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Micromeritics ASAP 2020 Confirm Operator's Manual

Micromeritics ASAP 2020 Confirm Operator's Manual

Developer/analyst

Table Of Contents

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ASAP 2020 Confirm

Developer/Analyst

Operator's Manual

V4.03

202-42811-01

Apr 2014

Table of Contents

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Do you have a question about the ASAP 2020 Confirm and is the answer not in the manual?

Questions and answers

Dr. Ban AL-Tabbakh

May 5, 2025

The pressure of vacuum pump greater than 5 How can we lower the pressure below 5 during degassing

0

1 comments:

Mr. Anderson

May 18, 2025

To lower the pressure of the Micromeritics 2020 Confirm vacuum pump below 5 during degassing, follow these steps:

1. Use the Degas ASAP option to evacuate the manifold.
2. Calibrate the Pressure Zero to zero the transducer.
3. Use the Calibrate Servo option to calibrate the servo valve to the manifold pressure transducer. The servo valve helps evacuate and equilibrate the manifold.
4. Monitor the pressure during the degassing process. If the pressure exceeds a set value during the temperature ramp, the process will pause until the pressure returns to a safe level.
5. Ensure valves are not leaking by checking the outgassing rate; it should be less than 50 µmHg/min.

These steps help achieve and maintain low pressure during degassing.

This answer is automatically generated

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Summary of Contents for Micromeritics ASAP 2020 Confirm

