page 119 ASAP 2460 Operator’s Manual Analysis Conditions Files Field or Button Description (continued) pº and T button Click to select options for obtaining the saturation pressure (p ) and analysis bath temperature. Each selected option presents a different set of parameters at the bottom of the screen.
Page 120 Analysis Conditions Files ASAP 2460 Operator’s Manual Field or Button Description (continued)  pº and T button Click to edit the values of the Psat vs T table. Editing the val- Psat vs T (continued) ues in the current table does not affect the original table.
Page 121 ASAP 2460 Operator’s Manual Analysis Conditions Files Field or Button Description (continued) Equilibration button Click to enter values for relative or absolute pressure. Column heading reads Absolute Pressure (mmHg) when Absolute Pressure Dosing is selected. Does not display when Absolute...
Page 122 Analysis Conditions Files ASAP 2460 Operator’s Manual Field or Button Description (continued) Equilibration button Click to enter values for relative or absolute pressure. Column heading reads Absolute Pressure (mmHg) when Absolute Pressure Dosing is selected Does not display when Absolute...
Page 123 ASAP 2460 Operator’s Manual Analysis Conditions Files Field or Button Description (continued) Backfill button Click to enter options for backfilling the sample tube. Indicate if the sample should be backfilled at the start and/or end of the analysis. Click the dropdown arrow and select the backfill gas to be used.
Page 124: Common Fields And Buttons - Report Options
Common Fields and Buttons - Report Options ASAP 2460 Operator’s Manual Common Fields and Buttons - Report Options Field or Button Description (continued) Pressures button This option is available when the sample file has a status of Analyzing or Complete. Use to enter a range of pressure points to be included in the report or to modify table values for pressure points.
Page 125: Report Options Files
ASAP 2460 Operator’s Manual Report Options Files Report Options Files File > Open > [.RPO file] (or click the Report Options tab when in Advanced format) Use to specify report options for 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 com- ponents of thickness curve equations.
Page 126 Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued) Overlays button Refer to Overlays, page 2-53. Multiple Sample Import button Use to import up to 25 pore distribution data files. These datasets are shown only in BJH and Dollimore-Heal reports.
Page 127: Summary Report
ASAP 2460 Operator’s Manual Report Options Files Summary Report The Summary Report provides a condensed listing of selected data results. In the Selected Reports list box, highlight Summary, then click Edit. Select the data types to include in the Summary report.
Page 128 Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued)  • Pass/Fail [n] button - select the S A: Single-point BET checkbox to Item [n] (continued) enable this button. Click the Pass/Fail [n] button to display the Pass/ Fail Options window for selection of pass/fail criteria.
Page 129: Isotherm Report Options
ASAP 2460 Operator’s Manual Report Options Files Isotherm Report Options The Isotherm report indicates adsorption (up to saturation pressure) and desorption (down from satu- ration pressure) of a gas by a solid held at constant temperature. In the Selected Reports list box, highlight Isotherm, then click Edit.
Page 130 Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued)  Select the options to include on the report. Tabular Options group box • Weight % - enter the weight percentage when plotting pressure composition. • Elapsed time - time elapsed during the analysis.
Page 131: Bet/Langmuir Surface Area Report Options
ASAP 2460 Operator’s Manual Report Options Files BET/Langmuir Surface Area Report Options The Langmuir and BET Surface Area windows are identical unless otherwise specified. In the Selected Reports list box, highlight BET (or Langmuir) Surface Area, then click Edit. • The BET calculation obtains the sample surface area value by determining the monolayer volume of adsorbed gas from the isotherm data.
Page 132 Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued)  Use to generate a traditional BET (Langmuir) surface area plot used to BET (or Langmuir) determine monolayer volume and BET C constant. Transform plot • Overlay samples checkbox - use to overlay sample files on the BET (or Langmuir) transform plot.
Page 133: Freundlich Report Options
ASAP 2460 Operator’s Manual Report Options Files Freundlich Report Options The Freundlich Isotherm is an empirical isotherm used to model low-pressure adsorption data. It can also be applied to model some micropore isotherms. In the Selected Reports list box, highlight Freundlich, then click Edit.
Page 134 Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued) Plots the absolute pressure vs quantity adsorbed. Shows best fit line. Freundlich Isotherm plot checkbox • Overlay samples checkbox - use to overlay sample files on the Freundlich isotherm plot.
Page 135: Temkin Isotherm Report Options
ASAP 2460 Operator’s Manual Report Options Files Temkin Isotherm Report Options The Temkin isotherm is used to model adsorption data where the heat of adsorption drops linearly with increasing coverage. In the Selected Reports list box, highlight Temkin, then click Edit.
Page 136 Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued) Overlays the Temkin isotherm with the analysis data. Temkin Isotherm plot checkbox • Overlay samples checkbox - use to overlay sample files on the isotherm plot. • Autoscale x-axis - linear x-axes begin at zero. The x-axis field shows the absolute pressure.
Page 137: T-Plot Report Options
ASAP 2460 Operator’s Manual Report Options Files t-Plot Report Options The t-Plot calculation allows quantitative analysis of the area and total volume ascribed to micropores. Matrix area (the area external to micropores) is directly determined and often proves to be a valuable way of characterizing complex mixed materials.
Page 138 Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued) Thickness Curve group box (continued) To import values from an existing thickness curve (.THK file), click Open and select the file containing the values. The table to be imported must have a .TXT or .THK file extension and have a two-column format with the relative pressures in the first column and the thickness values in the second column.
Page 139 ASAP 2460 Operator’s Manual Report Options Files Field or Button Description (continued)  Enter the value to correct for surface areas that are not smooth. Surface area correction factor text box This brings the values for BET surface area and micropore surface area into accordance.
Page 140: Alpha-S Method
Report Options Files ASAP 2460 Operator’s Manual Alpha-S Method The Alpha-S plot converts the standard adsorption isotherm into a dimensionless isotherm using the quantity adsorbed at a relative pressure of 0.4. In the Selected Reports list box, highlight Alpha-S Method, then click Edit.
Page 141 ASAP 2460 Operator’s Manual Report Options Files Field or Button Description (continued)  Enter the surface area from the reference curve. This value is used to Ref. surface area text box calculate the sample surface area. Enter minimum and maximum relative pressures to determine the fit.
Page 142: F-Ratio Method
Report Options Files ASAP 2460 Operator’s Manual f-Ratio Method The f-Ratio report uses the measured isotherm and normalizes it using a reference isotherm. In the Selected Reports list box, highlight f-Ratio Method, then click Edit. Field or Button Description Click Browse to select a sample file to use as a reference for the isotherm.
Page 143: Bjh Adsorption/Desorption Report Options
ASAP 2460 Operator’s Manual Report Options Files BJH Adsorption/Desorption Report Options The BJH calculation determines the mesopore volume/area distribution which accounts for both the change in adsorbate layer thickness and the liquid condensed in pore cores. Reports can be generated from both adsorption and desorption data.
Page 144 Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued) Pores group box Enter the minimum and maximum diameter (radius or width) of pores to include in the BJH reports. • Fraction of pores open at both ends - This field is not available for the BJH Desorption Report Options window.
Page 145: Tabular Report Options
ASAP 2460 Operator’s Manual Report Options Files Field or Button Description (continued) Pressures button Refer to button, page 3-30. Pressures Cancel button Edit button Refer to Options, page 3-1. Common Fields and Buttons - File Menu OK button Tabular Report Options Highlight BJH Tabular Report in the Selected Reports list box on the BJH Adsorption Report Options window and click Edit to specify the method of data reduction.
Page 146 Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued) Table button The fixed pore size table must contain a minimum of two points. The points must be strictly decreasing. Enabled only when Fixed pore size table is selected.
Page 147: Plot Options
ASAP 2460 Operator’s Manual Report Options Files Plot Options The fields for all plot options are identical for specifying plotting methods and customizing plots. Highlight any plot option in the Selected Reports list box in the BJH Report Options window and click Edit.
Page 148: Dollimore-Heal Adsorption/Desorption Report Options
Report Options Files ASAP 2460 Operator’s Manual Dollimore-Heal Adsorption/Desorption Report Options This report option generates Dollimore-Heal reports from both adsorption and desorption data. In the Selected Reports list box, highlight Dollimore-Heal Adsorption (or Dollimore-Heal Desorption), then click Edit. Dollimore-Heal Adsorption/Desorption fields and buttons are identical to the BJH Adsorption/ Options, page 3-49.
Page 149 ASAP 2460 Operator’s Manual Report Options Files Horvath-Kawazoe Report Options The Horvath-Kawazoe method plots individual peaks for different pore sizes even if the difference between one pore size and the next is only one angstrom (0.10 nm) or less. In the Selected Reports list box, highlight Horvath-Kawazoe, then click Edit.
Page 150 Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued) Properties button Click to view or edit the constants describing the physical properties of the adsorbent and adsorptive. These options are disabled if Entered is selected in the Interaction Parameter group box.
Page 151 ASAP 2460 Operator’s Manual Report Options Files Field or Button Description (continued) Properties button Adsorptive group box: (continued) Contains the parameters for the adsorptives (provided with the software and/or user-defined). If using Computed for the interaction parameter, all fields are enabled. If using Entered, only the values in the Diameter and Diameter at zero energy text fields may be edited.
Page 152: Tabular Report Options
Report Options Files ASAP 2460 Operator’s Manual Tabular Report Options Highlight H-K Tabular Report in the Selected Reports list box in the Horvath-Kawazoe Report Options window and click Edit. Select the data types to include in the report. Column [n] indicates the column order and data contents for the report.
Page 153 ASAP 2460 Operator’s Manual Report Options Files Field or Button Description (continued) • X-Axis - the x-axis field shows pore radius or diameter in angstroms or X-Axis / Y-Axis nanometers. • Y-Axis - the y-axis field shows the quantity of gas adsorbed.
Page 154: Dft Pore Size Report Options
Report Options Files ASAP 2460 Operator’s Manual DFT Pore Size Report Options The DFT Pore Size report contains the results of pore size distribution analyses using a non-local DFT range of micro and mesopore ranges. In the Selected Reports list box, highlight DFT Pore Size, then click Edit.
Page 155 ASAP 2460 Operator’s Manual Report Options Files Field or Button Description (continued)  Select the extent of smoothing to apply to the data. Regularization dropdown list and text box If 0.20000 (user) is selected, enter a number in the text box giving a relative weight for the smoothing during deconvolution.
Page 156: Dft Surface Energy Report Options
Report Options Files ASAP 2460 Operator’s Manual DFT Surface Energy Report Options The DFT Surface Energy report contains the results of surface energy distribution analyses. In the Selected Reports list box, highlight DFT Surface Energy, then click Edit. DFT Surface Energy Report Options fields and buttons are identical to the DFT Pore Size Report Options, page 3-60.
Page 157: Dubinin Report Options
ASAP 2460 Operator’s Manual Report Options Files Dubinin Report Options The Dubinin method provides pore volume distributions for microporous materials by making use of an expression for the adsorption potential. In the Selected Reports list box, highlight Dubinin, then click Edit.
Page 158: Tabular Report Options
Report Options Files ASAP 2460 Operator’s Manual Field or Button Description (continued)  Select the reports to generate. Highlight the report and click the Edit Selected Reports list box button to modify report options. Pressures button Refer to button, page 3-30.
Page 159 ASAP 2460 Operator’s Manual Report Options Files The transformed Dubinin isotherm is the logarithm of quantity adsorbed as a function of the log of rel- ative pressure raised to a power. Isotherms for which the Dubinin method is applicable produce straight lines when transformed in this way.
Page 160: Pore Volume Options