Page 1 ASAP 2020 Confirm Developer/Analyst Operator’s Manual V4.03 202-42811-01 Apr 2014...
Page 2 Windows is a registered trademark of Microsoft Corporation  Micromeritics Instrument Corporation 2004-2014. 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 2020 Confirm Table of Contents TABLE OF CONTENTS 1. GENERAL INFORMATION Organization of the Operator’s Manual ..........1-1 Conventions .
Page 6 Table of Contents ASAP2020 Confirm Determining the Mass of the Sample ......... . 3-19 Degassing the Sample.
Page 7 ASAP 2020 Confirm Table of Contents MP-Method Report Options..........4-85 Options Report .
Page 8 Table of Contents ASAP2020 Confirm Enable Manual Control........... . . 5-26 Show Instrument Schematic .
Page 9 ASAP 2020 Confirm Table of Contents 8. TROUBLESHOOTING AND MAINTENANCE Troubleshooting ............. . 8-1 Preventive Maintenance .
Page 10 Table of Contents ASAP2020 Confirm Relative Pressure ............. C-1 Free Space.
Page 11 ASAP 2020 Confirm Table of Contents Repairing Valves on the Analysis Manifold ....... . D-8 Replacing Valves on the Degas and Gas Inlet Manifold .
Page 13: General Information
This manual provides a description of the ASAP 2020 analyzer and the menu options and functions available for the ASAP 2020 Confirm program. This manual covers operations for a Developer and an Analyst. A Developer is authorized to perform all functions listed on the menu bar.
Page 14: Conventions
ASAP 2020 Confirm Organization of the Operator’s Manual Chapter 9 ORDERING INFORMATION Provides part numbers and descriptions of the ASAP 2020 System components and accessories. Appendix A FORMS Contains a form to assist you in determining the sample mass. Appendix B ERROR MESSAGES Lists the error messages that may be displayed by the software/hardware;...
Page 15: Equipment Description
Dewar automatically. A removable shield to enclose the Dewar is also included for safety purposes. The ASAP 2020 system includes Micromeritics’ Isothermal Jackets for the sample tube. The Isothermal Jacket maintains a stable thermal profile along the full length of the sample and Psat tubes.
Page 16: Gas Requirements
Micromeritics; refer to ORDERING INFORMATION for ordering information. , page Analysis Program The ASAP 2020 Confirm software is designed to operate in a Windows environment. The Windows environment provides a user-friendly interface for performing analyses and generating reports. Refer to Specifications 1-5.
Page 17: Specifications
Specifications ASAP 2020 Confirm Specifications The ASAP 2020 system has been designed and tested to meet the specifications provided below. Characteristic Specification PRESSURE MEASUREMENT Range: 0 to 950 mmHg Resolution: 1000-mmHg Transducer 0.001 mmHg (Analysis system) 1 mmHg (Degas system) 10-mmHg Transducer* 0.00001 mmHg...
Page 18 ASAP 2020 Confirm Specifications Characteristic Specification DEGAS SYSTEM (optional) Temperature Range: Ambient to 450 ºC Selection: 1 ºC increments Accuracy: Deviation less than 10 ºC of set point at thermocouple Backfill Gas: User-selectable, typically helium or nitrogen Pressure range: 0 to 950 mmHg...
Page 19 Specifications ASAP 2020 Confirm Characteristic Specification ELECTRICAL 100,115, 230 VAC 10% Voltage: Frequency: 50/60 Hz Power: 700 VA, operating ENVIRONMENT Temperature: 10 to 30 ºC operating; -10 to 55 ºC storing or shipping Humidity: 20 to 80% relative, noncondensing GASES...
Page 20 ASAP 2020 Confirm Specifications COMPUTER Minimum requirements: • Pentium 333 MHz computer (or equivalent) • 512 megabytes of main memory • 20-gigabytes hard drive • Ethernet port (capable of communicating with a 10 base- T ethernet card) * • Ethernet switch – required only if running multiple instruments •...
Page 21: User Interface
An Analyst is also allowed to perform other tasks as designated throughout this manual. Tasks not allowed are disabled. This manual is written for the Developer and Analyst levels of the ASAP 2020 Confirm software. Functions for the Administrator level are covered in the Administrator Utility User’s Guide.
Page 22: Front Panel
ASAP 2020 Confirm Controls, Indicators, and Connectors Front Panel Indicator Light Vacuum Pump Panel Elevator Green indicator light Illuminated when power is applied to the analyzer. Vacuum pump panel Allows access to the vacuum pumps. Remove this panel when you need to service the pumps.
Page 23 Controls, Indicators, and Connectors ASAP 2020 Confirm High vacuum pump A high vacuum pump is used when dry evacuation methods are required. Connections, as well as an on/off (breaker) switch, are located on the front right side of the analyzer beneath the work surface.
Page 24 Protects the circuitry for the heating mantle in the event of a breaker failure (one for each heating mantle). If the circuit breaker trips (pops out), call your Micromeritics service representa- tive. Cold Traps Two cold traps are provided; one for degassing and one for analysis.
Page 25: Side Panel
Controls, Indicators, and Connectors ASAP 2020 Confirm Side Panel Upper Chemisorption Ports (available if upgraded to Chemisorption capability) Gas Inlet Ports Degas Port Vapor Gas Port Helium Port Gas inlet ports Used to connect gas supplies to the analyzer. Vapor gas port For attaching the water vapor option, or connecting a vapor gas.
Page 26: Lower
Valve circuit breaker Protects the circuitry for the valves in the event of a failure. If the circuit breaker trips (pops out) and continues to trip after being reset, call your Micromeritics service representa- tive. Voltage selector switch For setting the analyzer to the correct incoming AC line voltage.
Page 27: Rear Panel
Controls, Indicators, and Connectors ASAP 2020 Confirm Rear Panel Vacuum Pump Location Vacuum pump recess Provides for placement of the vacuum pumps; two are required. Vacuum pumps can be serviced from the front of the instrument by removing the vacuum pump panel located on the lower left side of the front panel.
Page 28: Using The Software
Using the Software Using the Software The ASAP 2020 Confirm Program operates in the Windows environment and requires familiarity with standard Windows operations such as using the mouse, menus, and dialog boxes. While this manual provides brief instructions for such standard operations, you may have to refer to your Windows documentation or to its online help system to clarify functions which are specific to Windows.
Page 29: Shortcut Keys
Using the Software ASAP 2020 Confirm Shortcut Keys Shortcut keys can be used to activate some menu commands. Shortcut keys or key combinations (if assigned) are listed to the right of the menu item. Instead of opening the menu and choosing the command, simply press the key combination. For example, to open a sample information file, press ;...
Page 30: Dialog Boxes
ASAP 2020 Confirm Using the Software Dialog Boxes Dialog boxes are displayed when a item followed by an ellipsis (...) is selected. Subdialog boxes are displayed when certain push buttons are selected. Both types of boxes may contain one or more of the items listed below.
Page 31 Using the Software ASAP 2020 Confirm Push Buttons A push button is used to display a subdialog box in which to enter additional information about the subject matter, or to invoke an action. For example, if you click on the Open Sample Infor-...
Page 32: Selecting Files
ASAP 2020 Confirm Using the Software Selecting Files Sample information is stored in files and saved under file descriptions. Certain dialog boxes contain a Files list box which displays a list of files available for that particular operation. For example, the Open Sample Information File dialog box.
Page 33 Using the Software ASAP 2020 Confirm For convenience, the following shortcut keys are available when the Select Dates dialog is displayed: Clears the date Inserts the current date Displays a calendar from which you may select a date • Select a file status from the Status drop-down list. The table shown below describes each file status.
Page 34: Menu Structure
ASAP 2020 Confirm Menu Structure Menu Structure All functions for the ASAP 2020 are located on menus which are accessed from the Menu bar. Each menu contains commands, and in some cases a submenu. A submenu is indicated when the command is followed by an arrow.
Page 35: Windows Menu
Help Menu Operator’s Manual Displays the operator’s manual in PDF format Micromeritics on the Web Connects you to the Micromeritics web site. About ASAP 2020 Confirm Displays information about the ASAP 2020 Confirm pro- gram 202-42811-01 - May 2012 2-15...
Page 36 ASAP 2020 Confirm Menu Structure 2-16 202-42811-01 - May 2012...
Page 37: Operational Procedures
ASAP 2020 Confirm 3. OPERATIONAL PROCEDURES This chapter contains step-by-step procedures for operating the ASAP 2020 Confirm program. It does not provide detailed descriptions of the fields in the dialogs used to perform these procedures. Refer to Chapters 4 through 7 for field descriptions.
Page 38 Save containing the same description currently exists. Edit the description to enable . The Save ASAP 2020 confirm program does not allow duplicate file descriptions. 9. Click on the No Analysis sample file; the following error message is displayed: Close (file name) has been changed.
Page 39: Creating Parameter Files
Having these files exist independently allows you to use them over and over again. Several predefined parameter files are included with the ASAP 2020 Confirm program. Although these files may come close to the needs of your laboratory, you may wish to define additional ones.
Page 40: Degas Conditions
Save Sample Tube file dialog. If is disabled, the description is a duplicate one and must be Save edited. The ASAP 2020 Confirm program does not allow duplicate descriptions. 10. Click to close the dialog box. Close Degas Conditions Degas Conditions files contain degassing information for sample preparation.
Page 41: Analysis Conditions
Save Degas Conditions file dialog. If is disabled, the description is a duplicate one and Save must be edited. The ASAP 2020 Confirm program does not allow duplicate descriptions. 7. Click to close the dialog box. Close Analysis Conditions Analysis conditions specify the data used to guide an analysis.
Page 42 Save Analysis Conditions file dialog. If is disabled, the description is a duplicate one and Save must be edited. The ASAP 2020 Confirm program does not allow duplicate descriptions. 14. Click to close the dialog. Close 202-42811-01 - Mar 2011...
Page 43: Adsorptive Properties
Creating Parameter Files ASAP 2020 Confirm Adsorptive Properties Adsorptive properties provide the adsorptive characteristics for the analysis. 1. Perform the following steps to create an adsorptive properties file: 2. Select New, Adsorptive properties from the File menu; the Create an Adsorptive Properties dialog containing the available templates is displayed.
Page 44: Report Options
Save Adsorptive Properties file dialog. If is disabled, the description is a duplicate one Save and must be edited. The ASAP 2020 confirm program does not allow duplicate descriptions. 13. Click to close the dialog. Close...
Page 45 Creating Parameter Files ASAP 2020 Confirm 2. Choose a template, then click ; the Report Options dialog is displayed: Create 3. Enter a description (up to 42 characters) in the Description field. Enter an identifier that gives a more intuitive description of the files contents. For example, BJH Adsorption Report Options.
Page 46: Creating A Sample File
ASAP 2020 Confirm Creating a Sample File Creating a Sample File A sample information file must be created for each analysis. The sample information file consists of information groups which, collectively, identify the sample, guide the analysis, and specify report options.
Page 47 Choose the directory into which the file is to be saved. b. Ensure that the description is as desired; the ASAP 2020 Confirm program does not allow duplicate descriptions. c. Enter a comment in the Comment window; for example, you may wish to enter the date and time the file is created.
Page 48: Developer
ASAP 2020 Confirm Creating a Sample File Developer A Developer’s view of the sample information dialog is more flexible than that of an Analyst. A Developer is allowed to view and edit (if desired) all parameters of the file. Perform the following steps to create a sample information file: 1.
Page 49 Choose the directory into which the file is to be saved. b. Edit the description; the ASAP 2020 Confirm program does not allow duplicate descriptions. c. Enter a comment in the Comment window; for example, you may wish to enter the date and time the file is created.
Page 50: Preparing Samples
ASAP 2020 Confirm Preparing Samples Preparing Samples Care should be taken in choosing, conditioning, and filling sample tubes. The following guidelines help ensure accurate, reproducible results. Choosing Sample Tubes A sample tube set consists of the following parts: • Sample tube •...
Page 51: Cleaning And Labeling Sample Tubes
Preparing Samples ASAP 2020 Confirm Filler rods help to ensure accuracy in samples with lower total surface areas by reducing the free-space volume. It is generally a good practice to use filler rods for samples having less than 100 square meters of total surface area. Filler rods are unnecessary for samples with total surface areas greater than 100 square meters.
Page 52 ASAP 2020 Confirm Preparing Samples 1. Turn on the drying oven used for heating the sample tubes and filler rods and set the temperature to 110 ºC. 2. Check the reservoir of the ultrasonic cleaning unit to make sure it is clean.
Page 53 Preparing Samples ASAP 2020 Confirm 8. Using nitrogen, dry the interior of the sample tubes and filler rods under a vent hood. Use a tubing extension long enough and small enough in diameter to fit inside the tubes. 9. Stand the sample tubes on the sample tube rack and place the filler rods in a basket or in the rack.
Page 54 ASAP 2020 Confirm Preparing Samples 11. Using either rubber gloves or a lint-free cloth (but not bare hands), place a filler rod (if used) in each sample tube by holding the sample tube horizontally and sliding the filler rod into the sample tube slowly.
Page 55: Determining Amount Of Sample To Use
Preparing Samples ASAP 2020 Confirm Determining Amount of Sample to Use Clean, dry sample tubes are essential for accurate results. How much sample to use can be determined best by experiment. In general, a sample providing 40 to 120 square meters of total surface area is recommended for nitrogen analysis.
Page 56 ASAP 2020 Confirm Preparing Samples 7. Using a funnel, pour sample from the container into the sample tube. If some sample clings to the inside of the sample tube above the last 3 in. (7.5-cm) of the tube, use a pipe cleaner or lint-free wipe to remove it.
Page 57: Degassing The Sample
Preparing Samples ASAP 2020 Confirm Degassing the Sample Most solid materials absorb moisture and other contaminants when exposed to the atmosphere. The sample must be clean when an analysis is performed. The sample is heated and placed under vacuum to remove moisture and other contaminants. This process is referred to as degassing the sample.
Page 58 ASAP 2020 Confirm Preparing Samples 3. Remove the rubber stopper from the sample tube and attach the sample tube set to the degas port. Be sure to 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 to the degas port and turning the connector nut clockwise.
Page 59: Transferring The Degassed Sample To The Analysis Port
Preparing Samples ASAP 2020 Confirm Transferring the Degassed Sample to the Analysis Port The sample tube must be removed from the degas port, weighed and then installed onto the analysis port for analysis. If the sample tube is not mounted to the analysis port immediately, either leave it on the degas port or remove it and insert the rubber stopper (unless you are using a seal frit) into the sample tube opening.
Page 60 ASAP 2020 Confirm Preparing Samples 9. Place the sample tube Dewar cover over the sample tube stem just above the isothermal jacket as shown in the following illustration. Port Fitting Seal Frit (optional) Po Tube O-ring Ferrule Connector Nut Insulated...
Page 61: Installing Dewars
Installing Dewars ASAP 2020 Confirm Installing Dewars Precautions Always handle Dewars with care. Any product with a glass vacuum flask is a potential safety hazard and should be treated with caution. We recommend the following be observed when handling Dewars containing liquefied gases: •...
Page 62: Cold Trap Dewar
ASAP 2020 Confirm Installing Dewars Cold Trap Dewar Cryogens can cause frostbite injury. Wear safety glasses and insulating gloves when handling cryogens. 1. Fill the cold trap Dewar with a cryogen such as liquid nitrogen to about 5-cm (2-in.) from the top.
Page 63: Analysis Dewar
Installing Dewars ASAP 2020 Confirm Analysis Dewar 1. Fill the analysis Dewar with the analysis bath fluid to about 5-cm (2-in.) from the top. Incorrect fluid levels can lead to measurement errors. Do not overfill the Dewar. 2. Check the analysis bath fluid level with the dipstick as shown below.
Page 64: Performing An Analysis
ASAP 2020 Confirm Performing an Analysis Performing an Analysis After the sample has been degassed and transferred to an analysis port, you may begin an analysis. You cannot perform an analysis while calibration is in progress. Before beginning an analysis, make sure the tank pressure for the gas regulator is at least 200 psig.
Page 65 Performing an Analysis ASAP 2020 Confirm 4. To generate a report automatically after the analysis, click Report After Analysis choose report output options. You can generate reports to the screen (Preview) or directly to a printer. A Developer can also Export data to a file name; the Export option is unavailable for an Analyst.
Page 66: Printing File Contents
ASAP 2020 Confirm Printing File Contents Printing File Contents You can print the contents of one or more sample file, parameter file, or file template. 1. From the File menu, select Print; a drop-down list containing file types is displayed.
Page 67: Listing File Statistics
Listing File Statistics ASAP 2020 Confirm Listing File Statistics You can generate a list of the following information on a sample file, parameter file, or sample template for one or more files: • File name • Date the file was created (or last edited) •...
Page 68: Importing Sample And Parameter Files
The Import function allows you to import files which have been created on a computer other than the one controlling the analyzer and have them display in the Files list window. Review the Micromeritics PROGRAM License Agreement for restrictions on the use of another copy Perform the following steps to import a file: 1.
Page 69: Exporting A Sample Information File
Exporting a Sample Information File ASAP 2020 Confirm Exporting a Sample Information File An Analyst is not authorized to export sample files. Export allows a Developer to: • export the entire sample file to the Export directory. For example, you may wish to use this option to transfer a sample file to another computer.
Page 70: Generating Graph Overlays
ASAP 2020 Confirm Generating Graph Overlays Generating Graph Overlays Use graph overlays when you wish to compare graphically results for multiple samples or multiple graphs for one sample. Graphical lines are differentiated by the use of varying symbols and reported in a legend on the report. If color output capability is available, different colors are used instead of symbols.
Page 71: Multiple Samples Overlay
Generating Graph Overlays ASAP 2020 Confirm Multiple Samples Overlay 1. From the main menu bar, select File > Open > Sample Information to display the Open Sample Information File dialog box. 2. Select a sample on which to overlay graphs of other samples, then click ;...
Page 72 ASAP 2020 Confirm Generating Graph Overlays If you are overlaying this type of report..Then ..BET Surface Area Select the Overlay Samples check box. Langmuir Surface Area Click Freundlich Temkin t-Plot Alpha-S f-Ratio BJH Adsorption Choose the report variable from the Selected Reports...
Page 73 Generating Graph Overlays ASAP 2020 Confirm 11. Select Reports >Start Report; the Start Report dialog is displayed with the name of your primary file highlighted. 12. Click ; one of the following occurs: Report • if you clicked to save specified overlay options, the Select Reports dialog is Save displayed.
Page 74: Multiple Graphs Overlay
ASAP 2020 Confirm Generating Graph Overlays Multiple Graphs Overlay Remember that multiple graph overlays can be done only for: • BJH Adsorption • BJH Desorption • Dollimore-Heal Adsorption • Dollimore-Heal Desorption • DFT Pore Size • DFT Surface Energy • Horvath-Kawazoe •...
Page 75 Generating Graph Overlays ASAP 2020 Confirm 5. From the Selected Reports list, select the report for which you want multiple graph overlays, then select ; a Report Options dialog for that report is displayed (this Edit example shows BJH Adsorption).
Page 76 ASAP 2020 Confirm Generating Graph Overlays 12. Click ; one of the following occurs: Report • if you clicked to save specified overlay options, the Select Reports dialog is Save displayed. • If you did not click , a dialog stating that a preview report will be generated or you Save can cancel the operation is displayed.
Page 77: File Menu
Description ASAP 2020 Confirm 4. FILE MENU The File menu contains commands which allow you to manage sample and parameter files. Description Listed below are brief descriptions of the File menu commands. Detailed descriptions follow this section. Allows you to create a sample information or parameter file.
Page 78 Convert Allows you to convert a sample file in the MICMOS 2000 or 2000 micropore format to a format compatible with the ASAP 2020 Confirm program. Refer to Convert, page 108. Log in Allows you to log into the application. Refer to In, page 4-109.
Page 79: New
ASAP 2020 Confirm New allows you to create a sample information or parameter file. Regardless of the type of file you are creating, a dialog allowing you to choose a template is displayed. Title bar indicates type of file you are creating.
Page 80: Analyst
This field defaults to the description of the template. You must enter a new description or edit the existing one; the ASAP 2020 Confirm program does not allow duplicate descriptions. The description you enter in this field appears in the Files list window on the Open Sample Information dia- .
Page 81 ASAP 2020 Confirm Calculate Enables the Empty tube and Sample + tube fields, allowing you to enter appropriate values. These values are used to calculate the mass of the sample, Mass Mass – Mass sample sample tube tube Density If you plan to use a calculated free space, enter the sample’s density in this field.
Page 82 Comments window, a file with the same ID currently exists in the selected directory. You must choose a different directory or edit the identification of the current file. The ASAP 2020 Confirm program does not allow duplicate descriptions. 202-42811-01 - Mar 2011...
Page 83: Developer
ASAP 2020 Confirm Close Closes the dialog. If the file contains unsaved changes, you are prompted to save before the dialog box closes. Advanced Displays the sample information dialog in the Developer’s format. This format allows you to view details of the sample file and allows some fields to be edited.
Page 84 ASAP 2020 Confirm Operator Enter the name of the operator (analyst) who will be using Submitter this file to perform the analysis and the name of the person (or department) submitting the sample for analysis. You can use up to 40 characters in each field.
Page 85 ASAP 2020 Confirm User Parameters These fields are used primarily for SPC (Statistical Process Control) reporting. However, they can be used for other data as well. You may wish to enter specific analysis conditions or sample criteria. These parameters print on the Options report.
Page 86 Comments window, a file with the same ID currently exists in the selected directory. You must choose a different directory or edit the identification of the current file. The ASAP 2020 Confirm program does not allow duplicate descriptions. Save as Template Enables you to save all parameters of the current file as a sample information file template.
Page 87 ASAP 2020 Confirm Basic Displays the sample information dialog in the Analyst format (refer to Analyst, page 4-4). 202-42811-01 - Mar 2011 4-11...
Page 88: Sample Tube
ASAP 2020 Confirm Sample Tube The fields on this dialog are used for storing sample tube information. Before creating a sample tube file, you should perform a blank analysis (no sample) using the sample tube. Sample Tube Displays a description of the current file. If this is a new file, this field displays the template description;...
Page 89 Save ID currently exists. You must edit the identification of the current file before it can be saved. The ASAP 2020 Confirm program does not allow duplicate descriptions. Enables you to save all parameters of the current file as a Save as Template sample tube file template.
Page 90: Degas Conditions
ASAP 2020 Confirm Degas Conditions The fields on this dialog are used for specifying degas conditions when your ASAP 2020 is equipped with the SmartVac degas option. If you do not have the SmartVac, the values you enter are meaningless.
Page 91 ASAP 2020 Confirm Target temperature Allows you to specify a temperature at which the sample will be held for the remainder of the evacuation. Evacuation rate Enables you to specify an evacuation rate for initial evacuation. Unrestricted evac. from Enables you to specify a pressure at which unrestricted sample evacuation will begin.
Page 92 Save ID currently exists. You must edit the identification of the current file before it can be saved. The ASAP 2020 Confirm program does not allow duplicate descriptions. Save as Template Enables you to save the parameters of the current file as a Degas Conditions file template.
Page 93: Analysis Conditions
ASAP 2020 Confirm Analysis Conditions This dialog allows you to specify the analysis conditions for your sample. An analysis conditions file can be created as an independent parameter file or as part of the sample information file. ROA parameters display only if ROA option is installed.
Page 94 0.050 / 760.0 = 0.0000658 will result in an error. The analysis will terminate. Several analysis conditions files containing complete pressure tables are included with the ASAP 2020 Confirm software. The pressure table for automatically collected data includes the pressure points for data collection and identifies calculations through which the data are processed.
Page 95 ASAP 2020 Confirm Pressure Table Edit an existing value by highlighting the field and entering the desired value. Use to add rows for additional Insert values. To append to the beginning or to the end of the table, , respectively.