Report Options Files ASAP 2460 Operator’s Manual Pore Volume Options In the Dubinin Report Options window, highlight dV/dw Pore Volume in the Selected Reports list box and click Edit. This option plots differential pore volume as a function of pore width...
Page 161: Mp-Method Report Options
ASAP 2460 Operator’s Manual Report Options Files MP-Method Report Options The MP-Method provides pore volume distributions for microporous materials by correlating quantity adsorbed with the thickness of the adsorbed layer as determined from a user-selected thickness curve. In the Selected Reports list box, highlight MP-Method, then click the Edit button.
Page 162: Tabular Report Options
Report Options Files ASAP 2460 Operator’s Manual Tabular Report Options In the MP-Method Report Options window, highlight MP Tabular Report in the Selected Reports list box and click Edit. Column [n] indicates the column order and data contents for the report.
Page 163: Plot Options
ASAP 2460 Operator’s Manual Report Options Files Plot Options In the MP-Method Report Options window, highlight a plot option in the Selected Reports list box and click Edit to customize the plotting method. Field or Button Description Use to plot a curve and/or points.
Page 164: User-Defined Reports
Report Options Files ASAP 2460 Operator’s Manual User-Defined Reports You may create up to five user-defined reports, each with up to 10 summary reports, 10 tabular reports, and 10 graphical reports. In order to use this feature you must create a file containing a Python script that imports a "mic"...
Page 165 ASAP 2460 Operator’s Manual Report Options Files Click User-Defined, then click Edit. The User-Defined Report Options window is displayed. Field or Button Description User Report 1 through Use the dropdown lists to select currently-defined functions used to define the report calculations and output.
Page 166: Options Report
Report Options Files ASAP 2460 Operator’s Manual Options Report The Options report lists the conditions used to perform the analysis. It contains analysis information including: • Degas conditions • Adsorptive properties • Analysis conditions • Free space • Saturation pressure ( p ) and temperature •...
Page 167: Unit Menu
ASAP 2460 Operator’s Manual Introduction 4. UNIT MENU Introduction This chapter contains information specific to the Unit menu options. These options are used to run analyses on one or more units attached to a controlling computer. This chapter provides details of Unit menu options, and descriptions of commonly used functions and buttons.
Page 168: Common Fields And Buttons - Unit Menu Options
Common Fields and Buttons - Unit Menu Options ASAP 2460 Operator’s Manual Common Fields and Buttons - Unit Menu Options The following fields and buttons are common to many of the Unit menu options. References are made to these fields and buttons throughout this manual.
Page 169 ASAP 2460 Operator’s Manual Common Fields and Buttons - Unit Menu Options Field or Button Description (continued)  Mass group box • Calculate - enables the Empty tube and Sample + tube fields. Enter (continued) the values necessary to calculate the sample mass. Equation used to...
Page 170: Start Analysis
Start Analysis ASAP 2460 Operator’s Manual Field or Button Description (continued)  .REP (Report system) - saves the report in a format that can be opened Report after analysis button ( within any MicroActive program. .TXT (ASCII text) - saves the report as a text file.
Page 171 ASAP 2460 Operator’s Manual Start Analysis Field or Button Description View dropdown list Refer to Common Fields and Buttons - Unit Menu Options, page Browse button Refer to Common Fields and Buttons - Unit Menu Options, page Port button Allows you to select the port to be used for the analysis. Only one port may be selected at a time.
Page 172 Start Analysis ASAP 2460 Operator’s Manual Description (continued) Field or Button Bath temperature text field Enabled if you have chosen to enter the bath temperature ( p T option on the Analysis Conditions dialog). Enter (or confirm) the temperature for the analysis bath.
Page 173 ASAP 2460 Operator’s Manual Start Analysis Use the Skip function with caution; the ASAP 2460 performs multiple steps for a given task. Skipping certain steps may cause corruption of data, instrument damage, or personal injury. Description (continued) Field or Button ...
Page 174: Start Krypton Analysis
Start Krypton Analysis ASAP 2460 Operator’s Manual Start Krypton Analysis When you select this option from the Unit menu, the Krypton Analysis dialog is displayed. Use the following guidelines for performing krypton analyses: • All ports must be idle in order to start an analysis.
Page 175 ASAP 2460 Operator’s Manual Start Krypton Analysis Field or Button Description View dropdown list Refer to Common Fields and Buttons - Unit Menu Options, page Browse button Refer to Common Fields and Buttons - Unit Menu Options, page Ports 1 through 6 Allows you to select the ports to be used for the analysis.
Page 176 Click to skip to the next step. This button is visible only when an analysis is in progress. Select the ports containing the step to skip. Use the Skip function with caution; the ASAP 2460 performs multiple steps for a given task. Skipping certain steps may cause corruption of data, instrument damage, or personal injury.
Page 177 ASAP 2460 Operator’s Manual Start Krypton Analysis Live Graph Settings button Allows you to select Thermal transpiration, X-axis Quantity (relative or absolute pressure) and the X-Axis Scale (linear or logarithmic). Status window Displays the last point pressure and relative pressure for each port with varying numbers of digits after the decimal if 10 mmHg and 0.1 mmHg transducers are present on that port, as follows: P <...
Page 178: Start High Throughput Analysis
Start High Throughput Analysis ASAP 2460 Operator’s Manual Start High Throughput Analysis When you select this option, the High Throughput Analysis dialog is displayed. This dialog enables you to start up to six analyses at the same time. Use the following guidelines for performing high throughput analyses: •...
Page 179: Start Micropore Analysis
ASAP 2460 Operator’s Manual Start Micropore Analysis Start Micropore Analysis When you select this option, the Micropore Analysis dialog is displayed. This dialog enables you to start up to six analyses at the same time. Use the following guidelines for performing micropore analyses: •...
Page 180: Enable Manual Control
Start Micropore Analysis ASAP 2460 Operator’s Manual Enable Manual Control Unit [n] > Enable Manual Control Use to enable the manual control of certain system valves and elevator components. When this option is enabled, a checkmark appears to the left of the menu item.
Page 181 ASAP 2460 Operator’s Manual Start Micropore Analysis • Double-click on the valve or elevator symbol. • Select the valve or elevator symbol and press the Spacebar. System valves and their functions are listed below. Valves Actions: Open, Close, Pulse Pulse briefly opens and closes (or vice versa) the valve.
Page 182 This group of rectangles on the right side of the schematic displays the temperature, the 1000-mmHg and 10-mmHg transducer readings, and the vacuum gauge pressure. The 1000-mmHg transducer is present in all ASAP 2460 systems. The 10-mmHg transducer is shown only on units containing the Krypton or Micropore option.
Page 183: Show Instrument Schematic
Controls must be enabled (Unit [n] > Enable Manual Control). Select this option to display a schematic of the ASAP 2460 analysis system. The schematic is a graph- ical representation of the analysis system including system valves, analysis stations, and dewar positions.
Page 184 Show Instrument Schematic ASAP 2460 Operator’s Manual Four-port Instrument Schematic Six-port Instrument Schematic 4-18 246-42800-01 - Aug 2013...
Page 185: Show Dashboard
ASAP 2460 Operator’s Manual Show Dashboard The state of the valves can be determined quickly by color representation even when manual control is not enabled: Green = open White = closed If you wish to change the state of a valve, you must enable manual control.
Page 186 Show Dashboard ASAP 2460 Operator’s Manual Gauge Description Displays N/M where N is the number of analysis that have Analyses completed/started finished data collection and M is the number of analyses that have been started. Analyses canceled or terminated by errors before the termination stage starts are not counted as completed.
Page 187 ASAP 2460 Operator’s Manual Show Dashboard Gauge Description (continued) Manifold outgas rate (continued) At 60%, the center green LED turns off. At 90%, three green LEDs turn off and the yellow LED is turned on. At 110% and above, only the red LED is lit and attention is required.
Page 188: Show Status
Show Status ASAP 2460 Operator’s Manual Show Status Unit [n] > Show Status Use to show the current status for each port. If there are multiple units attached to the computer. Select Show Status on each unit menu and have the status for all units displayed at one time.
Page 189: Show Instrument Log
ASAP 2460 Operator’s Manual Show Instrument Log Show Instrument Log Unit [n] > Show Instrument Log Use to display a log of recent analyses, calibrations, errors or messages. This information is logged for a 7-day period for analyses and a 30-day period for messages and calibrations.
Page 190 Show Instrument Log ASAP 2460 Operator’s Manual Field or Button Description (continued) Report button Click to display the Instrument Log Report Settings window to specify report output options. • Start Date - click to display a calendar and select the start date for the report.
Page 191: Degas
ASAP 2460 Operator’s Manual Degas Degas If a SmartPrep is not connected to the analyzer, the menu options in this section are disabled. Unit > Degas 246-42800-01 - Aug 2013 4-25...
Page 192: Show Smartprep Status
Degas ASAP 2460 Operator’s Manual Show SmartPrep Status Unit > Degas > Show SmartPrep Status The SmartPrep Status window allows you to monitor the degas operations and stop gas flow after samples are degassed. Field or Button Description Skip button Use to skip the degassing of the selected sample.
Page 193: Start Smartprep Degas
ASAP 2460 Operator’s Manual Degas Start SmartPrep Degas Unit > Degas > Start SmartPrep Degas The six SmartPrep heating stations are represented by row numbers on the Automatic Degas window. Field or Button Description Browse button Use to locate a sample file to degas.
Page 194: Smartprep Configuration
Degas ASAP 2460 Operator’s Manual SmartPrep Configuration Unit > Degas > SmartPrep Configuration Displays the SmartPrep configuration and software versions. ASAP 2460 4-28 246-42800-01 - Aug 2013...
Page 195: Unit Configuration
• Change IP - click to display the Unit IP Setup window. The IP address and Subnet mask assigned during installation display. Do not edit these fields unless instructed by a Micromeritics service representative. • Board ID - click to read the board ID. The parameters on this window cannot be edited.
Page 196 Unit Configuration ASAP 2460 Operator’s Manual Field or Button Description (continued) Calibrations button Displays calibration information for instrument components. 4-30 246-42800-01 - Aug 2013...
Page 197: Show All Readings
ASAP 2460 Operator’s Manual Show All Readings Show All Readings The Show All Readings screen displays the calibrated and nominal readings of all sensors in the system. 246-42800-01 - Aug 2013 4-31...
Page 198: Diagnostics
Diagnostics ASAP 2460 Operator’s Manual Diagnostics This option enables you to perform diagnostic tests which your service representative may request to resolve a problem. The data generated from these tests may be insignificant to you as a user, but are very helpful to your service representative.
Page 199 ASAP 2460 Operator’s Manual Diagnostics Field or Button Description (continued) Test dropdown list Select the diagnostic test to be performed. • Analysis Leak Test Only No Clean • Analysis Inlet Valve Leak Test • Analysis Leak Test with Clean • Leak Test all Manifolds Enter information to identify the person running the service test.
Page 200: Calibration
Calibration ASAP 2460 Operator’s Manual Calibration Unit [n] > Calibrate Analysis Use to perform system calibrations. The options on this menu are not available for normal system operation. They are for use by authorized service test personnel only and are enabled only when the system is in Service Test mode.
Page 201: Load From File
Service Test Unit [n] > Service Test Use for service tests performed only with the assistance of a trained Micromeritics service representa- tive. These tests provide the service representative with troubleshooting tools and readouts. This option is enabled only when the analysis program is operating in Service Test mode. Refer to...
Page 202 Service Test ASAP 2460 Operator’s Manual 4-36 246-42800-01 - Aug 2013...
Page 203: Reports Menu
2460 Operator’s Manual Introduction 5. REPORTS MENU Introduction This chapter contains information specific to the Reports menu options used to customize and run reports. This chapter provides details of Reports menu options, commonly used functions and buttons, field-by-field descriptions, and sample reports. Reports can be generated for data: •...
Page 204 Common Fields and Buttons - Reports Menu Options 2460 Operator’s Manual Field or Button Description (continued)  • File Type - use to save the new file with a .TXT, .XLS or .REP file Destination  group box extension. This field is only enabled when File is selected. (continued) –...
Page 205: Start Report