Page 96 ASAP 2020 Confirm Inserts geometrically spaced points from the saturation Geometric from pressure. For example, to insert 5 points with a 0.99 starting saturation pressure and a 0.84 ending pressure, the following points are inserted into the table: 0.99 0.98 0.96...
Page 97 ASAP 2020 Confirm Absolute pressure dosing Select this option to specify pressure targets in mmHg, mbar, or kPa instead of relative pressure. This option is typically selected when using adsorptives at analysis conditions above the critical point of the gas; for example, H adsorption on carbon at liquid nitrogen temperature.
Page 98 ASAP 2020 Confirm Evacuation time Enables you to enter the length of time for preliminary evacuation, which takes place prior to the free-space measurement. Leak test Enables the system to check for leaks or sample outgassing before the analysis. The leak test allows sample pressure to rise during the test.
Page 99 ASAP 2020 Confirm Measure Select this option to have free space measured automatically by the system. Typically, it is best to measure the free space when analyzing macro- and mesoporous samples, and for routine surface area measurements. Select Lower dewar for evacuation to lower the dewar following free-space measurements.
Page 100 ASAP 2020 Confirm Calculate Select this option to have the free-space calculated using the mass, density, and sample tube parameters entered in the Sample Information and Sample Tube files. Calculated free space measurement takes less time than measured free space, so if you know the mass and density of the sample and the sample tube parameters, you may wish to use this choice of free space methods.
Page 101 ASAP 2020 Confirm Option Prompts for... a Po and analysis bath temperature an analysis bath temperature only (when Absolute pressure dosing is selected on the Analysis dialog) a psat gas other than the adsorptive; the temperature and pressure ranges for the chosen gas are displayed.
Page 102 ASAP 2020 Confirm First Pressure Fixed The first point on the pressure table is the threshold value, Dose triggering the transition from the Fixed Dose Mode to (continued) Pressure Table Mode. When the first pressure table value is reached, Fixed Dose Mode is disabled, and points are equilibrated and recorded in accordance with the specified pressure table.
Page 103 ASAP 2020 Confirm Low pressure Enabled only if the MicroPore option is installed. Choose this incremental option when you are performing an analysis of microporous dose mode materials. At low pressures on Type 1 isotherms, the pressure points are very closely spaced, making a useful pressure table difficult to define.
Page 104 ASAP 2020 Confirm Equilibration Displays the Equilibration dialog. Does not display when Absolute dosing is selected. Equilibration interval Use this table to enter pressure ranges and intervals between table them. Long equilibration intervals tend to lengthen analyses, however, they do improve data integrity. Short equilibration intervals produce a faster analysis but may reduce the accuracy of data.
Page 105 ID Save currently exists. You must edit the identification of the current file before it can be saved. The ASAP 2020 Confirm program does not allow duplicate descriptions. Save as Template Enables you to save all parameters of the current file as an analysis conditions file template.
Page 106: Adsorptive Properties
ASAP 2020 Confirm Adsorptive Properties This dialog allows you to specify the characteristics of the gases used in the ASAP 2020 system. An Adsorptive Properties file can be created as an independent parameter file or included as part of the sample information file.
Page 107 ASAP 2020 Confirm Maximum manifold The maximum gas pressure allowed in the manifold. pressure Density conversion factor This value is used to convert the gas volume at STP to liquid volume for the adsorptive. It is the ratio of gas density at STP to liquid density.
Page 108 ASAP 2020 Confirm You can edit the table by clicking on the desired saturation Psat vs. T pressure or temperature and entering a different value. (continued) to insert a new row above the selected line; the Insert cursor moves to the new line. Use...
Page 109 ID Save currently exists. You must edit the identification of the current file before it can be saved. The ASAP 2020 Confirm program does not allow duplicate descriptions. Save as Template Enables you to save all parameters of the current file as an adsorptive properties file template.
Page 110: Report Options
ASAP 2020 Confirm Report Options This dialog allows you to specify report options. A report options file can be created as an independent parameter file or included as part of the sample information file. Description Displays a description of the current Report Options template.
Page 111 ASAP 2020 Confirm Show graphic Select this option to have a graphic display above the report title. The graphic can be in a bitmap (bmp) or an enhanced metafile (emf) format. For example, you may wish to display your company logo. Click...
Page 112 ASAP 2020 Confirm Apply thermal Select this option to correct for the temperature-induced transpiration correction pressure difference between the manifold and the chilled sample tube. This option is most significant for pressures less than approximately 1.0 mmHg. Never use filler rods in...
Page 113 ID Save currently exists. You must edit the identification of the current file before it can be saved. The ASAP 2020 Confirm program does not allow duplicate descriptions. Enables you to save all parameters of the current file as an Save as Template adsorptive properties file template.
Page 114: Summary Report
ASAP 2020 Confirm Summary Report The Summary report provides a condensed listing of analysis statistics and data results. The Summary Report Options dialog allows you to choose the type of information to include in the report. The choices on this dialog allow you to choose the types of data to include in the Summary report.
Page 115 ASAP 2020 Confirm Displays the Pass/Fail Options dialog so that you can choose Pass/Fail a parameter on which to specify pass/fail criteria. Upper/Lower Select these options to specify upper and lower limits for the selected parameter; a valid range for the selected field is displayed in the information bar.
Page 116: Isotherm Report Options
ASAP 2020 Confirm Isotherm Report Options The isotherm report indicates adsorption (up to saturation pressure) and desorption (down from saturation pressure) of a gas by a solid held at constant temperature. Select Reports Lists the formats of reports offered. Choices: Tabular Report, Linear plot, Logarithmic plot,...
Page 117 ASAP 2020 Confirm Displays the related Plot Options dialog; this example shows Options the dialog for the Linear plot. All plot dialogs contain the same options. You can plot the graphs as a curve, points, or both. Select Overlay samples to overlay data from the current plot with data from other samples.
Page 118 ASAP 2020 Confirm Volume Adsorbed Enables you to choose the manner in which the volume adsorbed is reported. These data are reported by default as Per Gram (cm /g). However, you can choose to report data Per BET Surface Area (cm...
Page 119: Bet/Langmuir Surface Area Report Options
ASAP 2020 Confirm BET/Langmuir Surface Area Report Options • The BET calculation obtains the sample surface area value by determining the monolayer volume of adsorbed gas from the isotherm data. • The Langmuir calculation determines the surface area of a sample by relating the surface area to the volume of gas adsorbed as a monolayer.
Page 120 ASAP 2020 Confirm Autoscale x-axis Select these options to have the X- and/or Y-axes scaled Autoscale y-axis automatically. Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points. If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges.
Page 121 ASAP 2020 Confirm Displays the Surface Area Report Pressure Selection dialog, Insert predefined allowing you to select predefined points. Choices: 1 Point, 3 Point, 5 Point, 5 Point Low Pressure Insert Inserts a row into the table above the selected line.
Page 122: Freundlich Isotherm
ASAP 2020 Confirm Freundlich Isotherm The Freundlich isotherm is an empirical isotherm that is used to model low-pressure adsorption data. It can also be applied to model some micropore isotherms. Specify monolayer In this field, enter the monolayer capacity of the sample.
Page 123 ASAP 2020 Confirm Autoscale x-axis Select these options to have the X- and/or Y-axis scaled Autoscale y-axis automatically. Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points. If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges.
Page 124: Temkin Isotherm
ASAP 2020 Confirm Temkin Isotherm The Temkin isotherm is used to model adsorption data where the heat of adsorption drops linearly with increasing coverage. Specify monolayer In this field, enter the monolayer capacity of the sample. capacity Specify differential Enter the differential heat of adsorption at zero surface heat of adsorption coverage.
Page 125 ASAP 2020 Confirm Temkin isotherm plot Overlays the Temkin isotherm with the analysis data. Overlay samples Choose this option to overlay Freundlich isotherm data from the current file with the same type of data from other samples (files). The desired files are chosen by selecting Overlays the Report Options dialog.
Page 126: T-Plot Report Options
ASAP 2020 Confirm 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 127 ASAP 2020 Confirm Reference Displays the Entered t-Curve dialog allowing you to define a t-curve by entering the relative pressure and thickness values. This table can also be created in another application if desired and imported into this dialog using .
Page 128 ASAP 2020 Confirm Kruk-Jaroniec-Sayari Displays the Kruk-Jaroniec-Sayari Thickness Equation dialog. You can edit the values for the numerator, the first element of the denominator, and the exponent.The range for a selected field is shown in the information bar at the bottom of the dialog.
Page 129 ASAP 2020 Confirm Halsey Displays the Halsey Thickness Equation dialog. You can edit the values for the multiplier, numerator, and exponent.The range for a selected field is shown in the information bar at the bottom of the dialog. Refer to t-Plot, page C-11, for additional information.
Page 130 ASAP 2020 Confirm Broekhoff-de Boer Displays the Broekhoff-de Boer Thickness equation dialog. You can edit the values for the multiplier, numerator, and exponent. The range for a selected field is shown in the information bar at the bottom of the dialog.
Page 131 ASAP 2020 Confirm Pressure Range Displays the Report Relative Pressure Range dialog so that you may specify minimum and maximum relative pressures to use with this report. • If Use calculation assignments is not selected on the Col- lected/Entered dialog, all of the nonoutlier points of the collected data within the specified range are used for calcu- lating the data for this report.
Page 132 ASAP 2020 Confirm Autoscale x-axis Select these options to have the X- and/or Y-axes scaled Autoscale y-axis automatically. Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points. If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges.
Page 133: Alpha-S Plot
ASAP 2020 Confirm Alpha-S Plot The Alpha-S plot converts the standard adsorption isotherm into a dimensionless isotherm using the quantity adsorbed at a relative pressure of 0.4. Table Provides two columns for entering the relative pressure (first column) and the alpha-s values (second column). This table...
Page 134 ASAP 2020 Confirm Allows you to import the values from an existing alpha-s Open curve (ALS) into the table. One predefined curve is shipped with the analysis program. After the values are copied into the table, you may edit them if desired. Editing these values will not affect the file from which they were copied.
Page 135: F-Ratio Plot
ASAP 2020 Confirm From/To fields Enabled when you choose not to autoscale data (deselect the Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot.
Page 136 ASAP 2020 Confirm Relative pressure range Allows you to enter a pressure range when calculations assignments are not used. Tabular report Choose this option to have a tabular report generated The tabular report contains four columns: relative pressure, quantity adsorbed for the isotherm of interest, quantity adsorbed for the reference isotherm, and the ratio of the quantities adsorbed.
Page 137: Bjh Adsorption/Desorption Report Options
ASAP 2020 Confirm BJH Adsorption/Desorption Report Options This field does not display on the BJH Desorption dialog The BJH Adsorption and Desorption dialogs include the same fields; the operating instructions for both are the same. 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.
Page 138 ASAP 2020 Confirm Displays the equation for the type of thickness curve selected. Edit Refer to Report Options, page 4-34 for information on the equations for thickness curves. Minimum/Maximum Provides fields for entering the minimum and maximum size pore to be included in BJH reports. The size can be reported in width (default), radius, or diameter.
Page 139 ASAP 2020 Confirm The recommended adsorptives and their values are shown. Adsorptive (continued) You may specify up to six additional adsorptive/adsorbate property factor combinations. The adsorbate property factor is the combination of constants in the numerator of the BJH equation which is specific to the type of gas used.
Page 140 ASAP 2020 Confirm Selected Reports Lists the available BJH reports. • Tabular Report • Cumulative Pore Volume • dV/d* Pore Volume • dV/dlog(*) Pore Volume • Cumulative Pore Area • dA/d* Pore Area • dA/dlog(*) Pore Area * = width, radius, or diameter...
Page 141 ASAP 2020 Confirm Tabular Report The BJH Adsorption/Desorption tabular report allows you to specify the method of data reduction. You can measure pore width, diameter, or radius; pore size can be expressed in angstroms or nanometers. Select Options > Units to specify desired units.
Page 142 ASAP 2020 Confirm Enabled when Fixed pore size table is selected for tabular Table data. Displays the BJH Adsorption (or Desorption) Fixed Pore Size Table dialog, allowing you to enter or edit a fixed pore size table. The table must contain a minimum of two points and may include as many as one thousand.
Page 143 ASAP 2020 Confirm Plot Options Selecting a BJH plot option from the BJH Adsorption or Desorption Report Options dialog enables you to specify the plotting method used for your report and to customize the plot. You can measure pore width, diameter, or radius; pore size can be expressed in angstroms or nanometers.
Page 144 ASAP 2020 Confirm Autoscale X-axis range fields show pore radius or diameter in (continued) angstroms or nanometers. Data ranges are displayed in the information bar across the bottom of the dialog when the cursor is in a numerical data entry field.
Page 145: Dollimore-Heal Adsorption/Desorption Report Options
ASAP 2020 Confirm Dollimore-Heal Adsorption/Desorption Report Options You can generate DH reports from both adsorption and desorption data. Or Dollimore-Heal Desorption Report Options The options for Dollimore-Heal reports are the same as those for the BJH reports with the exception of BJH Correction and Adsorptive properties; this item is not applicable to DH reports.
Page 146: Horvath-Kawazoe Report Options
ASAP 2020 Confirm Horvath-Kawazoe Report Options This report is available only if you have the Micropore option installed. Pore Geometry Select the option in this group box which best represents the physical geometry of the micropores in the sample material.
Page 147 ASAP 2020 Confirm Computed The interaction parameter is calculated using the parameters on the Horvath-Kawazoe Physical Properties dialog. You can click to view or edit these parameters. Each time Properties you change one of the parameters, the interaction parameter is recalculated. The formula for computing the interaction parameter is given in CALCULATIONS, page C-1.
Page 148 ASAP 2020 Confirm Adsorbent Group Box Diameter (continued) The diameter of the sample atom. Diameter at zero energy The diameter of an atom at zero interaction energy, (2/5) x diameter. Polarizability The polarizability of the adsorbent. Magnetic susceptibility The magnetic susceptibility of the adsorbent.
Page 149 ASAP 2020 Confirm Selected Reports Lists the available Horvath-Kawazoe reports. Choose a report by double-clicking on the report name or highlight the report name and press the . A report is selected Spacebar when it is preceded with a check mark.
Page 150 ASAP 2020 Confirm Plot Options Selecting a Horvath-Kawazoe plot option from the Horvath-Kawazoe Report Options dialog enables you to specify the plotting method used for your report and to customize the plot. Plots for Cumulative Pore Volume and dV/dw Pore Volume are available.
Page 151 ASAP 2020 Confirm Y-axis options Choose Autoscale to have the y-axis scaled automatically. Y- (continued) axes begin at zero. The system uses the highest value collected during analysis as the ending point. If you deselect Autoscale, the corresponding fields are enabled so that you may enter a beginning and ending value.
Page 152: Dft Pore Size
If the list is empty, there were no models that meet the selected criteria. Link to Models Provides access to the Micromeritics web page containing information on the DFT models. 4-76 202-42811-01 - Mar 2011...
Page 153 ASAP 2020 Confirm Displays the Report Relative Pressure Range dialog so that Pressure Range you may specify minimum and maximum relative pressures to use with this report. • If Use calculation assignments is not selected on the Col- lected/Entered dialog, all of the nonoutlier points of the collected data within the specified range are used for calcu- lating the data for this report.
Page 154 ASAP 2020 Confirm Use this push button to edit details of a selected graph; a Edit dialog like the following is displayed. Displays the type of graph you are editing. Displays the range for the selected field This push button is disabled for tables and Goodness of Fit graphs.
Page 155: Dft Surface Energy
ASAP 2020 Confirm DFT Surface Energy The fields on the Surface Energy dialog are identical to those on the DFT Pore Size dialog with the following exceptions: Geometry drop-down list Is not applicable to the Surface Energy report and, therefore, does not display on its dialog.
Page 156: Dubinin Report Options
ASAP 2020 Confirm Dubinin Report Options Report Type Allows you to specify the type of report you want. At least one type of report must be selected. Select Radushkevich to generate the Radushkevich report. Select Astakhov to generate the Astakhov report. With this choice, you may select Optimize Astakhov exponent.
Page 157 ASAP 2020 Confirm Displays the Dubinin Adsorptive Options dialog allowing Adsorptive you to specify up to 8 Adsorptive/Affinity Coefficient (beta) combinations. Pressure Range Displays the Report Relative Pressure Range dialog so that you may specify minimum and maximum relative pressures to use with this report.
Page 158 ASAP 2020 Confirm Tabular Report The Tabular report enables you to customize your report with one to six columns of data for Astakhov reports and one to five columns of data for Radushkevich reports. The Dubinin Tabular Report Column Options dialog box is displayed.
Page 159 ASAP 2020 Confirm Autoscale x-axis If you choose not to autoscale data for either (or both) axis, Autoscale y-axis the adjacent fields are enabled so that you may enter a (continued) beginning and ending value. Data collected outside these ranges are not included in the plot.
Page 160 ASAP 2020 Confirm Autoscale x-axis Select these options to have the X- and/or Y-axes Autoscale y-axis automatically scaled. Both X- and Y-axes begin at zero, and the system uses the highest values collected during analysis as the ending points for axes ranges.
Page 161: Mp-Method Report Options
ASAP 2020 Confirm MP-Method Report Options Thickness Curve Select the type of thickness curve from this group box. You group box must choose either the Halsey equation or the Harkins and Jura equation. Use to edit the values in the Equation equation.
Page 162 ASAP 2020 Confirm Halsey Displays the Halsey Thickness Equation dialog. You can edit the values for the multiplier, numerator, and exponent.The range for a selected field is shown in the information bar at the bottom of the dialog. Refer to CALCULATIONS, page C-1, for additional information.
Page 163 ASAP 2020 Confirm Tabular Report The Tabular report enables you to customize your report with one to six columns of data. (The data types in the first and second columns cannot be changed.) The MP-Method Tabular Report Column Options dialog is displayed.
Page 164 ASAP 2020 Confirm Plot options You can plot data with a curve, points, or both. X-axis options Choose Autoscale to have the x-axis scaled automatically. The X-axis begins at zero and the system uses the highest value collected during analysis as the ending point.
Page 165: Options Report
ASAP 2020 Confirm Options Report The Options report provides pertinent information for the following: • Degas conditions • Adsorptive properties • Analysis conditions • Sample tube criteria • Free space • Po and temperature • Equilibration • Isotherm collection Sample Log Report The Sample Log report displays the following: •...
Page 166: Validation Report
ASAP 2020 Confirm Validation Report Use this report to have your data examined by the software to determine if the results are within typical ranges. If the data for any reports you selected for validation are determined to be out of range, a warning is displayed and suggestions are given for corrective action.
Page 167: Collected/Entered Data
ASAP 2020 Confirm Collected/Entered Data If you choose Manually entered as the type of data in the Sample Information dialog, an Entered tab is added allowing you to enter the data. If you choose Automatically collected as the type of data in the Sample Information dialog, a Collected Data tab is added when analysis is complete.
Page 168 ASAP 2020 Confirm Enabled for entered data; inserts a row into the pressure Insert table. Delete Enabled for entered data; deletes the selected row. Clear Enabled for entered data; clears the entire table of all entries except one (one is required).
Page 169: Open
Open ASAP 2020 Confirm Open Open allows you to open an existing sample or parameter file, as well as a sample or parameter template. Sample Information File The following dialog displays for the Analyst and Developer when Open, Sample information is selected from the File menu.
Page 170 ASAP 2020 Confirm Open Status This drop-down list allows you to choose the types of sample files to display in the Files window. All files of the type you choose, within the range of dates, and in the current directory are displayed.
Page 171: Analyst
Open ASAP 2020 Confirm Analyst When an Analyst opens a sample information file, the dialog displays in this manner: If desired, an Analyst can click to access a Developer’s view of the dialog. This Advanced view allows an Analyst to review the parameters used in the analysis. An Analyst can edit certain parameters of the sample file;...
Page 172: Developer
ASAP 2020 Confirm Open Developer When a Developer opens a sample information file, the dialog displays in this manner: A Developer can view all parameters of the file, as well as edit certain parameters; those parameters are enabled. Report options can also be edited and reports generated.
Page 173: Parameter Files
Open ASAP 2020 Confirm Parameter Files Parameter files (Sample Tube, Degas Conditions, Analysis Conditions, Adsorptive Properties, and Report Options) can be opened by an analyst or a Developer. An Analyst, however, can only view the values. An Analyst’s view of a parameter file contains only a push button.
Page 174: Save
The ASAP 2020 confirm program does not allow duplicate descriptions. The new file is saved as specified, but does not remain in the active window. Be sure to open the new file before making any changes.
Page 175 Save As ASAP 2020 Confirm • save a parameter file in the active window with a different name. The parameter file must be of the same type; for example, you can save an Analysis conditions file only as another Analysis conditions file.
Page 176: Save As Template
ASAP 2020 Confirm Save As Template Save As Template An Analyst is not authorized to create sample and parameter file templates. Save As Template is unavailable for an Analyst; a Developer can use this function to: • save the values of the sample file in the active window as a sample template •...
Page 177: Close
Close ASAP 2020 Confirm Close Close enables you to close the file in the active window. If the file contains changes that have not been saved, the following message is displayed: (file name) has been changed. Save changes before closing?
Page 178: Print
ASAP 2020 Confirm Print Print Print enables you to print the contents of a sample file, sample template, or parameter file. Regardless of the type of file you choose, the dialogs are similar; the options presented in the header vary slightly.
Page 179 Print ASAP 2020 Confirm The remainder of the options display regardless of the type of file you request to print. Allows you to specify a range of dates for the files you wish Date Range to display in the Files list window, or you can choose All for all files to display.
Page 180: List
ASAP 2020 Confirm List List List enables you to generate a listing of the following information on a selected sample file, parameter file, or a sample template. • File name • Date the file was created • Time the file was created •...
Page 181: Import
Import ASAP 2020 Confirm Import An Analyst is not authorized to import sample and parameter file templates. A Developer can use this option to import files that have been created external to the Confirm software and copied into the Import directory. If the files are not copied into the Import directory, they will not display in the Files window.
Page 182: Export
ASAP 2020 Confirm Export Export An Analyst is not authorized to export sample files. A Developer can use the Export option to: • export the entire sample file to the Export directory. For example, you may wish to use this option to transfer a sample file to another computer.
Page 183: Format Of Data Output
Export ASAP 2020 Confirm Format of Data Output Description Operator Submitter Sample mass Type of Data* Elapsed time Relative pressure Quantity dosed Absolute pressure *0 = automatically collected 1 = entered (relative pressures) Specific quantity adsorbed 2 = entered (absolute pressures)
Page 184: Convert