2460 Operator’s Manual Start Report Start Report Reports > Start Report (or use the F8 keyboard shortcut) Use to generate a report on a sample analysis. Close Reports Reports > Close Reports (or use the F9 keyboard shortcut) Use to close all open report windows. This option is unavailable if reports are being generated. 246-42800-01 - Aug 2013...
Page 206: Open Report
Open Report 2460 Operator’s Manual Open Report Reports > Open Report > [file} Use to open a saved report. 246-42800-01 - Aug 2013...
Page 207: Spc Report Options
2460 Operator’s Manual SPC Report Options SPC Report Options Reports > SPC Report Options Use to generate reports with various SPC (Statistical Process Control) options. All selected variables must be computed for each sample file used in an SPC report; therefore, it is more efficient to select only the necessary variables.
Page 208 SPC Report Options 2460 Operator’s Manual The selected items also appear as options on the Reports > Control Chart screen. (Click the Graph [n] button, then click the Statistic dropdown arrow.) 246-42800-01 - Aug 2013...
Page 209: Regression Report
2460 Operator’s Manual Regression Report Regression Report Reports > Regression Report Use to generate an SPC (Statistical Process Control) Regression report to determine the interdepen- dency between two variables. Up to three dependent variables (y-axis) may be plotted against a single independent variable (x-axis).
Page 210 Do not show me this message again. If Do not show me this message again is selected, the message cannot be redisplayed without Micromeritics’ assistance. The first time this option is used, the time it takes to generate the report is lengthened.
Page 211 2460 Operator’s Manual Regression Report Field or Button Description (continued) Samples button Click to select sample files for report generation. Multiple files can be selected by holding down the Ctrl key on the keyboard while selecting the files. • Available Files - contains files located in the directory specified in the Look In text box.
Page 212: Control Chart
Control Chart 2460 Operator’s Manual Control Chart Reports > Control Chart Use to generate an SPC (Statistical Process Control) control chart report which plots the changes in a statistic. Field or Button Description Show report title text Select and enter a report title to appear on the report header. ...
Page 213 2460 Operator’s Manual Control Chart Field or Button Description (continued)  Select the order in which x-axis statistics are placed. X Axis Order by group box • Time - sorts by the time the files were analyzed. • File name - sorts in alphanumeric order. •...
Page 214 Control Chart 2460 Operator’s Manual Field or Button Description (continued)  Graph [n] buttons • Y-Axis group box - (continued) Statistic dropdown list - displays the SPC variables selected at Reports > SPC Report Options window. The selected variable will be plotted against time.
Page 215: Heat Of Adsorption Report
2460 Operator’s Manual Heat of Adsorption Report Heat of Adsorption Report Reports > Heat of Adsorption Use to select sample files, define quantities and generate a Heat of Adsorption report. The isosteric heat of adsorption is an important parameter for characterizing the surface heterogeneity and for pro- viding information about the adsorbent and the adsorption capacity.
Page 216 Heat of Adsorption Report 2460 Operator’s Manual Field or Button Description (continued)  Click to remove all entries from the table. Clear Samples button  Use to specify the range of surface coverage to include in the report. Edit Quantities button •...
Page 217: Report Features And Shortcuts
2460 Operator’s Manual Report Features and Shortcuts Field or Button Description (continued)  Refer to Report, page 5-7. Tabular report Regression checkbox  Select to generate a graph showing quantities of gas adsorbed versus the Isostere plot temperature. checkbox  Select to generate the Heat of Adsorption data in a graphical format.
Page 218: Report Header
Report Features and Shortcuts 2460 Operator’s Manual Report Header All reports contain a header displaying file statistics. If configured, the report header can also contain a graphic and a title. • Tabular and graphical reports contain sample and instrument statistics such as analysis date / time, analysis conditions, etc.
Page 219: Report Tool Bar
2460 Operator’s Manual Report Features and Shortcuts Report Tool Bar The Report window has a tool bar and selectable tabs across the top of the report header. To view a specific report, select its tab or select the report in the Reports list box and click Show. Reports can be customized and manipulated using the tool bar, shortcut menus, the zoom feature, or axis cross-hairs.
Page 220 Report Features and Shortcuts 2460 Operator’s Manual Field or Button Description (continued) Print button Displays the Print window for report output. • Name dropdown list and Properties button - select the printer and click the Properties button to change printer setup, etc. •...
Page 221 2460 Operator’s Manual Report Features and Shortcuts Field or Button Description (continued) Default Style button Click to specify default report parameters for fonts and curve properties. • Font group box - Font Type list box - allows font type and attributes to be edited for the selected item.
Page 222: Report Shortcut Menus
Report Features and Shortcuts 2460 Operator’s Manual Field or Button Description (continued) Default Style button • Curve group box - (continued) Thickness text box - enter a thickness number for the curve. Histogram Fill dropdown list - select a histogram fill option from the list.
Page 223: Tabular Reports Shortcuts
2460 Operator’s Manual Report Features and Shortcuts Tabular Reports Shortcuts Display tabular report shortcuts by right-clicking in the body of the tabular report. Column shortcuts require right-clicking on the column to be modified. Option Description Right-click on the column to be resized. Select Resize Column on the Resize column shortcut menu and enter the new column width in inches.
Page 224: Graph Shortcuts
Report Features and Shortcuts 2460 Operator’s Manual Option Description (continued) Use to copy the report contents to the clipboard as tab delimited text. It can Copy table as text then be pasted into another document. Graph Shortcuts Display graph report shortcuts by right-clicking in the body of the graph report. Option Description Returns the report to full view after using the zoom feature.
Page 225 2460 Operator’s Manual Report Features and Shortcuts Option Description (continued) Edit curve (continued) • Style dropdown list - use to select another style for the collected data curve. • Curve group box - options are disabled if Histogram is selected in the Style dropdown list.
Page 226 Report Features and Shortcuts 2460 Operator’s Manual Option Description (continued) Use to edit the selected axis properties. Edit axis • Title group box - use to edit the selected axis label. Title text box - use to modify the label of the selected axis. Title font button - use to modify the font for the selected axis label.
Page 227 2460 Operator’s Manual Report Features and Shortcuts Option Description (continued) Use to change the legend location and font. Click Font to modify legend Edit legend fonts. Deselect the Use default font to enable font options. Use to change the graph title and font. Deselect the Use default font to Edit title enable font options.
Page 228: Other On-Screen Features
Report Features and Shortcuts 2460 Operator’s Manual Other On-Screen Features Zoom Feature Use the zoom feature to closer examine graph details. To use this feature: Open the graph. Hold down the left mouse button and drag the cursor across the graphical area to be enlarged. A box will display in the area to be enlarged.
Page 229: Report Examples
2460 Operator’s Manual Report Examples Report Examples This section of the manual contains samples of some of the available reports. Most of the reports can be customized. 246-42800-01 - Aug 2013 5-27...
Page 230: Isotherm Linear Plot
Report Examples 2460 Operator’s Manual Isotherm Linear Plot 5-28 246-42800-01 - Aug 2013...
Page 231: Bet Surface Area Report
2460 Operator’s Manual Report Examples BET Surface Area Report 246-42800-01 - Aug 2013 5-29...
Page 232: Bet Surface Area Plot
Report Examples 2460 Operator’s Manual BET Surface Area Plot 5-30 246-42800-01 - Aug 2013...
Page 233: T-Plot Report
2460 Operator’s Manual Report Examples t-Plot Report 246-42800-01 - Aug 2013 5-31...
Page 234: Bjh Adsorption: Cumulative Pore Volume
Report Examples 2460 Operator’s Manual BJH Adsorption: Cumulative Pore Volume 5-32 246-42800-01 - Aug 2013...
Page 235: Bjh Desorption: Cumulative Pore Volume
2460 Operator’s Manual Report Examples BJH Desorption: Cumulative Pore Volume 246-42800-01 - Aug 2013 5-33...
Page 236 Report Examples 2460 Operator’s Manual 5-34 246-42800-01 - Aug 2013...
Page 237: Options Menu
2460 Operator’s Manual Introduction 6. OPTIONS MENU Introduction This chapter contains information specific to the Options menu selections used to configure the system by setting defaults for sample and parameter files. This chapter contains information on: • changing the default presentation format - Restricted, Basic, or Advanced. •...
Page 238: Default Method
Option Presentation 2460 Operator’s Manual Enter a password, then click OK. In order to switch to either Basic or Advanced when Restricted for- mat is selected, you must enter the same password. Default Method Options > Default Method Use to specify default parameters for sample information files. Manage Libraries Options >...
Page 239 2460 Operator’s Manual Option Presentation To add or remove folders from a library, go to Options > Manage Libraries. Select the library to modify then click the Manage button. To add a folder, click Add to browse and locate a folder. Select the folder and click the Include Folder button.
Page 240: Units
Units 2460 Operator’s Manual Units Options > Units Use to specify how data should appear on the application windows and reports. This menu option is not available if using Restricted format. Graph Grid Lines Options > Graph Grid Lines Use to select how grid lines appear on reports. This menu option is not available if using Restricted format.
Page 241: Service Test Mode
Service Test mode is a password protected option used to perform certain service tests with the assis- tance of a trained Micromeritics service representative. The password is supplied by your service representative. After Service Test Mode has been enabled, the tests are accessible from the Unit menu (Unit >...
Page 242 Service Test Mode 2460 Operator’s Manual 246-42800-01 - Aug 2013...
Page 243: Troubleshooting And Maintenance
Troubleshooting 7. TROUBLESHOOTING AND MAINTENANCE The ASAP 2460 system has been designed to provide efficient and continuous service. However, to get the best results over the longest period of time, certain maintenance procedures must be followed. This chapter includes troubleshooting information, recommended preventive maintenance procedures, and routine maintenance procedures.
Page 244 Troubleshooting ASAP 2460 Operator’s Manual What Happened What To Do Vacuum makes loud Sample tube fitting is loose. Tighten the fitting securely with noise continuously. a wrench. (continued) Sample tube O-ring is worn or Replace the sample tube O-ring. cracked.
Page 245 ASAP 2460 Operator’s Manual Troubleshooting What Happened What To Do Alumina in the oil vapor trap Replace the alumina. Refer to Vacuum gauge shows is holding moisture because reading above 20 Replacing the Alumina in the it was not sufficiently dried Traps, page 7-13.
Page 246: Preventive Maintenance
The table below lists the preventive maintenance procedures you should complete to keep your ana- lyzer operating at peak performance. Instructions for each procedure follow the table. Micromeritics also recommends that you have preventive maintenance procedures and calibration performed by one of our service representatives every 12 months.
Page 247: Checking And Cleaning The Analysis Port Dewars
ASAP 2460 Operator’s Manual Preventive Maintenance Checking and Cleaning the Analysis Port Dewars When handling dewars, be sure to observe the dewar precautions outlined in Dewars, page Filling 3-31 Ice and suspended frost particles may accumulate in the bottom of an analysis port dewar. Particles or deposits exceeding 1/4 in.
Page 248 Preventive Maintenance ASAP 2460 Operator’s Manual Using a wrench, remove the sample tube fitting from the analyzer. Sample tube fitting Remove the filter and O-ring. O-ring Filter Replace the filter and the O-ring. To avoid analysis problems, the new filter and O-ring must be clean. Do not touch them with bare hands.
Page 249: Replacing A Sample Tube O-Ring
ASAP 2460 Operator’s Manual Preventive Maintenance Replacing a Sample Tube O-ring It is important to maintain a vacuum-tight seal near the top of the sample tube stem. If an O-ring becomes worn or cracked, it does not provide a good seal and will need to be replaced. This procedure applies to both degas and analysis ports.
Page 250 Preventive Maintenance ASAP 2460 Operator’s Manual The connector nut contains a ferrule and an O-ring. Remove the O-ring from the top of the sample tube. O-ring Ferrule If the O-ring remains inside the sample port, you may use a pair of tweezers or needle-nose pliers to remove it.
Page 251: Inspecting And Changing Vacuum Pump Fluid
(requiring increased time to reach vacuum levels). The fluid can first be inspected to determine if a change is necessary. Use oil supplied by Micromeritics, or refer to the vacuum pump manual for other acceptable oils. Inspecting Fluid View the vacuum pump fluid through the oil level window.
Page 252: Changing Fluid
Preventive Maintenance ASAP 2460 Operator’s Manual Changing Fluid Always drain the vacuum pump while the pump is warm and disconnected from the power source. Unplug the vacuum pump from the power source. Loosen the wing nut on the clamp at the top of the oil vapor trap. Swing the clamp open and remove the trap from the hose.
Page 253 ASAP 2460 Operator’s Manual Preventive Maintenance Drain the used oil: a.) Place a waste container under the drain spout. b.) Remove the plug from the drain spout. Oil-fill level Drain plug c.) Allow the oil to drain into the waste container.
Page 254 Preventive Maintenance ASAP 2460 Operator’s Manual Insert the oil-fill plug and turn counterclockwise to tighten. If the fluid was badly contaminated (dark brown color), flush the pump with fresh fluid as follows: a.) Cover the top of the oil vapor trap.
Page 255: Replacing The Alumina In The Oil Vapor Traps
ASAP 2460 Operator’s Manual Preventive Maintenance Replacing the Alumina in the Oil Vapor Traps This procedure applies to oil-based vacuum pumps only. Oil vapor trap Alumina The activated alumina in the oil vapor traps becomes saturated during use. The alumina should be replaced if either of the following conditions exist: •...
Page 256 Preventive Maintenance ASAP 2460 Operator’s Manual c.) Bake the alumina for two hours; turn off the oven. d.) Allow the alumina to cool in the oven before pouring it into the traps. Loosen the wing nut on the clamp at the bottom of the oil vapor trap. Swing the clamp open and remove it.
Page 257 ASAP 2460 Operator’s Manual Preventive Maintenance Ensure adequate ventilation when using solvents for cleaning purposes. Screw the end fitting back onto the trap and tighten securely by hand. Insert the O-ring and screw the end fitting back onto the trap and tighten securely by hand.
Page 258: Cleaning The Analyzer
Preventive Maintenance ASAP 2460 Operator’s Manual 10. Reconnect the hose from the analyzer to the oil vapor trap using the clamp and wing nut as described in step 9 above. Tighten clamp to attach trap to hose 11. Plug the pump power cord into the power source.
Page 259: Checking The Analysis Manifold Outgassing Rate
ASAP 2460 Operator’s Manual Preventive Maintenance Checking the Analysis Manifold Outgassing Rate Close the supply valves (Nupro valves) on the gas inlet lines. Insert leak tight plugs in unused gas inlet ports. If the analysis system schematic in manual control mode is not displayed on the computer screen, select Unit >...
Page 260 Preventive Maintenance ASAP 2460 Operator’s Manual Close valves 8 and 18, and record the pressure as the Initial Reading for Inlet Ports in the table below. Test Initial Reading 3 Min. Reading Difference Limits Inlet Ports 30 microns (0.3 mmHg) Valve 21 2.1 microns...
Page 261: Testing The Analyzer For Leaks
ASAP 2460 Operator’s Manual Preventive Maintenance Testing the Analyzer for Leaks Refer to Diagnostics, page 4-32. Replacing the Vacuum Pump Exhaust Filter This procedure applies to oil-based vacuum pumps only. The gases used by the analyzer are exhausted by vacuum pumps. An exhaust filter is installed on the exhaust port of each oil-sealed vacuum pump.
Page 262 Preventive Maintenance ASAP 2460 Operator’s Manual Loosen the wing nut of the clamp at the vacuum pump exhaust port. Swing the clamp away from the exhaust port and remove it. Filter Clamp Wing Nut Exhaust Port Discard the oil filter.
Page 263: Routine Maintenance
ASAP 2460 Operator’s Manual Routine Maintenance Routine Maintenance The procedures in this section are performed as needed. Changing Gases Guidelines for Connecting Gases to the Analyzer Use these guidelines when installing regulators and gas lines: • Ensure that all gases needed are available and near the instrument. If the gas bottles are not located near the instrument, you will have to use gas line extenders, which may degrade gas quality and reduce pressure.
Page 264 Routine Maintenance ASAP 2460 Operator’s Manual Low-pressure gauge High-pressure gauge Gas bottle shut-off valve 1/8-in. copper tubing 1/4-in. to 1/8-in. brass reducer fitting Regulator shut-off/ Pressure isolation valve control knob If the regulator has a 1/8-in. outlet, proceed to the next step. If the regulator has a 1/4-in. outlet, attach the reducer fitting to the outlet of the regulator shut-off/isolation valve and tighten the valve nut with a 9/16-in.
Page 265: Connecting The Gas Delivery Tubing To The Analyzer
ASAP 2460 Operator’s Manual Routine Maintenance d.) Observe the high pressure gauge. If the pressure decreases, tighten the nut connecting the regulator to the gas bottle. If the pressure is stable, proceed to step e. If you are using hazardous gases, make sure the gas supply equipment is adequately vented to prevent purging the regulator and tubing into the lab atmosphere in the following step.
Page 266: Specifying Gas Ports
Routine Maintenance ASAP 2460 Operator’s Manual Specifying Gas Ports When you change the gas attached to a port on the analyzer, you must enter the change in the analysis program as follows. Select Unit [n] > Unit Configuration from the main menu. The Unit Configuration dialog is displayed.
Page 267: Cleaning And Verifying The Gas Line
ASAP 2460 Operator’s Manual Routine Maintenance Cleaning and Verifying the Gas Line Always clean the gas lines and verify there are no leaks at the connections after a gas bottle is con- nected. This test examines the gas line from the instrument to the gas bottle, then from the instrument to the regulator shut-off valve.
Page 268 Routine Maintenance ASAP 2460 Operator’s Manual From the View dropdown list, select either Operation, Instrument Log, or Instrument Schematic. A series of prompts display on the screen when operator response is required. Answer these prompts. A popup window indicates the test is complete. Click OK. The reports display on the screen.
Page 269: Calibrating The System
The instrument was calibrated at the factory. A calibration file was created specifically for your ana- lyzer and included with your accessories. If your system needs recalibration, contact your Micromeritics service representative. The calibration procedures under the Calibrate Analysis com- mand on the Unit menu are accessible by service personnel only.
Page 270 Calibrating the System ASAP 2460 Operator’s Manual 7-28 246-42800-01 - Aug 2013...
Page 271: Ordering Information
ASAP 2460 Operator’s Manual Ordering Information 8. ORDERING INFORMATION The ASAP 2460 system components and accessories can be ordered using one of the following  methods: • Call our Customer Service Department at (770) 662-3636 • Email orders to orders@micromeritics.com •...
Page 272 Ordering Information ASAP 2460 Operator’s Manual Part Number Item and Description 004-25104-00 Ferrule, rear, Nylon 1/4 in. 004-25913-00 Ferrule set, 1/8-in. PEEK, used on gas lines 290-25846-00 Copper tube, for gas inlet, 1/8-in. diameter, 6 ft. 290-25846-01 Copper tube, for gas inlet, 1/8-in. diameter, 16 ft.
Page 273 Activated alumina, 500 grams, for oil vapor trap 004-25652-00 O-ring, size 217, for oil vapor trap Software and Manuals 246-33002-00 Software package, ASAP 2460; includes current version of software and operator’s manual 246-42801-00 ASAP 2460 Operator’s manual 246-42800-01 - Aug 2013...
Page 274: Sample Tubes And Components
Ordering Information ASAP 2460 Operator’s Manual Part Number Item and Description 202-33027-00 MicroActive; includes software and operator’s manual. This program allows you to generate and manipulate data on a computer other than the one controlling the analyzer or to compare data from another...
Page 275 ASAP 2460 Operator’s Manual Ordering Information Part Number Item and Description 004-25044-00 F O-ring, size 013 for 1/2-in. sample tube 260-25843-00 G Ferrule, 1/2 in. 300-25824-00 H Nut, sample tube 004-32604-00 I Cap (stopper), for 1/4-in. sample tube 004-32004-00 J Stopper, for 3/8-in.
Page 276 Ordering Information ASAP 2460 Operator’s Manual 246-42800-01 - Aug 2013...
Page 277: Forms
ASAP 2460 Operator’s Manual Appendix A A. FORMS This appendix contains the following form: • Sample Data Worksheet Copy and use this form as needed. 246-42800-01 - Aug 2013...
Page 279: Sample Data Worksheet
Sample Data Worksheet Use this worksheet to record the values necessary to calculate the sample mass. Sample Tube Identification:_________________________________ Sample Mass (g) NOTE: Record all values in grams. Before Degas After Degas After Analysis ____________ A. Mass for empty sample tube set: ____________ ____________ _____________...
Page 281: Error Messages
The 1000-series error messages, used primarily for software testing, are not included in this appendix. These errors should not occur during normal operation. If a 1000- series message appears, contact a Micromeritics service representative after making backup copies of any files involved in the operation.
Page 282 Several ASAP 2460 files (sample information, analysis conditions, adsorptive properties, or report options) have been added to this direc- tory by some function other than the ASAP 2460 program. to update the directory information with data from each new Action: Select file.
Page 283 ASAP 2460 Operator’s Manual Appendix B 2444- Not a valid file format. 2445- Subset wrote the wrong amount of data. 2446- Error reading data. 2447- Error writing data. Cause: An unexpected error occurred when you tried to access a data file.
Page 284 Appendix B ASAP 2460 Operator’s Manual Action: Wait a few minutes before attempting to exit the application again. 2459- An instrument is busy. A delay in restarting this application could result in loss of new data. Continue with program Exit?
Page 285 ASAP 2460 Operator’s Manual Appendix B 2471- Unit n - S/N; nn has an invalid communications port specified. It cannot be initialized. Cause: The communications port specified for this analyzer during installation (or configuration) is invalid. Action: Use the setup program to change the analyzer configuration.
Page 286 Appendix B ASAP 2460 Operator’s Manual Action A: Run the Setup program and ensure that a valid port is specified; if not, specify a valid one when prompted. Action B: Reinstall the software, then restart application. Action C: Contact your service representative if you continue to get this message.
Page 287 You are attempting to open a file that is currently being used (either by this application or another). Action: Locate the application using the file (in the Micromeritics application, use the Windows menu item to get a list of all windows, one of which may contain this file).
Page 288 The .INI file may have become cor- rupted. The application cannot operate without this file Action: Use the Setup CD to uninstall the ASAP 2460 application. When you uninstall the application, only the application files are deleted; data files remain intact.
Page 289 ASAP 2460 Operator’s Manual Appendix B 2491- Highlighted fields contain errors. Please correct the errors before closing dia- log box. Cause: The highlighted fields contain invalid entries. You will not be able to close the dialog box until you correct the errors.
Page 290: 2500 Series
Appendix B ASAP 2460 Operator’s Manual 2498- The requested change to the Sample’s status is invalid at this time. Cause: A request to change the file’s status (for example, from automatically collected to manually entered) could not be done. Action: Contact your service representative if you continue to receive this error message.
Page 291 ASAP 2460 Operator’s Manual Appendix B Action: Contact your service representative. 2506- Sample file (filename) has "No Analysis" status and cannot be used for this operation. Cause: The action you are trying to perform requires a file with collected data.
Page 292 Calibration operations should only be done by or under the direction of qualified service personnel. 2516- Warning: Keeping a backup copy of the calibration data is recommended by Micromeritics. Would you like to do so now? Cause: You have performed a calibration operation; a backup copy is recom- mended.
Page 293 Cause: The application has discovered a different version of software operat- ing in the analyzer. Action: If there are no analyzers other than the ASAP 2460 connected to the computer, select and allow the updated software to load. 2533- Analyzer initialization failed.
Page 294 If this error persists, contact your service representative. 2551- Cannot access web page (name) (code [n]) Cause: You tried to access Micromeritics on the web and the operating system could not take you there. Action: Make sure you have internet access.
Page 295 ASAP 2460 Operator’s Manual Appendix B Action: If the named directory was accidentally renamed or move, restore the directory. Action: If the file reference is incorrect, remove the file reference. The requested operation cannot be executed. 2558- The instrument is busy.
Page 296 Appendix B ASAP 2460 Operator’s Manual 2563- Cannot write. File or directory (file/directory name) read only. Cause: The referenced file or directory is read-only. You cannot write to this file. Action: Have the administrator of the computer set up proper read/write access to the directories and files.
Page 297: 4000 Series
ASAP 2460 Operator’s Manual Appendix B 4000 Series 4002- Thermal Transpiration correction had no effect. Cause: The Thermal transpiration correction option was selected on the Report Options dialog box. However, the correction did not change any pres- sure by more than one percent.