Convert allows a Developer to convert sample information files created using the ASAP 2000 to files compatible with the ASAP 2020 Confirm program. The files to be converted must be copied into the Import directory so they will display in the Convert dialog. You do not have to use the Convert function for ASAP 2010 files.
Page 185: Log In
Log In ASAP 2020 Confirm Log In Log in enables you to log into the application; the User Log in dialog is displayed. Simply enter your user name and password, then click O User name Typically in this field, you should enter your Windows User name, unless your Administrator has specified a different user name.
Page 186: Exit
ASAP 2020 Confirm Exit Exit Exit enables you to exit (close) the ASAP 2020 confirm program. • If a window containing a modified file is open, the following message is displayed: (file name) has been changed. Save changes before closing?
Page 187: Unit Menu
Description ASAP 2020 Confirm 5. UNIT MENU The Unit menu contains the options for the operations that can be performed with the ASAP 2020 analyzer. The main menu will contain a Unit menu for each attached analyzer. For example, if you have two attached analyzers, the main menu contains two Unit menus. The appropriate unit number and serial number display in the title bar of the operational windows.
Page 188 ASAP 2020 Confirm Description Show Status Shows the status window of the operation in progress. Page 5-13. Show Instrument Log Displays a log of recent analyses, calibrations, and error mes- sages. Page 5-14. Unit Configuration Displays the configuration of the analyzer. Page 5-16.
Page 189: Sample Analysis
Sample Analysis ASAP 2020 Confirm Sample Analysis When you select this option from the Unit menu, the Sample Analysis dialog is displayed with all fields disabled (greyed) and the Start Analysis dialog positioned on top. This allows you to select a sample file for your analysis.
Page 190 ASAP 2020 Confirm Sample Analysis Sample Displays an identification of the sample file. Mass Enables you to enter the sample’s mass. Sample Tube Displays the description of the Sample Tube file for the cur- rent sample file. The drop-down list contains a list of predefined parameter files.
Page 191 Sample Analysis ASAP 2020 Confirm Warm and Cold Free space Enabled if you have chosen to enter the free space values (Free Space option on the Analysis Conditions dialog). Enter (or confirm) the appropriate values. Report After Analysis Displays the Report Settings dialog so that you may specify report output options.
Page 192 ASAP 2020 Confirm Sample Analysis Allows you to have isotherm generated automatically after Export After Analysis the analysis; displays the Export Settings dialog so that you may specify output options. Start Begins the analysis; a logon dialog is displayed. This dialog is used to verify that the logged-in user is actu- ally performing the analysis.
Page 193 Sample Analysis ASAP 2020 Confirm Suspends the analysis. Suspend This push button is disabled for an Analyst. Skip Skips the current step of the analysis. This push button is disabled for an Analyst. Use the Skip function with caution; the ASAP performs multiple steps for a given task.
Page 194: Start Degas
ASAP 2020 Confirm Start Degas Start Degas This option allows you to choose the file and start degas operations on one or two samples; the Automatic Degas dialog is displayed. Sample Click to the right of this field to select a sample file, Browse to create one) to use with the current sample.
Page 195: Enable Manual Control
Enable Manual Control ASAP 2020 Confirm Enable Manual Control Select this option to control certain components of your system manually. If the instrument schematic is not displayed, select Show Instrument Schematic. When manual control is enabled, the valve symbols change color on the monitor screen to indicate their status.
Page 196 ASAP 2020 Confirm Enable Manual Control Valves System valves and their functions are listed in Table 5-1. Actions: Open, Close, Pulse Closed Open Pulse briefly opens and closes (or vice versa) the valve. Table 5-1. System Valves Valve Description Unrestricted vacuum...
Page 197 Enable Manual Control ASAP 2020 Confirm The remainder of the components are displayed for informational purposes only; they cannot be controlled manually. Represents the sample tube. Represents the Psat tube. This group of rectangles on the left side of the schematic dis-...
Page 198: Show Instrument Schematic
ASAP 2020 Confirm Show Instrument Schematic Show Instrument Schematic Select this option to display a schematic of the ASAP 2020 analyzer. The schematic is a graphical representation of the plumbing system including system valves, the analysis station, and the Dewar position. The valves and Dewar can be controlled from the schematic when Manual control is enabled.
Page 199: Show Status
Show Status ASAP 2020 Confirm Show Status A status window is shown across the bottom of all operational dialogs as well as the instru- ment schematic. The Show Status option enables you to show only the status window. This frees up your computer screen allowing you to perform other tasks (such as creating or edit- ing sample files), while still monitoring the progress of your analysis.
Page 200: Show Instrument Log
ASAP 2020 Confirm Show Instrument Log Show Instrument Log Displays a log of recent analyses, calibrations, and errors or messages. By default, this information is logged for a 60-day period for analyses and messages, and a 90-day period for calibrations. A Developer can change the time for which Analyses, Cali- brations, and/or Messages are retained by making an entry in the Unit section of the CFR 2020.INI file located in the Status directory;...
Page 201 Show Instrument Log ASAP 2020 Confirm Displays the Log Report Settings dialog allowing you to Report generate the log contents to a specified destination. Use the Start Date field to specify the date at which to start the printout. This date does not limit the entries that display in the window, it is only pertinent to the entries that will be printed on the report.
Page 202: Unit Configuration
ASAP 2020 Confirm Unit Configuration Unit Configuration Select this option to view the current calibration settings, the date on which calibration was performed, and the software and hardware configuration of your system. Volume Calibration Displays the system, lower, and reference volumes from the most recent calibration.
Page 203 Unit Configuration ASAP 2020 Confirm Configuration Displays the following: • The hardware code specifying the hardware components (for example transducers) present in your analyzer. This code is provided so the Service Department may quickly identify your hardware configuration and provide prompt assistance.
Page 204: Diagnostics
ASAP 2020 Confirm Diagnostics Displays the Board ID dialog so that you can view the sta- Board ID tistics of the board contained in the requested slot of the computer. Diagnostics This option enables you to clean and verify gas lines when connecting or changing a gas. This option also allows you to perform diagnostic tests which your service representative may request.
Page 205 Diagnostics ASAP 2020 Confirm View Allows you to view the current operation, the instrument schematic, or the instrument log in the Service Test dialog. Operation is the appropriate choice for tests. Test Contains a list of diagnostic tests. These tests will always include the latest revision letter at the end of the test name.
Page 206 ASAP 2020 Confirm Diagnostics Report (field) Contains a list of the reports that will be generated during this test. Item [n] Lists the data in the two panes. Item 1 is the upper pane and Item 2, the lower pane.
Page 207: Calibration
Calibration ASAP 2020 Confirm Calibration An Analyst is not authorized to perform calibrations. This option allows you to calibrate the vacuum gauge, pressure gauge, pressure scale, mani- fold temperature, and system volume. You can also save the current calibrations to a file or load a different calibration file.
Page 208: Pressure Scale
ASAP 2020 Confirm Calibration Pressure Scale Use this option to adjust the scale of the transducer to match a reference standard; the Cali- brate Pressure Scale dialog is displayed. A Pressure Scale option will be available for each type of transducer you have installed. For example, if you have the 1000-mmHg and the 10-mmHg transducers installed, a Pressure Scale option is displayed for the adjustment of each one.
Page 209: Volume
Calibration ASAP 2020 Confirm Volume Use this option to calibrate the system volume; the Calibrate System Volume dialog is displayed. Displays as Next if you choose Measured. The system volume typically is calibrated after servicing valves, transducers, or any part of the analysis plumbing.
Page 210 ASAP 2020 Confirm Calibration Reference Volume Enter the volume in cubic centimeters for the reference vol- ume you are using in this calibration. Reference Volume Temp. Enter the temperature of the reference volume. Since the ref- erence volume should be submerged in an ice bath, this value should remain at 0.0 for best accuracy.
Page 211: Save To File
Calibration ASAP 2020 Confirm Save to File Use this option to save the current calibration settings to a file; the Select Calibration File dia- log is displayed. File name Defaults to the next sequence number for calibration files. The sequence number consists of: xxx-yyy.CAL, where xxx = serial number of unit and yyy = sequence number.
Page 212: Degas
ASAP 2020 Confirm Degas Degas This option on the Unit menu is enabled if your ASAP 2020 is equipped with the SmartVac degassing option. The choices on this cascading menu allow you to select operations for the SmartVac degasser. Enable Manual Control Select this option to control manually certain components of the degas operation.
Page 213: Show Instrument Schematic
Degas ASAP 2020 Confirm Table 5-2. Degasser Valves Valve Description D1 and D2 Sample port valves Vacuum valve Servo isolation valve Gas inlet port valve Servo Valve Actions: Set, Close Set displays the Servo Valve Settings dialog so that you can enter a target pressure for sample evacuation.
Page 214: Show Status
ASAP 2020 Confirm Degas Show Status This option allows you to monitor the degassing operation. Sample Displays the sample file being used with the degassing oper- ation for each port. Status Displays the current stage of the degassing operation for each port.
Page 215: Calibrate Pressure Zero
Degas ASAP 2020 Confirm Calibrate Pressure Zero Use this option to evacuate the manifold and zero the transducer. Begins the calibration. Start Status messages are displayed during this procedure, then the dialog closes automatically. Calibrate Pressure Scale Use this option to adjust the scale of the pressure transducer.
Page 216: Calibrate Vacuum Gauge
ASAP 2020 Confirm Degas Calibrate Vacuum Gauge Displays the Calibration Vacuum Gauge dialog containing the current vacuum level. This dialog also allows you to enter a new calibration value (if necessary) obtained using an external reference gauge. Calibrate Servo Use this option to calibrate the servo valve to the manifold pressure transducer. The servo valve should always be recalibrated after a pressure calibration has been performed.
Page 217: Service Test
Various service tests are included in the ASAP 2020 operating program. These tests can be enabled and performed only with the assistance of a trained Micromeritics service represen- tative. These tests are designed to provide your service representative with instrument readouts, as well as to assist him in troubleshooting potential problems and, perhaps, elimi- nating unnecessary repair services.
Page 219: Reports Menu
Description ASAP 2020 Confirm 6. REPORTS MENU This chapter describes the commands on the Reports menu; it also contains examples of reports. Reports can be generated for data: • collected on a sample that has completed analysis • collected on a sample that is currently being analyzed (includes only the information collected up to the time of the report) •...
Page 220 ASAP 2020 Confirm Description SPC Report Options Allows you to specify the sample data to be included in SPC reports. Page 6-7. Allows you to generate a regression report. Page 6-8. Regression Report Control Chart Allows you to generate a control chart report. Page 6-12.
Page 221: Start Report
Start Report ASAP 2020 Confirm Start Report Select this option to generate a report on a sample analysis. Select Start report from the Reports menu to display the Start Report dialog 202-42811-01 - Mar 2008...
Page 222 ASAP 2020 Confirm Start Report Category/Subcategory Use these drop-down lists (directories) to navigate to the desired file(s). • If you select multiple files on which to have reports gener- ated, the reports specified in each sample file are printed to the output destination.
Page 223 Start Report ASAP 2020 Confirm Preview Choose this option to have the report(s) generated to the screen. If a printed copy is desired, you can print the report from the report window. Options for customizing and fine-tuning data are available for onscreen reports.
Page 224: Close Reports
ASAP 2020 Confirm Close Reports Close Reports This option enables you to close all open report windows at one time. This avoids having to select close on each report window. Open Report Enables you to open a report that was saved from the Report window.
Page 225: Spc Report Options