Page 298 Appendix B ASAP 2460 Operator’s Manual 4012- Psat gas in sample file does not match Psat gas in unit. Cause: You attempted to start an analysis using a sample information file in which the Psat gas does not match the Psat gas entered in the unit con- figuration.
Page 299 ASAP 2460 Operator’s Manual Appendix B 4017- Damage to the instrument will result if the sample has not been manually evac- uated. Have you evacuated the sample? Cause: You did not select Backfill sample at start of analysis on the Sample Backfill Options dialog box.
Page 300 Appendix B ASAP 2460 Operator’s Manual 4022- The entered bath temperature value (Po and Temperature Options of the Anal- ysis Conditions) is outside the range of the temperatures listed in the Psat vs. Temperature Table (Adsorptive Properties). Cause: The Po that corresponds to the entered temperature cannot be found because the entered temperature is outside of the range of values in the Psat vs.
Page 301 ASAP 2460 Operator’s Manual Appendix B 4026- Cannot calculate Dubinin-Astkahov: bad least squares data. Cause: Less than two selected data points are within the fitted pressure range. Action: Edit the calculation assignments on the Collected Data dialog, or change the fitted pressure range on the Dubinin report options dialog.
Page 302 Appendix B ASAP 2460 Operator’s Manual 4031- Not enough points with a relative pressure in the range (n,n) Cause: Fewer than two data points selected for the Dubinin report falls within the selected relative pressure range. Action: Edit the calculation assignments or the fitted relative pressure range.
Page 303 ASAP 2460 Operator’s Manual Appendix B 4036- Fewer than 2 points available for Horvath-Kawazoe calculations. Cause: You must select at least two data points for inclusion in the Horvath- Kawazoe analysis on the Collected Data dialog. No report will be pro- duced.
Page 304 Appendix B ASAP 2460 Operator’s Manual 4039- The isotherm does not meet the constraints of the Cheng/Yang assumption. Cheng/Yang correction will not be applied. Cause: The Cheng/Yang correction to the Horvath-Kawazoe equation requires the value of the monolayer volume as calculated from the Langmuir equation.
Page 305 ASAP 2460 Operator’s Manual Appendix B 4041- Cheng/Yang correction is inappropriate for some P/Po. Cause: The Cheng/Yang correction is usually inappropriate for any P/Po above the isotherm knee. In some instances, the computed pore sizes may decrease above the knee. While it is possible to include these relative pressures (usually above 0.1 P/Po) in the analysis, the computed pore...
Page 306 Appendix B ASAP 2460 Operator’s Manual 4045- Points in the report pressure table lie outside the collected data. Cause: Calculation assignments are not being used and more than one of the report pressure table points is above the range of the collected data, and more than one is below.
Page 307 ASAP 2460 Operator’s Manual Appendix B 4052- Fewer than two points are selected for this report. Cause: At least two points are required for the BET calculations. Action: Edit the calculation assignments for the BET report. 4053- At least two data points must be selected for t-Plot calculations.
Page 308 Appendix B ASAP 2460 Operator’s Manual 4057- At least two data points are needed for Freundlich calculations. Cause: Less than two data points have been selected for the Freundlich report; at least two are required. Action: Select Freundlich points on the Collected Data dialog. If calculation assignments are not being used, edit the Freundlich Report options, Absolute pressure range in the sample file.
Page 309 ASAP 2460 Operator’s Manual Appendix B 4061- The t-curve must contain at least 2 points. Cause: At least two points are required in a thickness curve definition. Action: Edit the thickness curve. 4062- Error during report preparation. Cause: An internal processing error has occurred.
Page 310 Appendix B ASAP 2460 Operator’s Manual 4069- Dosing method choice is invalid. The Analysis Conditions choice of Absolute pressure dosing requires that the Adsorptive Properties (Dosing Method) is set to Normal. Cause: There is an incompatibility between the analysis conditions choice of Absolute pressure dosing and the adsorptive properties dosing method.
Page 311 ASAP 2460 Operator’s Manual Appendix B 4073- The analysis gas (name) does not match the model gas (name). Cause: The model assumes a specific gas and the sample file uses a different one. Action: Select a model that assumes the same gas.
Page 312 Appendix B ASAP 2460 Operator’s Manual 4077- Cannot get surface area for: (file name) Cause: The Isotherm report for the named overlay file has Per gram selected for the Volume Adsorbed, and the Isotherm report for the primary file has a surface area option selected for the Volume Adsorbed.
Page 313: 6100 Series
The instrument (unit number) is not calibrated. Cause: One or more calibration operations have not been performed. Action: If using the setup CD, reinstall the calibration files. If this does not cor- rect the problem, contact your Micromeritics representative. 246-42800-01 - Dec 2013 B-33...
Page 314: 6200 Series
Appendix B ASAP 2460 Operator’s Manual 6200 Series 6204- This sample has an invalid status and cannot be used for degassing. Cause: You tried to degas a sample that has a status other than No Analysis. Action: Select a sample with a status of No Analysis.
Page 315 ASAP 2460 Operator’s Manual Appendix B 6218- SmartVac is not in a valid state to check degas. Cause: You clicked to check degassing but the sample was not in an Check appropriate state. You can only check the degassing operation after the vacuum setpoint has been attained, or during a temperature ramp or hold.
Page 316 Appendix B ASAP 2460 Operator’s Manual 6223- There is no Nitrogen attached to the unit. Cause: A calibration requiring nitrogen was attempted but the software does not recognize that nitrogen is attached. Action: Ensure that a nitrogen gas bottle is installed at one of the analysis ports, then Select Unit >...
Page 317 ASAP 2460 Operator’s Manual Appendix B Action: Select another sample information file. 6230- Dosing method does not match analysis type. Cause: You tried to perform a nitrogen or nitrogen-like analysis with From last port selected as the dosing method. Action: Change the Dosing Method to Normal in the Adsorptive Properties dialog, then start the analysis.
Page 318 Appendix B ASAP 2460 Operator’s Manual 6236- An evacuation cannot be started because all analysis ports are currently in use. Cause: You tried to evacuate one or more analysis ports while all ports are in use. Action: Wait until the current operation completes to evacuate a port.
Page 319 ASAP 2460 Operator’s Manual Appendix B Set the Psat gas regulator to 15 psig (1.03 bar). Then restart the  Action A: analysis. Cause B: The Psat gas bottle is empty. Action B: Connect a new Psat gas bottle. Then restart the analysis.
Page 320 Appendix B ASAP 2460 Operator’s Manual Action: Contact your service representative. 6250- Matching of Sample port transducer failed. Analysis Canceled. Cause: The transducer did not respond correctly. Action: Contact your service representative. 6251- Matching of Psat port transducer failed. Analysis Canceled.
Page 321: 6500 Series
ASAP 2460 Operator’s Manual Appendix B 6500 Series 6510- Main pressure transducer overrange detected. 6511- Sample transducer (number) overrange detected. 6512- Po transducer (number) overrange detected. 6513- Hardware pressure overrange detected. Cause: A manifold pressure over 1000 mmHg was detected by the hardware.
Page 322 Appendix B ASAP 2460 Operator’s Manual Action C: Reduce the amount of sample. 6518- (Unit [number]) Analysis canceled: Pressure of (pressure point) mmHg exceeds the maximum manifold pressure of (pressure point) mmHg. Cause: An absolute pressure greater than (pressure) mmHg was attained that exceeded the specified maximum manifold pressure.
Page 323 ASAP 2460 Operator’s Manual Appendix B Action A: Set the analysis gas regulator to 15 psig (1.0 bar). Then resume the analysis. Cause B: The analysis gas bottle is empty. Connect a new analysis gas bottle. Then resume the analysis.
Page 324 Appendix B ASAP 2460 Operator’s Manual 6524- Analysis suspended: Time limit exceeded while evacuating sample (servo). Cause: The maximum time for evacuating the sample through the restricted valve was exceeded. Possible causes are a leak in the sample tube fit- ting, a crack in the sample tube, or a poorly degassed sample.
Page 325: Calculations
ASAP 2460 Operator’s Manual Appendix C C. CALCULATIONS This appendix contains the calculations used in the analysis program. Saturation Pressure Saturation pressure (Po) is selected on the Po and Temperature Options window. It may be entered or measured in the Po tube. The software uses the following methods to get Po: Po is measured in the Po tube for each isotherm point.
Page 326: Relative Pressure Calculations
Appendix C ASAP 2460 Operator’s Manual Relative Pressure Calculations If Po is measured in the Po tube, the current pressure is measured in the Po tube when each point is taken, and used to calculate relative pressure for that point:...
Page 327: Quantity Adsorbed Calculations
ASAP 2460 Operator’s Manual Appendix C Quantity Adsorbed Calculations For the i dose, the quantity dosed is     n P     – dosed i   dosed i 1 – The pressure, volume, and temperature are those of the dosing manifold before and after expanding into the sample tube.
Page 328: Free Space
Appendix C ASAP 2460 Operator’s Manual Free Space Measured Measured free-space volumes are calculated using the following equations:   T ----------- - ----- - 1 –     ----- -   – --------------------- - bath bath ----------- - –...
Page 329: Calculated
ASAP 2460 Operator’s Manual Appendix C Calculated The calculated free space is determined by subtracting the gas capacity of the volume occupied by the sample from the measured free space of the empty tube.   ----------- - – ...
Page 330 Appendix C ASAP 2460 Operator’s Manual Equilibration Equilibration is reached when the pressure change per equilibration time interval (first derivative) is less than 0.01% of the average pressure during the interval. Both the first derivative and average pres- sure are calculated using the Savitzky-Golay convolution method for polynomial functions.
Page 331: Thermal Transpiration Correction
ASAP 2460 Operator’s Manual Appendix C Thermal Transpiration Correction During data reduction, thermal transpiration correction is applied to the data if the user selected Apply thermal transpiration correction from the Report Options window. Starting with the first collected pressure, the following calculations are performed until the pressure ratio (PC/P) is greater than or equal to 0.99.
Page 332: Bet Surface Area
Appendix C ASAP 2460 Operator’s Manual BET Surface Area For each point designated for surface area calculations, the BET transformation is calculated as: ------------------------------------------ - where B is in units of g/cm STP.  N 1.0 P – ads 1 ...
Page 333: Langmuir Surface Area
ASAP 2460 Operator’s Manual Appendix C Error of the BET Surface Area (m /g):   ---------------------------------------------------------- - Langmuir Surface Area For each point designated for surface area calculations, the Langmuir transformation is calculated as: --------- - where L is in units of g/cm STP.
Page 334: Freundlich Isotherm
Appendix C ASAP 2460 Operator’s Manual Quantity of the Monolayer (cm /g STP): -- - Langmuir b Value: Error of the Langmuir Surface Area (m /g): ----------------------- Freundlich Isotherm The Freundlich isotherm has the form --- - ------- - where...
Page 335: Temkin Isotherm
ASAP 2460 Operator’s Manual Appendix C Temkin Isotherm The Temkin isotherm has the form   ------- - -------- -  where  –  ------- - , where    and a are adjustable constants   equilibrium pressure measured by gauge at temp T...
Page 336: T-Plot
Appendix C ASAP 2460 Operator’s Manual t-Plot A least-squares analysis fit is performed on the (t ) data pairs where t is the independent variable ads, and N is the dependent variable. Only the values of t between t and t...
Page 337: Alpha-S Method
ASAP 2460 Operator’s Manual Appendix C Alpha-S Method The alpha-S curve is calculated from the reference isotherm by dividing each quantity adsorbed by the quantity adsorbed at 0.4 relative pressure. --------- - where Q is found by linear interpolation. A least-squares analysis fit is performed on the (α...
Page 338: F-Ratio Method
Appendix C ASAP 2460 Operator’s Manual f-Ratio Method The f-ratio is the quantity adsorbed divided by the quantity adsorbed in a reference isotherm at the same pressure. ---------------- - The reference quantity adsorbed is found by spline interpolation of the reference isotherm.
Page 339: Explanation Of Terms
ASAP 2460 Operator’s Manual Appendix C Explanation of Terms A pore filled with condensed liquid nitrogen has three zones: a.) The core - evaporates all at once when the critical pressure for that radius is reached; the relationship between the core radius and the critical pressure is defined by the Kelvin equation.
Page 340: Calculations
Appendix C ASAP 2460 Operator’s Manual Calculations The quantities adsorbed (Qa) are converted to the liquid equivalent volumes (Vl, cm /g): ------------------------------------ - 22414cm where V is the liquid molar volume from the fluid property information. The relative pressure (P ) is assumed to be close to unity so that substantially all the pores in the sam- ple are filled.
Page 341 ASAP 2460 Operator’s Manual Appendix C a.) The thickness of the adsorbed layer at the end of the interval is calculated using the equation located in Calculations, page C-44. Thickness Curve For the last pressure interval from the lowest Pr...
Page 342 Appendix C ASAP 2460 Operator’s Manual b.) The physical processes occurring for this pressure interval are determined as: (1.) If Vd is greater than the current increment of volume desorbed (Vl - Vl ), desorption from walls only is occurring. Total surface of walls exposed thus far (cm...
Page 343 ASAP 2460 Operator’s Manual Appendix C All new pores opened in this interval are represented by one pore having a length- weighted average pore diameter and a corresponding length sufficient to account for the required volume of adsorbate. The weighted average pore diameter is calculated ...
Page 344 Appendix C ASAP 2460 Operator’s Manual Pore diameters and radii are adjusted for the change in thickness of the adsorbed wall layer during this interval. If new pores were opened during this interval, the average diameter is adjusted by the change in layer thickness during the second portion of the desorption interval as: 2 Td...
Page 345 ASAP 2460 Operator’s Manual Appendix C (3.) Incremental Surface Area (SA /g): 2 – –   D    LP     --------------- ----------------- -     avg i  Å (4.) Cumulative Surface Area (SA...
Page 346 Appendix C ASAP 2460 Operator’s Manual For fixed pore size tables (if selected), the following calculations are performed: (1.) Average Fixed Pore Size (DF , A): avg,j ----------------------------------- - avg j  calculated for all intervals in the fixed pore size table.
Page 347 ASAP 2460 Operator’s Manual Appendix C (6.) dV/dD pore volume (dV/dDpF , cm /g-A):   --------------- - INTERP DpF dDpF and  where INTERP(x) is the value interpolated from the function X = D avg,j Y = dV/dD (7.) dV/dlog(D) pore volume [dV/dlog(DpF...
Page 348: Compendium Of Variables
Appendix C ASAP 2460 Operator’s Manual Compendium of Variables  thickness of layer desorbed from walls of newly opened pores (Å)  thickness of adsorbed layer desorbed during interval (Å) adsorbate property factor; from the BJH Adsorptive Options window analysis gas molecular cross-sectional area (nm...
Page 349: Dollimore-Heal Adsorption
ASAP 2460 Operator’s Manual Appendix C Dollimore-Heal Adsorption The calculations for the Dollimore-Heal reports are the same as those for BJH, except for the calcula- tion of average pore diameter and pore length. Pore Diameter Pore diameter is determined from the Kelvin radius and thickness equation: ...
Page 350: Horvath-Kawazoe
Appendix C ASAP 2460 Operator’s Manual where ΔV Change in pore volume Pore surface area Summations over the lengths and areas calculated so far p,i,cum i,cum Volume correction factor Density conversion factor Average Kelvin radius Average thickness Horvath-Kawazoe A relative pressure lower limit is determined such that L-d never equals zero.
Page 351: Cylinder Pore Geometry (Saito/Foley
ASAP 2460 Operator’s Manual Appendix C interaction parameter (erg-cm ) from the Horvath-Kawazoe Report Options window Avogadro’s number (6.023 × 10 pore width (nucleus to nucleus) (Å) equilibrium pressure saturation pressure gas constant (8.31441 × 10 erg/mol K) analysis bath temperature (K), from an entered or calculated value on the Po...
Page 352: Sphere Pore Geometry (Cheng/Yang
Appendix C ASAP 2460 Operator’s Manual equilibrium pressure saturation pressure gas constant (8.31441 × 10 erg/mol K) -- - radius of the cylindrical pore, analysis bath temperature (K), from an entered or calculated value on the Po and Temperature Options window...
Page 353: Cheng/Yang Correction
ASAP 2460 Operator’s Manual Appendix C ------------------ - ------------------ - –     – ------------------ - ------------------ - –     – ------------------ - ------------------ - –     – ------------------ - ------------------ - –...
Page 354: Interaction Parameter
Appendix C ASAP 2460 Operator’s Manual Interaction Parameter The interaction parameter (IP) results from the following calculations: The Kirkwood-Muller dispersion coefficients ------------------------- -   ----- - ------ -     --------------------------- where  polarizability of gas molecule (cm ...
Page 355: Additional Calculations
ASAP 2460 Operator’s Manual Appendix C Additional Calculations Based on the previous calculations, the following can be calculated: Adjusted Pore Width (Å): (Shell to Shell) – Cumulative Pore Volume (cm /g): ------------------------------------ - cum i  22414cm where liquid molar volume from the fluid property information dV/dD Pore Volume (cm /g-Å):...
Page 356: Interaction Parameter Components
Appendix C ASAP 2460 Operator’s Manual Interaction Parameter Components Table C-1. Interaction Parameters Interaction Bath Parameter Sample Type Temperature Calculated Value* Argon 87.3 Carbon (Ross/Olivier value) 2.61 Carbon (Horvath/Kawazoe value) 5.89 Zeolite 3.19 Carbon 298.15 Carbon (Ross/Olivier value) 4.20 Dioxide Carbon (Horvath/Kawazoe value) 9.20...
Page 357 ASAP 2460 Operator’s Manual Appendix C The following values were used to calculate the values in Table C-1. Carbon-Graphite Zeolite 3.40 3.04 = 3.845 × 10 3.75 × 10   = 1.05 × 10 (Ross/Olivier) 1.94 × 10 ...
Page 358: Dft (Density Functional Theory
Appendix C ASAP 2460 Operator’s Manual DFT (Density Functional Theory) The adsorption isotherm is known to convey a great deal of information about the energetic heteroge- neity and geometric topology of the sample under study. The data of physical adsorption have been used for many years as the basis for methods to characterize the surface area and porosity of adsor- bents.
Page 359: Application To Surface Energy Distribution
ASAP 2460 Operator’s Manual Appendix C Application to Surface Energy Distribution Under certain conditions, an energetically heterogeneous surface may be characterized by a distribu- tion of adsorptive energies. The conditions are that the sample is not microporous, i.e., that adsorption is taking place on essentially a free surface with no pore filling processes at least to about 0.2 relative...
Page 360: Performing The Deconvolution
Appendix C ASAP 2460 Operator’s Manual Performing the Deconvolution The integrations in equations (2) and (3) are carried out over all surface energies or pore sizes in the model. The functions q(p,) and q(p,H), which we call the kernel functions, are contained in numeric form as model isotherms.
Page 361: Dubinin-Radushkevich
ASAP 2460 Operator’s Manual Appendix C Dubinin-Radushkevich The Dubinin-Radushkevich equation is:     ---------  – ------ -  where:  the affinity coefficient of analysis gas relative to Po gas (for this application  is taken to be 1)
Page 362: Dubinin-Astakhov
Appendix C ASAP 2460 Operator’s Manual Error of Monolayer Capacity (cm /g STP):  YI err   –  0 err Micropore surface area (m /g): Q    6.023 --------------------------------------------------------    ---------------------- -  22414 cm ...
Page 363 ASAP 2460 Operator’s Manual Appendix C For each point designated for Dubinin-Astakhov calculations, the following calculations are done:   ------ - A least-squares fit is performed on the (LP,LV) designated pairs where LP is the independent variable and LV is the dependent variable. If the user selected Yes for the Optimize Astakhov Exponent prompt, a systematic search for the optimum value of N is conducted by recalculating the linear regres- sion and selecting the value of N that gives the smallest standard error of the y-intercept.
Page 364 Appendix C ASAP 2460 Operator’s Manual Limiting Micropore Volume (cm /g): ------------------------------------ 22414cm where liquid molar volume from the fluid property information Error of Limiting Micropore Volume (cm /g):   10YI –  0 err Characteristic Energy (KJ/mol): ...
Page 365 ASAP 2460 Operator’s Manual Appendix C Mean Equivalent Pore Width (Å):   Å  ---------------------------------- -  E   ---------------------------------------------- mean    --------------- -   Micropore surface area (m /g):     ...
Page 366: Mp-Method
Appendix C ASAP 2460 Operator’s Manual dV/dD Pore Volume (cm /g-Å):       – –   Å Å     -------- -   ---------------------------------- - -----  ------------------------------- - -----  ...
Page 367 ASAP 2460 Operator’s Manual Appendix C dA/dR pore surface area for the i point (m /g-Å): ------- - ------------------ - – – Incremental pore volume occluded for the i point (cm /g): 4 –  inc i  inc i ...
Page 368: Thickness Curve Calculations
Appendix C ASAP 2460 Operator’s Manual Thickness Curve Calculations For each point designated, the following parameters are used in thickness curve calculations: parameter #1 parameter #2 parameter #3 relative pressure for the i point (mmHg) rel,i thickness for i point Kruk-Jaroniec-Sayari ...
Page 369: Spc Report Variables
ASAP 2460 Operator’s Manual Appendix C SPC Report Variables Regression Chart Variables The line of best fit for the Regression Chart is calculated by the usual Least Squares method. (Refer to BASIC Scientific Subroutines Vol II, by F.R. Ruckdeschel, Copyright 1981 BYTE Publications/ McGraw Hill, p.
Page 370: Control Chart Variables
Appendix C ASAP 2460 Operator’s Manual Control Chart Variables  y --------- Mean =  y Mean   – ----------------------------------- - StdDev = – StdDev ------------------- CoefVar = Mean  Mean n StdDev PlusNSig =  Mean n StdDev –...
Page 371 ASAP 2460 Operator’s Manual Appendix C e.) t-Plot External Surface Area See t-Plot calculations f.) BJH Cumulative Adsorption g.) BJH Cumulative Desorption h.) Adsorption Total Pore Volume i.) Desorption Total Pore Volume j.) t-Plot Micropore Pore Volume See t-Plot calculations k.) Freundlich...
Page 372 Appendix C ASAP 2460 Operator’s Manual q.) Dubinin-Astakhov Micropore Volume See Dubinin-Astakhov calculations r.) Dubinin-Radushkevich Micropore Surface Area See Dubinin-Radushkevich calculations s.) Dubinin-Radushkevich Monolayer Capacity See Dubinin-Radushkevich calculations t.) MP-Method Cumulative Surface Area of Pores , (see MP-method Calculations) for the last collected data point used in the MP-...
Page 373: References
ASAP 2460 Operator’s Manual Appendix C References Savitzky, A. and Golay, M.J.E., Anal. Chem. 36, 1627 (1964). Brunauer, S.; Emmett, P.H.; and Teller, E., J. Am. Chem. Soc. 60, 309 (1938). Langmuir, I., J. Am. Chem. Soc. 38, 2267 (1916); J. Am. Chem. Soc. 40, 1361 (1918); Phys. Rev 8, 149 (1916).
Page 374 Appendix C ASAP 2460 Operator’s Manual C-50 246-42800-01 - Aug 2013...
Page 375: Free Space Correction
ASAP 2460 Operator’s Manual Appendix D D. FREE SPACE CORRECTION Free space is that volume of the sample tube which is unoccupied by the sample. The quantity of gas dosed into the sample tube is calculated from the difference in pressures in the manifold before and after the dose is delivered.
Page 376: Enter
Appendix D ASAP 2460 Operator’s Manual • Helium is unavailable; free space determination by the application software requires the use of helium • Analysis speed is a major factor; a helium free space measurement of 10 to 15 minutes is required •...
Page 377: Maintaining High Purity Gases
Micromeritics offers the following suggestions to assist you in maintaining high purity gases (particu- larly helium) for the instrument.
Page 378: Purge Method
Apendix E ASAP 2460 Operator’s Manual Purge Method This is the preferred method for removing trapped air. Go to Unit > Enable Manual Control (if the instrument schematic is not displayed, select Show Instrument Schematic). If multiple instruments are installed, make sure to choose the correct Unit menu.
Page 379: Evacuation Method
ASAP 2460 Operator’s Manual Appendix E Open the gas bottle valve briefly and allow the regulator to be charged with gas until the high- pressure gauge reads just over half the tank pressure; then quickly close the valve High-Pressure gauge...
Page 380 Apendix E ASAP 2460 Operator’s Manual If... Then... (continued) The regulator is filled with Close the gas bottle valve. gas: Open the regulator Shut-off valve. Loosen the helium inlet fitting (or nut) on the rear panel of the instrument. Allow all of the gas in the regulator to expel from the line (pressure reading will be zero).
Page 381: Dft Models
ASAP 2460 Operator’s Manual Appendix F F. DFT MODELS Theories are developed by scientists in an attempt to explain a class of observed behavior. In the exper- imental physical sciences, theories are often expressed in terms of a model that can be visualized and described mathematically.
Page 382: Molecular Simulation Methods
Appendix F ASAP 2460 Operator’s Manual If the equilibrium distribution of the gas atoms near the surface could be described as a function of pressure and the molecular properties of the components of the system, then a model could be con- structed for the adsorption isotherm for the system.
Page 383: Density Functional Formulation
ASAP 2460 Operator’s Manual Appendix F If the move results in a configuration of higher energy, a probability for that event is calculated, and a random number between zero and one is generated. If the generated number is smaller than the proba- bility of the event, then the move is accepted;...
Page 384 Appendix F ASAP 2460 Operator’s Manual Figure D-1. Density Profile for Argon on Carbon at 87.3 K and a Relative Pressure of 0.5 This figure represents a cross-section of the region near the surface. Note the layerwise distribution of adsorbate; the first monolayer is sharply defined and a third layer can be distinguished. The area under the profile curve represents the amount adsorbed per unit area at this pressure.