SPC Report Options ASAP 2020 Confirm SPC Report Options When you select SPC Report Options, the SPC Report Options dialog is displayed. The SPC Report Options dialog lists the variables that are most frequently used for SPC reporting. You can check as many as desired. All variables selected are computed for each sample file used in an SPC report.
Page 226: Regression Report
ASAP 2020 Confirm Regression Report Regression Report Select this option to generate a regression report. The regression report is used to determine the interdependency between two variables. Up to three dependent variables (Y-axis) may be plotted against a single independent variable (X-axis). The degree of correlation between the variables also is reported.
Page 227 Regression Report ASAP 2020 Confirm X- and Y-Axes Allows you to designate the X- and Y-axes variables. Click Variable fields on the down arrow to display a list of variables. The variables in this list are the ones you specified in the SPC report options.
Page 228 ASAP 2020 Confirm Regression Report Category Enables you to change the files shown in the files list by SubCategory selecting another directory. Status Enables you to limit the files shown in the files list to those of a selected status. Refer to Table 2-2.
Page 229 Regression Report ASAP 2020 Confirm Preview Enables you to specify the report destination. Print The Export options is not available for an Analyst. Export text Saves the current definition of the report as the default. Save As Default Generates the report.
Page 230: Control Chart
ASAP 2020 Confirm Control Chart Control Chart This option enables you to generate a control chart report which plots the changes in a statistic. Select this option to have a title display on your report. Show report title Accept the default or enter a new title. You can enter up to 40 alphanumeric characters.
Page 231 Control Chart ASAP 2020 Confirm Displays the Control Chart Graph [n] Options dialog, Graph [n] allowing you to define the Y-axis of each graph. Statistic This drop-down list displays the SPC variables selected on the SPC Report Options dialog. The variable you choose will be plotted against time.
Page 232 ASAP 2020 Confirm Control Chart Displays the Control Chart Sample Selection dialog, allowing Samples you to choose the sample files on which you wish to report. This dialog functions in the same manner as the Regression Report Sample Selection Dialog. Refer to Regression Report, page 6-8.
Page 233: Heat Of Adsorption
Heat of Adsorption ASAP 2020 Confirm Heat of Adsorption The isosteric heat of adsorption is an important parameter for characterizing the surface het- erogeneity, providing information about the adsorbent and the adsorption capacity. Multiple adsorption isotherms are obtained on the same sample using the same adsorptive but at dif- ferent temperatures to obtain the heat of adsorption.
Page 234 ASAP 2020 Confirm Heat of Adsorption Edit Quantities Displays the Edit Quantities Adsorbed dialog so that you can specify the range of surface coverage to include in the heat of adsorption report. Quantity Adsorbed Allows you to enter the points.
Page 235 Heat of Adsorption ASAP 2020 Confirm Clears the entire table of all entries except one; one is Clear required. Load Table Allows you to import a previously saved table. Save Table Allows you to save the current table as a file (QNT extension).
Page 236: Rate Of Adsorption (Roa)
ASAP 2020 Confirm Rate of Adsorption (ROA) Print Select this option to have reports generated to the system printer. When you choose this option, the Copies field is enabled allowing you to print up to four copies. Export Choose this option to export data in ASCII format to a file.
Page 237: Printed Reports
Printed Reports ASAP 2020 Confirm Printed Reports Header All printed reports (either to the screen or to a printer) contain a header displaying file statistics. • Tabular and graphical reports contain sample and instrument statistics such as when the file was created and by whom, date and time of analysis, analysis conditions, and so forth.
Page 238: Tool Bar
ASAP 2020 Confirm Onscreen Reports Tabs display for each type of report you choose to generate. Header List of reports requested Displays graphical (or tabular) data Options on Tool Bar Tool Bar Reports Contains a list of all requested reports.
Page 239 Onscreen Reports ASAP 2020 Confirm Delete Deletes the selected report. A deletion confirmation dialog is displayed since this function cannot be undone. The deleted report(s) will have to be regenerated if deleted in error. Hide Hides (removes) the selected report from the report window.
Page 240 ASAP 2020 Confirm Onscreen Reports Save Saves all reports of the currently open file in a report format using the same name as the sample file, only with an rep extension. If you wish to specify a name and/or specific reports to save, use the push button.
Page 241 Onscreen Reports ASAP 2020 Confirm Graph border line Enables you to specify a thickness for the border of the thickness graph. Load Loads the last saved defaults. Save Saves the changes as the defaults. If you do not click Save the changes will apply to the current report set only.
Page 242: Shortcut Menus
ASAP 2020 Confirm Onscreen Reports Shortcut Menus Shortcut menus are accessed when you right-click on the tabular or graphical portion of a report. Tabular Reports Resize column Displays a dialog so that you can specify the width of the selected column (in inches).
Page 243: Graphs
Onscreen Reports ASAP 2020 Confirm Edit title Allows you to edit the table title and font. Copy table as text Enables you to copy the entire table (column headers and data) and then insert it into another program. Columns are...
Page 244 ASAP 2020 Confirm Onscreen Reports Edit curve Displays the Curve Properties dialog, allowing you to edit curve properties. Title Displays the title of the curve you are editing. You can edit the title if desired. Style This drop-down list contains the styles in which collected data can be displayed.
Page 245: Zoom Feature
Onscreen Reports ASAP 2020 Confirm Title group box Displays the title of the axis you have selected to edit; you can edit the title if desired. You can also choose a different font. Scale group box The options in this group box allow you to edit the scale as well as its font.
Page 246: Axis Cross Hair
Report Examples The remainder of this chapter contains samples of some of the reports that can be generated by the ASAP 2020 Confirm Program. Most of the reports can be varied through entries on the report options screens. 6-28...
Page 247: Tabular Report
Report Examples ASAP 2020 Confirm Tabular Report This is the first page of a tabular isotherm report. 202-42811-01 - Mar 2008 6-29...
Page 248: Isotherm Plot
ASAP 2020 Confirm Report Examples Isotherm Plot 6-30 202-42811-01 - Mar 2008...
Page 249: T-Plot
Report Examples ASAP 2020 Confirm t-Plot This is an example of the t-Plot using Harkins and Jura as the thickness curve. 202-42811-01 - Mar 2008 6-31...
Page 250: Bet Surface Area Plot
ASAP 2020 Confirm Report Examples BET Surface Area Plot 6-32 202-42811-01 - Mar 2008...
Page 251: Bjh Adsorption
Report Examples ASAP 2020 Confirm BJH Adsorption This example shows the cumulative pore volume overlaid with the dV/dw Pore volume. 202-42811-01 - Mar 2008 6-33...
Page 252: Summary Report
ASAP 2020 Confirm Report Examples Summary Report 6-34 202-42811-01 - Mar 2008...
Page 253: Options Report
Report Examples ASAP 2020 Confirm Options Report This example is page 1 of an Options report. 202-42811-01 - Mar 2008 6-35...
Page 254: Sample Log Report
ASAP 2020 Confirm Report Examples Sample Log Report 6-36 202-42811-01 - Mar 2008...
Page 255: Options Menu
Description ASAP 2020 Confirm 7. OPTIONS MENU The choices on the Options menu allow you to configure the system to your laboratory’s requirements. With the options on this menu, you can: • Add directories • Edit labels for sample files and directories •...
Page 256: Add Archive Location
Page 7-6. Service Test Mode Enables you to perform certain troubleshooting procedures. under the direction of a Micromeritics service representative. Page 7-6. Add Archive Location Archive locations (directories) can be added by an Analyst or a Developer; the Add Archive Location dialog box is displayed.
Page 257: Edit Labels
Edit Labels ASAP 2020 Confirm Sequence number Allows you to enter a new sequence number for the directory you create. This number is incrementally sequenced for each sample file you create and displays as part of the identifica- tion if the sample template includes a $ symbol.
Page 258: Update File List
ASAP 2020 Confirm Update File List Update File List This function cannot be performed by an Analyst nor a Developer, unless the Developer has Administrator rights. This is an Administrator function only; details for performing this oper- ation are covered in the Administrator’s Guide.
Page 259: Graph Grid Lines
Graph Grid Lines ASAP 2020 Confirm Graph Grid Lines Graph Grid Lines enables you to choose the type(s) of grid lines to show on your reports; the Graph Grid Lines dialog is displayed. X-Axis Enables you to choose Major and/or Minor lines to...
Page 260: Live Graph
Various service tests are included in the ASAP 2020 operating program. These tests can be performed only with the assistance of a trained Micromeritics service representative. When you select Options > Service Test Mode, a dialog prompting you to enter a password is dis- played.
Page 261: Troubleshooting And Maintenance
Troubleshooting ASAP 2020 Confirm 8. TROUBLESHOOTING AND MAINTENANCE The ASAP 2020 system has been designed to provide efficient and continuous service. How- ever, to get the best results over the longest period of time, certain maintenance procedures must be followed. This chapter includes troubleshooting information, recommended preven- tive maintenance procedures, and routine maintenance procedures.
Page 262 ASAP 2020 Confirm Troubleshooting Table 8-1. Troubleshooting Chart (continued) What Happened What To Do Vacuum gauge shows Cold trap obstructed by Refer to Cleaning the Cold Trap reading above 20 condensation. Tubes, page 8-15. mHg, even after Filter in port being used is dirty. Replace filter in port. Refer to...
Page 263: Preventive Maintenance
Table 8-2 lists the preventive maintenance procedures you should perform to keep your ana- lyzer operating at peak performance. Instructions for each procedure follow the table. Micromeritics recommends that you perform these procedures as indicated, as well as by one of our service representatives every 12 months.
Page 264 **After about 12 to 18 months of operation, the diaphragm in the pump will wear out and become completely inoperable. To prevent any instrument downtime due to an inoperable pump, it is recommended that you have the diaphragm replaced by a Micromeritics Service Representative every 12 months.
Page 265: Lubricating The Elevator Screw
Preventive Maintenance ASAP 2020 Confirm Lubricating the Elevator Screw Apply a light coat of lithium grease to the elevator screw as needed. Checking the Analysis Port Dewar When handling Dewars, be sure to observe the Dewar precautions (refer to Precautions, page 3-25 Ice and suspended frost particles may accumulate in the bottom of the analysis port Dewar.
Page 266: Replacing The Sample Tube O-Ring
ASAP 2020 Confirm Preventive Maintenance Replacing the Sample Tube O-ring It is important to maintain a vacuum-tight seal near the top of the sample tube stem. If an O- ring becomes worn or cracked, it does not provide a good seal and will need to be replaced.
Page 267: Replacing The Port Filters
Preventive Maintenance ASAP 2020 Confirm 4. After the new O-ring is in place, insert the sample tube back into the sample port until it is fully seated. 5. Slide the sample tube connector nut up the tube (the ferrule and O-ring will move along with the connector nut).
Page 268: Degas Port
ASAP 2020 Confirm Preventive Maintenance Degas Port 1. Using a wrench, remove the degas port fitting and remove the filter and O-ring. 2. Replace the filter and the O-ring. Carefully reassemble the sample tube fitting, filter, O- ring and manifold connector, and tighten by hand. Then tighten with the wrenches to prevent leaks when evacuated.
Page 269: 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 manual for the vacuum pump for other acceptable oils.
Page 270 ASAP 2020 Confirm Preventive Maintenance 3. Disconnect the vacuum pump power cord from its power source. Always drain the vacuum pump while the pump is warm and switched off (unplugged). 4. Disconnect the vacuum pump hose from the top of the vacuum pump.
Page 271 Preventive Maintenance ASAP 2020 Confirm 8. Check the washer or O-ring used at the oil-filling port; replace if necessary. Replace the oil-fill plug. 9. Place the vacuum pump back into the analyzer onto the drip tray and reconnect the vacuum pump hose.
Page 272: Replacing The Alumina In The Oil Vapor Traps
ASAP 2020 Confirm Preventive Maintenance Replacing the Alumina in the Oil Vapor Traps The activated alumina in the oil vapor traps becomes saturated during use. The alumina should be replaced if any of the following conditions exist: • The alumina has been used for a three-month period.
Page 273 Preventive Maintenance ASAP 2020 Confirm 4. Remove the traps by opening both vacuum clamps and separating the trap from the vacuum pump and hose connections. Hose Hose Fitting Centering Ring Clamp Oil Vapor Trap (optional) Clamp Centering Ring Intake 5. Remove one end fitting from each trap body.