Page 385 ASAP 2460 Operator’s Manual Appendix F Figure D-2. Model Isotherm for Argon at 87.3 K in a 40 Å Slit in a Carbon Substrate The profiles show the density distribution from one wall to the center of the slit; the other half of the distribution is a mirror image of the profile shown.
Page 386 Appendix F ASAP 2460 Operator’s Manual Figure D-3. Model Isotherms for Some Larger Pore Widths Argon on Carbon at 87.3 K Figure D-4 shows model isotherms for pores in the micropore size range. Note the logarithmic scale for pressure. Figure D-4. Model Isotherms in the Micropore Size Range of Pore Width Argon on Carbon at 87.3 K...
Page 387: Models Included
ASAP 2460 Operator’s Manual Appendix F Pores of 4 Å width, barely larger than the argon atom (3.38 Å), fill at pressures below 1 millitorr. Pores below 15 Å fill before a monolayer is completed on the surface of the larger pores. In the micropore size range, the pore volume fills more gradually with pressure and the total shape of the isotherm is important in characterizing the pore size.
Page 388 Appendix F ASAP 2460 Operator’s Manual N2 - Cylindrical Pores - Oxide Surface AR - Cylindrical Pores - Oxide Surface Cylinder Geometry Oxide Substrate Porosity Category: Nitrogen at 77 K; Argon at 87 K Method: Model isotherms were calculated using a combination of statistical mechanical calculations and exper- imental observations for macroporous silicas and MCM-41 mesoporous silicas as well as zeolites.
Page 389 ASAP 2460 Operator’s Manual Appendix F Mietec Jaroniec, Michal Kruk, James P. Olivier and Stefan Koch, “A References: New Method for the Characterization of Mesoporous Silicas,” Proceedings of COPS-V, 1999, Studies in Surface Science, Vol 128, Characterization of porous Solids V , Unger, et al, Eds, Elsevier, Amsterdam, 2000.
Page 390 Appendix F ASAP 2460 Operator’s Manual Oxide Substrate Porosity Category: Nitrogen at 77 K Method: Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting functions and a cylindrical pore geometry. The wall potential used is k = 30 K, typical for a silica or alumina surface.
Page 391 ASAP 2460 Operator’s Manual Appendix F Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting functions assuming 2D model of finite slit pores having a diameter-to-width aspect ratio of 6. This model is particularly useful for microporous carbon materials. The reported pore size range is from 3.5 to 250 Å.
Page 392 Appendix F ASAP 2460 Operator’s Manual This model is particularly useful for characterizing carbon single-wall nanotubes. The reported pore size range is from 3.5 to 1000 Å. P. Tarazona, Phys. Rev. A 31: 2672 (1985). Reference: Idem, Phys. Rev. A 32: 3148 (1985)....
Page 393: Models Based On Classical Theories
ASAP 2460 Operator’s Manual Appendix F Ar - Zeolites Me-Form by NLDFT Cylinder Geometry Zeolite Substrate Porosity Category: Argon at 77 K Method: Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting functions and cylindrical pore geometry. The pore wall potential is described by the Lennard-Jones potential of interaction between a gas molecule and the oxide surface of an infinitely long cylinder.
Page 394: Models Included
Appendix F ASAP 2460 Operator’s Manual quently leads to inconsistencies when carried to small mesopore sizes. If the thickness curve used is too steep, it finally will predict a larger increment of adsorptive for a given pressure increment than is actually observed;...
Page 395: Kelvin Equation With Harkins And Jura Thickness Curve
ASAP 2460 Operator’s Manual Appendix F Kelvin Equation with Harkins and Jura Thickness Curve N2 - Harkins and Jura Thickness Curve Slit Geometry Average Substrate Porosity Category: Nitrogen at 77 K Method: The kernel function is calculated using the Harkins and Jura equation with standard parameters: 13.99...
Page 396: Kelvin Equation With Broekhoff-De Boer Thickness Curve
Appendix F ASAP 2460 Operator’s Manual Kelvin Equation with Broekhoff-de Boer Thickness Curve N2 - Broekhoff-de Boer Model Slit Geometry Average Substrate Porosity Category: Nitrogen at 77 K Method: The kernel function is calculated using the Broekhoff-de Boer equation with standard parameters: –...
Page 397: References
“Determination of Pore Size Distribution from Density Functional Theoretic Models of Adsorption and Condensation within Porous Solids,” J.P. Olivier and W.B. Conklin, Micromeritics Instrument Corp; presented at the International Symposium on the Effects of Surface Heterogeneity in Adsorption and Catalysts on Solids, Kazimierz Dolny, Poland (July 1992).
Page 398 Appendix F ASAP 2460 Operator’s Manual F-18 246-42800-01 - Aug 2013...
Page 399 ASAP 2460 Operator’s Manual Appendix G G. "mic" MODULE FOR PYTHON SCRIPTED USER-DEFINED REPORTS The mic Python module allows you to access primary and overlay isotherm data and create graphical, tabular, and summary reports. Graphical reports consist of a single graph with one or more curves on one or two y-axes.
Page 400 Appendix G ASAP 2460 Operator’s Manual TABLE 1: Example Python Script for User-defined Reports (continued) 26. mic.table.addcolumn( "Column 1", Add columns to the table. Note that the column values are strings; this allows arbitrary formatting. ["1", "2.5", "%8.3f" % np.exp(5.0)] ) 28.
Page 401 ASAP 2460 Operator’s Manual Appendix G TABLE 2: Function Reference for mic Python Module (User-defined Reports) mic.isotherm(press_type='rel') Get the primary isotherm data. Keyword arguments: press_type --- the pressure basis; use 'rel' for relative pressure, 'abs' for absolute (default = 'rel') Usage: p, qads, num_ads, warm_fs, cold_fs, mass, desc = mic.isotherm('rel')
Page 402 Appendix G ASAP 2460 Operator’s Manual TABLE 2: Function Reference for mic Python Module (User-defined Reports) (continued) mic.imported_pore_data( import_number = 1 ) Get imported pore data. Keyword arguments: import_number --- the import number (1 through 8) Usage: xdat, ydat, desc = mic.imported_pore_data(1) xdat --- array of pore dimension boundaries (angstroms);...
Page 403 ASAP 2460 Operator’s Manual Appendix G TABLE 2: Function Reference for mic Python Module (User-defined Reports) (continued) mic.graph(title='User Graph', xlabel='X axis', ylabel='Y axis', yylabel='YY axis', xlinear=True, ylinear=True, yylinear=True) Create a new graphical report. Keyword arguments: title --- the graphical report title (default = 'User Graph')
Page 404 Appendix G ASAP 2460 Operator’s Manual TABLE 2: Function Reference for mic Python Module (User-defined Reports) (continued) graphtype --- graph type; (default = 'both') 'curve' or 'c' : curve 'points' or 'p' : points 'both' or 'b' : curve-and-points 'hist' or 'h' : histogram mic.table(title='User Table')
Page 405 ASAP 2460 Operator’s Manual Index INDEX F-12 Argon Cylinder, single-wall nanotube by NLDFT model, Absolute pressure tolerance, 3-20 F-11 Adsorption isotherm, F-1 ASAP 2460 on the web, 1-17 Adsorptive properties file, creating, 2-21 ASAP 2460 system, 1-1 Advanced format Avogadro's...
Page 406 Index ASAP 2460 Operator’s Manual CO2 DFT Model, F-9 Dubinin-Astakhov calculations, C-38 Cold free space, 3-11, 3-24 Dubinin-Radushkevich calculations, C-37 Common fields and buttons for file menu, 3-1 for reports menu, 5-1 for unit menu, 4-2 Elevator, 1-5, 4-15 Complete file...
Page 407 ASAP 2460 Operator’s Manual Index calculations, C-4 physical properties window, 3-56 cold, 3-11, 3-24 report, 3-55 correction, D-1 report calculations, C-26 entered method, D-2 report plot options, 3-58 measured method, D-1 report, tabular options, 3-58 warm, 3-11, 3-24 Slit pore geometry (original HK)
Page 408 Index ASAP 2460 Operator’s Manual MCM-41 materials, F-8 Menu N2 Broekhoff-de Boer model, F-16 bar, 1-15 N2 Broekhoff-de Boer Model model, F-16 structure, 1-15 N2 Carbon Finite Pores, As=12, 2D-NLDFT model, Mesoporous materials, 3-19 F-11 mic Python module, G-1 N2 Carbon Finite Pores, As=6, 2D-NLDFT...
Page 409 ASAP 2460 Operator’s Manual Index inlet, 1-5, 1-8 shortcut menus for, 5-20 connector, 1-7 Statistical Process Control (SPC), 5-5 sample, connector, 1-7 Summary, 3-33 specifying gas, 7-24 tabular, editing, 5-21 Power tool bar, 5-17 connector, 1-9 t-Plot, 3-43 switch, 1-9...
Page 410 Index ASAP 2460 Operator’s Manual Shield, safety, 2-38 Harkins and Jura, 3-44 Shortcut Kruk-Jaroniec-Sayari, 3-44 graphs, 5-22 reference, 3-43 for tabular reports, 5-21 Title properties window, 5-25 keys, 1-11 Tool bar, reports window, 5-17 menu, 1-11 t-Plot report, 3-43 Show all readings...
Page 411 ASAP 2460 Operator’s Manual Index X-axis order by, 5-11 Zeolites H-Form by NLDFT model, F-12 Zeolites Me-Form by NLDFT model, F-13 Zoom feature, 5-26 246-42800-01 - Aug 2013 Index-7...
Page 412 Index ASAP 2460 Operator’s Manual Index-8 246-42800-01 - Aug 2013...
Page 413 ASAP 2460 Operator’s Manual Appendix G SVP. Smart VacPrep Operator Manual Aug 2013 SVP-1...
Page 414 Appendix G ASAP 2460 Operator’s Manual SVP-2 Aug 2013...
Page 415 MART NTELLIGENT ACUUM AMPLE REPARATION YSTEM PERATOR ANUAL Smart VacPrep Operator Manual Nov 2013...
Page 416 Smart VacPrep is a registered trademark of Micromeritics Instrument Corporation. _____________________________________________________________________________________ © Micromeritics Instrument Corporation 2013. All rights reserved. Printed in the U.S.A. The software described in this manual is furnished under a license agreement and may be used or...
Page 417 2. If an instrument or product is found defective during the warranty period, replacement parts may, at the discretion of MICROMERITICS, be sent to be installed by the purchaser, e.g., printed cir- cuit boards, check valves, seals, etc. 3. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs (rotor) and stems, seals and O-rings, ferrules, etc., are excluded from this warranty except for...
Page 418 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 419: Elements Used In This Manual
Elements Used in this Manual LEMENTS SED IN THIS ANUAL The following icons and format may be used throughout this manual to identify notes of importance, warnings, and cautions. NOTE - Notes contain important information pertinent to the subject mat- ter. CAUTION - Cautions contain information to help prevent actions that may damage the analyzer or components.
Page 420 Elements Used in this Manual Field Labels and Screen Titles Labels and Buttons Description Buttons (in the applic- Buttons in the application are represented as bold font weight and blue let- ters. Some examples are: Save, Edit, Replace All, etc. ation) Buttons (on the equip- Buttons on the equipment are represented as bold font and black letters.
Page 421: Contact Us
Contact Us ONTACT Micromeritics Instrument Corporation 4356 Communications Drive Norcross, GA 30093-2901, U.S.A. Phone: (770) 662-3636 Fax: (770) 662-3696 www.Micromeritics.com --------------- U.S. Inquiries U.S. Sales: (770) 662-3633 ussales@micromeritics.com --------------- Quotes, Orders, and Customer Satisfaction Customer Service: (770) 662-3636 orders@micromeritics.com --------------- U.S. Instrument Service Department...
Page 422 Contact Us Smart VacPrep Operator Manual...
Page 423 Table of Contents Warranty Elements Used in this Manual Contact Us 1 About the Smart VacPrep 1 - 1 Specifications for the Smart VacPrep 1 - 3 Set the Voltage for the Smart VacPrep 1 - 4 2 About the Software 2 - 1 Add or Remove a Smart VacPrep 2 - 1...
Page 424 Diagnostic Test Report for Smart VacPrep 5 - 1 Schedule Smart VacPrep Diagnostic Test 5 - 1 6 Maintenance and Troubleshooting 6 - 1 Enable Manual Control for Smart VacPrep 6 - 1 Replace the Smart VacPrep Fuse 6 - 2 Sample Tube Installation on the Smart VacPrep 6 - 2 Oil Based Vacuum Pump...
Page 425: About The Smart Vacprep
1 About the Smart VacPrep BOUT THE MART The Smart VacPrep is an advanced six-port degassing system that utilizes vacuum to degas samples by heating and evacuation. Each of the ports may be operated independently of one another. Samples may be added or removed from degas ports without disturbing the treatment of other samples undergoing preparation.
Page 426 1 About the Smart VacPrep QuickStart menu option and Smart VacPrep panel buttons. Accessed from the Smart VacPrep > menu selection. Provides the option to enter commonly used Unit [n] > QuickStart Degas Conditions degas conditions for each Smart VacPrep port without the need for a sample information file. This option provides three ways to load information into QuickStart Degas Conditions: 1.
Page 427: Specifications For The Smart Vacprep
Specifications for the Smart VacPrep Related Topics See "QuickStart Degas Conditions" on page 3 - 2 See "Start Smart VacPrep Degas" on page 3 - 5 See "Set the Voltage for the Smart VacPrep" on the next page PECIFICATIONS FOR THE MART The Smart VacPrep degasser has been designed and tested to meet the following specifications: Specifications for the Smart VacPrep...
Page 428: Set The Voltage For The Smart Vacprep
1 About the Smart VacPrep ET THE OLTAGE FOR THE MART The Smart VacPrep voltage setting is housed in a compartment adjacent to the power connector on the back of the unit. 1. Use a flat head screwdriver to gently pry open the cover of the compartment. 2.
Page 429: About The Software
If a software update is required for the analyzer to support the Smart VacPrep, the software can be downloaded from the internet at this location: www.micromeritics.com/Smart-VacPrep-Software.aspx The degasser software is installed as a part of the analyzer installation. During installation, an IP address will be assigned to the unit allowing the unit to connect automatically during startup.
Page 430: Add A Smart Vacprep Unit
2 About the Software DD A MART REP UNIT Smart VacPrep > Add 1. When prompted, enter the serial number of the unit being added. Duplicate serial numbers are not allowed. 2. Click Add. Initialization begins. EMOVE A MART REP UNIT Smart VacPrep > Remove 1.
Page 431: Smart Vacprep Configuration
Click to display the Unit IP Setup window. The IP address and Subnet Change IP mask assigned during installation display. Do not edit these fields unless instructed by a Micromeritics service representative. Saves and closes the active window. Remove 067 Unit Click to remove the selected Smart VacPrep unit.
Page 432 2 About the Software 2 - 4 Smart VacPrep Operator Manual...
Page 433: Operate The Smart Vacprep
3 Operate the Smart VacPrep PERATE THE MART ACKFILL THE MART ORTS Smart VacPrep > Unit [n] > Backfill Ports Use to backfill ports with gas. 1. Enter the backfill pressure in the Backfill pressure field. 2. Select the ports to be backfilled. 3.
Page 434 3 Operate the Smart VacPrep Smart VacPrep Evacuate Ports Fields and Buttons Field or Button Description Cancel Discards any changes or cancels the current process. Evacuate Options Unrestricted evac. pressure. Pressure value at which unrestricted sample evacuation should begin. Vacuum level. Specify the vacuum level to be achieved before evac- uation begins.
Page 435: Quickstart Degas Conditions
QuickStart Degas Conditions 1. Go to Smart VacPrep > Unit [n] > QuickStart Degas Conditions 2. The six ports are represented by row numbers. Ports that are busy are grayed out and disabled. Edit Click for the port to be configured. 3. Enter degas conditions using one of the following methods: To select degas conditions from a Degas Conditions file, click the dropdown arrow to the right of the Degas Conditions field.
Page 436: Load Quickstart Degas Conditions Into A Sample File
3 Operate the Smart VacPrep 10. Install the safety shield. 11. Press the Select button for the port to be degassed. A blue LED is lit. 12. Press the Start button on the Smart VacPrep panel to start the degas process for all ports that have a blue LED lit.
Page 437: Start Smart Vacprep Degas
Start Smart VacPrep Degas Degas Conditions Fields and Buttons Table (continued) Field or Button Description Save Saves changes to the active window. This option is applicable only when degassing with a Smart VacPrep. Smart VacPrep Evac- uation Backfill sample tube. Indicate if the sample tube should be backfilled automatically or wait for operator response.
Page 438 3 Operate the Smart VacPrep Degas conditions remain the same from degas to degas unless the Degas Conditions file is changed or replaced by the operator. A manual evacuation can be performed on any idle degas port. The six ports are represented by row numbers. Ports that are busy are grayed out and disabled. 1.
Page 439: Show Smart Vacprep Dashboard
Show Smart VacPrep Dashboard Degas ports can also be canceled using buttons on the Smart VacPrep unit. Press on the unit to select the port, then press the but- Select Cancel ton. MART ASHBOARD Smart VacPrep > Unit [n[ > Show Dashboard The dashboard displays the following: Number of days until roughing pump maintenance is due Manifold outgas rate Data for the dashboard comes from the logged diagnostic data.
Page 440: Show Smart Vacprep Log
3 Operate the Smart VacPrep Smart VacPrep Dashboard Gauges and Descriptions Table (continued) Field or Button Description Three green LEDs are lit if outgas rate is below 30% of outgas rate limit. At 30%, the left LED turns off. At 60%, the center LED turns off. At 90%, three green LED lights turn off and the center yellow LED is turned on.
Page 441: Show Smart Vacprep Schematic
Show Smart VacPrep Schematic Analyzer Log Fields and Buttons Table (continued) Field Description Start Date. Displays a calendar to select the start date for the report. Preview. Previews the predefined report on the screen. Print. Sends the report to the default printer. Copies.
Page 442: Smart Vacprep Schematic Shortcut Menus
3 Operate the Smart VacPrep Smart VacPrep Schematic Components Table Schematic Description Components Sample port valves 7, 8, 9 Vacuum and backfill valves Heating mantle con- Sets the ramp rate and target temperature trols MART CHEMATIC HORTCUT ENUS Each manually controlled schematic component has a shortcut menu displaying the operations available for that particular component.
Page 443: Show Smart Vacprep Status
Show Smart VacPrep Status Smart VacPrep Schematic Shortcuts Table (continued) Schematic Shortcut Icon Available Options: Cool the sample to less than 50 °C Set heater power percent MART TATUS Smart VacPrep > Unit [n] > Show Status The Smart VacPrep Status window allows the monitoring of degas operations for a manual degas operation.
Page 444 3 Operate the Smart VacPrep Smart VacPrep Status Fields and Buttons Table (continued) Field or Button Description Sample The name of the sample file. Skip Skips the current degas operation. Status Indicates the current status of the degas. 3 - 12 Smart VacPrep Operator Manual...
Page 445: Smart Vacprep Calibration
Smart VacPrep > Unit [n] > Calibration > Pressure Offset Use to perform system calibration. This option evacuates the system and zeros the pressure transducer. Disabled calibration options can be accessed only with the assistance of an authorized Micromeritics service representative. Start Click to begin the process.
Page 446: Smart Vacprep Servo Valve Calibration
4 Smart VacPrep Calibration MART ERVO ALVE ALIBRATION Smart VacPrep > Unit [n] > Calibration > Servo Valve Use to calibrate the servo valve to the manifold pressure transducer. The servo valve should always be recalibrated after a pressure calibration has been performed. The pressure transducer should be calibrated before starting this calibration procedure.
Page 447: Smart Vacprep Diagnostics
5 Smart VacPrep Diagnostics MART IAGNOSTICS IAGNOSTIC EPORT FOR MART Smart VacPrep > Unit [n] > Diagnostics > Diagnostic Test Report Displays previously run diagnostic tests. Separate directories store tests run once, daily, weekly, and monthly. CHEDULE MART IAGNOSTIC Smart VacPrep > Unit [n] > Diagnostics > Schedule Diagnostic Tests Allows the specification of one-time or periodic running of a sequence of diagnostic tests.
Page 448 5 Smart VacPrep Diagnostics Schedule Diagnostics Fields and Buttons Table Field or Button Description Available Tests drop- Select one or more tests to run unattended. Select the test and click the down list Insert button for the test to display in the Test Sequence box. Cancel Discards any changes or cancels the current process.
Page 449 6 Maintenance and Troubleshooting AINTENANCE AND ROUBLESHOOTING NABLE ANUAL ONTROL FOR MART Smart VacPrep > Unit [n] > Enable Manual Control Use to enable the manual control of certain system valves and elevator components. When this option is enabled, a checkmark appears to the left of Unit [n] >...
Page 450 6 Maintenance and Troubleshooting Smart VacPrep Schematic Components Icon Table (continued) Field or Button Description Servo Valve. Open. Sample Tube. Cannot be manually controlled. EPLACE THE MART The Smart VacPrep uses two 5 amp fuses located in a compartment adjacent to the power connector on the back of the unit.
Page 451 Oil Based Vacuum Pump 3. If using a Check Seal, verify that the Check Seal opener is installed in the sample port. 4. To attach the sample tube set to the degas port, push the sample tube in to a full stop. Secure the sample tube in place by sliding the connector nut, ferrule, and O-ring up onto the degas port and turning the connector nut clockwise.
Page 452 Drain the oil while the pump is warm and disconnected from the power source. Use oil supplied by Micromeritics or refer to the vacuum pump manual for other acceptable oils. 1. Unplug the vacuum pump from the power source. 2. Loosen the wing nut on the clamp at the top of the oil vapor trap. Swing the clamp open and remove the trap from the hose.
Page 453 Inspect and Change Vacuum Pump Oil 3. Grasp the handle on top of the vacuum pump and place the pump on a work surface. 4. Place a waste container under the drain spout. 5. Remove the drain plug and drain the oil into the waste container. 6.
Page 454 6 Maintenance and Troubleshooting Do not allow oil to rise above the midway position when the pump is run- ning. Doing so may cause oil to splash into the oil filter causing con- tamination. 7. Check the washer or O-ring used at the oil-filling port and replace if necessary. 8.
Page 455 Replace the Alumina in the Oil Vapor Trap EPLACE THE LUMINA IN THE APOR The equipment shown in this section may differ slightly from yours. However, the process is the same unless otherwise noted. The activated alumina in the oil vapor trap becomes saturated during use. The alumina should be inspected periodically and replaced when most of the alumina pellets are no longer white.
Page 456 6 Maintenance and Troubleshooting 4. Remove one end fitting from the trap body and dispose of the used alumina in an appropriate manner. 5. Wash the trap body with a detergent-based soap. Rinse with water, then rinse with isopropyl or ethyl alcohol.
Page 457 Replace the Alumina in the Oil Vapor Trap 6. Inspect the O-rings. If dusty, clean with a lint-free tissue. If damaged, replace with a new O-ring. 7. Screw one of the end fittings onto the trap body. 8. Ensure the trap body is dry and the alumina is lukewarm. Pour the alumina pellets into the trap until level with the top of the trap body.
Page 458: Maintenance And Troubleshooting
6 Maintenance and Troubleshooting rings. Use the one with the smaller opening at the intake port. 12. Place the centering ring on the intake port. 13. Place the trap on the centering ring. 14. Open the clamp and place it around the flange of the intake port and the flange of the trap. Swing the clamp fastening screw toward the intake port until it fits into the slot in the other half of the clamp.
Page 459: Replace The Vacuum Pump Exhaust Filter
Replace the Vacuum Pump Exhaust Filter 16. Plug the pump power cord into the power source. Allow the pump to run a few hours (overnight if possible) to eliminate air and moisture from the fresh oil and to produce efficient vacuum operations.
Page 460 6 Maintenance and Troubleshooting 3. Remove and discard the exhaust filter. Ensure the centering ring remains in place on the exhaust port. 4. Place the new filter on the centering ring. 5. Open the clamp and place it around the exhaust port flange and the exhaust filter flange. Swing the clamp fastening screw toward the exhaust port until it fits into the slot in the other half of the clamp.
Page 461: Parts And Accessories For The Smart Vacprep
7 Parts and Accessories for the Smart VacPrep ARTS AND CCESSORIES FOR THE MART Part Number Item and Description Cables 003-63801-01 Cable, Ethernet straight-thru; for connecting instrument to control module (computer) Gas Cylinder Accessories 004-25549-00 Reducer, 1/8 in tube × 1/4 in tube 004-33601-00 Expansion kit;...
Page 462 7 Parts and Accessories for the Smart VacPrep Part Number Item and Description Option kit, 9 mm ferrules and O-rings (6 ferrules and 12 O-rings) 067-33605-00 260-25843-00 Sample tube ferrule, 1/2 in 300-25824-00 Sample tube nut 300-25825-00 Sample tube ferrule, 1/4 in 300-25826-00 Sample tube ferrule, 3/8 in Smart VacPrep Systems...
Page 463: Error Messages
RROR ESSAGES Program error messages are listed numerically. If the Action response indicates to contact a Micromeritics service representative, record the error message, then make backup copies of any files involved in the operation. 4407 Error searching for installed Smart VacPreps. The registry could not be read..
Page 464 Cause: The temperature of the indicated mantle exceeded the maximum allowed value. Action: Ensure the power and thermocouple connectors for the mantle are properly installed. If they are, the mantle may be defective; contact your Micromeritics service rep- resentative. 4414 Error thermocouple unplugged on port [0].
Page 465 8 Error Messages 4422 The file %s does not exist. Cause: The selected file does not exist on the disk drive. Action: Select an existing file. Ensure that the file has been created before use. 4423 The sample %s is already selected on port %d. Cause: The selected sample file is already selected for use on a different port.
Page 466 8 Error Messages 8 - 4 Smart VacPrep Operator Manual...
Page 467 Index NDEX Fuses replace on the Smart VacPrep 6 - 2 Backfill port, Smart VacPrep 3 - 1 Heating phase table, degas conditions 3 - 4 Calibration Smart VacPrep 4 - 1 Smart VacPrep, pressure offset 4 - 1 Smart VacPrep, servo valve 4 - 2 Mainteane Configuration fuse replacement on the Smart VacPrep 6 -...
Page 468: Index Index
Index backfill ports 3 - 1 calibrate servo valve 4 - 2 calibrate, pressure offset 4 - 1 calibration 4 - 1 configuration 2 - 3 diagnostic test report 5 - 1 Diagnostics 5 - 1 evacuate ports 3 - 1 install additional unit 2 - 1 install sample tube 6 - 2 Parts and accessories 7 - 1...

Micromeritics ASAP 2460 Operator's Manual

Section 1

1 Using the Analyzer

2 Operational Procedures

3 File Menu

4 Unit Menu

5 Reports Menu

6 Options Menu

7 Troubleshooting and Maintenance

8 Ordering Information

Forms

Error Messages

Calculations

Free Space Correction

Maintaining High Purity Gases

Dft Models

Section 2

1 About the Smart Vacprep

2 About the Software

3 Operate the Smart Vacprep

4 Smart Vacprep Calibration

5 Smart Vacprep Diagnostics

6 Maintenance and Troubleshooting

7 Parts and Accessories for the Smart Vacprep

8 Error Messages

Index Index

Quick Links

Chapters

Troubleshooting

Need help?

Questions and answers

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Summary of Contents for Micromeritics ASAP 2460