Page 274 ASAP 2020 Confirm Preventive Maintenance 7. If the trap body interior appears oily or dirty, wash it with isopropyl alcohol or ethyl alcohol and dry it thoroughly. Exposure of the trap body to oil vapor may cause small cracks on the inside surface of the trap body.
Page 275: Cleaning The Cold Trap Tubes
Preventive Maintenance ASAP 2020 Confirm Cleaning the Cold Trap Tubes Oil vapor from the vacuum pumps accumulates in the cold trap. Clean the tubes as follows: 1. Place the analyzer ON/OFF switch in the OFF position and turn off the vacuum forepumps.
Page 276: Calibrating The Manifold Temperature Sensor
ASAP 2020 Confirm Preventive Maintenance Calibrating the Manifold Temperature Sensor You should calibrate the manifold temperature on an annual basis. This allows you to correct for any changes in the manifold temperature sensor that occur with time. You will need a small diameter probe, such as a 1/16-in. (1.5-mm) thermocouple to calibrate the manifold temperature sensor.
Page 277: Performing A Leak Test
Preventive Maintenance ASAP 2020 Confirm Performing a Leak Test This procedure may be performed at the request of your service representative to determine if there is a leak in your system This test generates a report that your service representative will request that you send to him for observation.
Page 278 ASAP 2020 Confirm Preventive Maintenance 4. Click ; the second view of the Service Test dialog is displayed. Next Data will be inserted into the pane as collected. 5. After the test is finished, a dialog stating the test is complete is displayed.
Page 279 Preventive Maintenance ASAP 2020 Confirm 8. Click ; the Save As dialog is displayed. Save as 9. Accept the default name displayed in the File name field, then click to return to the Save report window. 10. Click to close the report window.
Page 280: Routine Maintenance
ASAP 2020 Confirm Routine Maintenance Routine Maintenance The procedures in this section are performed as needed. Cleaning the Analyzer The ASAP 2020 should be cleaned every six months, or sooner if required. Clean the outside casing of the analyzer (except for the shields) with a clean cloth dampened with isopropyl alcohol (IPA), a mild detergent in water, or a 3% hydrogen peroxide solution.
Page 281: Calibrating The Pressure Scale
Routine Maintenance ASAP 2020 Confirm 3. When the calibration is complete, click to close the dialog. You may cancel a calibration at any time by selecting Cancel. If you cancel a calibration, no new calibration data are saved. Calibrating the Pressure Scale Calibration, Pressure scale allows the software to adjust the gain of the selected transducer to match a reference standard.
Page 282: Cleaning And Verifying The Gas Line
ASAP 2020 Confirm Routine Maintenance Cleaning and Verifying the Gas Line You should always clean the gas lines and verify there are no leaks at the connections after you connect a gas bottle. This test examines the gas line from the instrument to the gas bottle. A report is generated at the completion of the test verifying that it has passed or failed.
Page 283 Routine Maintenance ASAP 2020 Confirm 4. Click ; the second view of the Service Test dialog is displayed. On this dialog a series Next of messages is displayed. These messages are of the following types: • Informative; for example, advising how long the test will take or how long before you will be required to open or close a valve.
Page 284 display Passed, indicating that the gas line from the instrument to the gas bottle is clean and leak-free. If Failed is shown, a leak is indicated between this connection. Check the connections from the instrument to the gas bottle. Tighten as necessary, then try the test again. 7.
Page 285: Ordering Information
The ASAP2020 system components and accessories can be ordered using one of the follow- ing method: • Call our Customer Service Department at (770) 662-3636 • Email orders to orders@micromeritics.com • Contact your local sales representative When ordering, please use the information provided in this chapter to place your order.
Page 286 ASAP 2020 Confirm Ordering Information Part Number Item and Description 004-25103-00 Ferrule, front, Teflon 1/4 in. 004-25104-00 Ferrule, rear, Nylon 1/4 in. 290-25846-00 Copper tube, for gas inlet, 1/8-in. diameter, 6 ft. long 290-25846-01 Same as 290-25846-00, but uses 16-ft. (5m) tubing 004-25549-00 Reducer, 1/8-in.
Page 287 Ordering Information ASAP 2020 Confirm Part Number Item and Description 200-25840-00 Saturation pressure tube, includes isothermal jacket 250-25608-00 Valve gasket, Kel-F, for analysis manifold 250-25627-00 Valve plunger, Buna-N seal, for analysis manifold 201-22600-00 Valve spring, for Buna-N plunger, for analysis manifold...
Page 288: Sample Tubes And Components
ASAP 2020 Confirm Ordering Information Sample Tubes and Components 1/4-in., 3/8-in, and 1/2-in Sample Tubes Part Number Item and Description Sample Tubes and Components 004-25466-00 O-ring, size 010, Buna-N; for 1/4-in. sample tube 004-25465-00 O-ring, size 010, Kalrez; for 1/4-in. sample tube 004-25022-00 O-ring, size 012, Buna-N;...
Page 289: 22-Mm Sample Tube Kit
Ordering Information ASAP 2020 Confirm Part Number Item and Description 300-25824-00 Nut, sample tube 004-32604-00 Cap (stopper), for 1/4-in. sample tube (not shown) 004-32004-00 Stopper, for 3/8-in. sample tubes 240-32000-00 Stopper, for 1/2-in. sample tube 260-25890-00 Seal Frit with built-in check valve for air-sensitive samples 202-25901-00 Isothermal jacket, 1/4 in.
Page 290: Cold Trap Tubes And Components
ASAP 2020 Confirm Ordering Information Cold Trap Tubes and Components Part Number Item and Description Cold Trap Tube and Components 004-25469-00 O-ring, Buna-N, size 014 004-25979-00 Nut, cold trap 004-61063-00 Tube, 1/2-in. OD stem, cold trap 202-42811-01 - May 2012...
Page 291: Forms
ASAP 2020 Confirm Appendix A A. FORMS This appendix contains the following form: • Sample Data Worksheet Copy and use this form as needed. 202-42811-01 - Oct 2003...
Page 293: Asap Series Sample Data Worksheet
ASAP Series Sample Data Worksheet This form is provided to assist you in obtaining an accurate sample mass for report calculations. You may use the After Degas value (Step 5) or the After Analysis value (Step 7), provided they are close to the same.
Page 295: Error Messages
Action: Restart the computer. If the problem persists, reinstall the application (this will not affect any of your sample files). If the problem continues, contact a Micromeritics service representative. 2331- Logged-in Windows user is not an application user. Cause: You attempted to log into the application but the user logged into Win- dows is not an application user.
Page 296 ASAP 2020 Confirm Appendix B 2332- Logged-in Windows user is not an administrator. Cause: You attempted to perform a task that can only be accomplished by someone with administrator rights. Contact your administrator or someone with administrator rights to Action: perform the task.
Page 297 Appendix B ASAP 2020 Confirm 2336- This user account is locked. Please contact administrator. Cause: You entered an incorrect password more than the allowed number of times (by default, this is three), and your account has been locked (dis- abled).
Page 298 ASAP 2020 Confirm Appendix B 2341- Error writing file or the user is not Windows OS user. Cause: You attempted to log into the application but have been denied access. Your password file may have become corrupt. Action: Contact your Administrator.
Page 299 Appendix B ASAP 2020 Confirm 2346- This user account is disabled. Please contact an administrator. Cause: You have attempted to log into the application repeatedly but all attempts have failed. Action: Contact your Administrator. 202-42811-01 - Mar 2011...
Page 300: 2400 Series
ASAP 2020 Confirm Appendix B 2400 Series 2401- FATAL ERROR: (error message). Cause: An internal processing and/or hardware error has occurred. Action: Contact your service representative if you continue to receive this error message. 2430- Error accessing file (file name), error code = (number).
Page 301 Appendix B ASAP 2020 Confirm 2432- Invalid response from MMI ‘FILE_READ’ request. Cause: An internal processing and/or hardware error has occurred. Action: Contact your service representative if you continue to receive this error message. 2433- New entries have been found in this directory. Refresh the directory...
Page 302 ASAP 2020 Confirm Appendix B 2437- File (file name) does not exist. Cause: You entered a file specification that does not exist. Action: Enter an existing file specification or select a file name from the list box. 2438- Disk drive (letter): is inaccessible.
Page 303 Appendix B ASAP 2020 Confirm 2450- Sample Defaults may not be edited while this operation is in progress. Do you wish to save and close the Sample Defaults edit session? Cause: You are in the process of initiating an automatic analysis (an analysis in which sample files are created using the defaults) while editing the defaults.
Page 304 ASAP 2020 Confirm Appendix B 2457- Results cannot be displayed. More than (number) windows are currently dis- playing or printing results. Cause: You have too many windows open in the application. Action: Close some of the open windows. 2458- An instrument is performing a critical operation. Wait a few moments before exiting the application.
Page 305 Appendix B ASAP 2020 Confirm 2461- No instruments are in operation. This application will unconditionally terminate. Cause: At least one analyzer must be active for the application to operate. The initialization of the analyzers configured with the Setup program has failed.
Page 306 Action B: Reinstall the software, then restart application. Action C: Contact your Micromeritics service representative if you continue to get this message. 2478- Error copying sequential data segment. Cause: An internal processing and/or hardware error occurred while accessing a portion of a sample file.
Page 307 Appendix B ASAP 2020 Confirm 2479- (Unit n; Serial nn) The instrument is busy performing an operation of which this application is unaware. Do you want to cancel? (Yes, No) Cause: During initialization of the application, the status of the analyzer was found to be in a different state than expected.
Page 308 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 309 Appendix B ASAP 2020 Confirm 2488- File (file name) cannot be opened for editing. It is already in use. Cause: The file you specified is being used in another edit operation. Action: Check the Windows list to locate the other edit session.
Page 310 ASAP 2020 Confirm Appendix B 2494- Value is out of the valid range. 2495- Value is out of the valid range. Enter a value between (value) and (value). Cause: The value you entered in the highlighted field is outside the valid range of values.
Page 311: 2500 Series
Appendix B ASAP 2020 Confirm 2500 Series 2500- All sample file names that can be created using the sequence number pattern already exist. You may want to modify the next sequence number. Cause: No more sample information files can be created using the currently entered file name sequence number.
Page 312 ASAP 2020 Confirm Appendix B 2504- Cannot create output file for sample (sample name). Cause: Insufficient space may be available on the hard disk. Action: Ensure that sufficient space is available. Contact your service repre- sentative if you continue to receive this error message.
Page 313 Appendix B ASAP 2020 Confirm 2510- (sample file) Error parsing reports from file (name). Reports cannot be produced. Cause A: One or more data entry fields in the sample file may contain an invalid character (such as a single quote or double quotes).
Page 314 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 315 Appendix B ASAP 2020 Confirm 2521- Unable to program controller. Cause: A hardware malfunction has occurred. Action: Contact your local Micromeritics service representative. 2522- Invalid controller application file. Cause: The application’s control file has been corrupted or deleted. Action: Reinstall the ASAP 2020 analysis program.
Page 316 The directory (name) has already been added to the repository. Cause: An internal conflict with the repository structure has occurred. Action: Contact your Micromeritics service representative. 2538- The archive location name (name) has already been used. Cause: An internal conflict with the repository structure has occurred.
Page 317 Appendix B ASAP 2020 Confirm 2539- The repository location (name) cannot be created. Cause: You attempted to create a new directory (category) or subdirectory (sub-category) but the directory-creating function of the Windows operating system has prevented you from doing so.
Page 318 ASAP 2020 Confirm Appendix B 2544- Cannot write to the repository. Check that the directory permissions are correct Cause: The system has prevented you from saving your file to the repository. Action: Contact your Administrator to review user rights for the application and the Windows operating system.
Page 319: 4000 Series
Appendix B ASAP 2020 Confirm 4000 Series 4000- Memory Allocation Error. Cause: An internal processing and/or hardware error occurred during report generation. Action: Contact your service representative if you continue to receive this error message. 4002- Thermal Transpiration correction had no effect.
Page 320 ASAP 2020 Confirm Appendix B 4006- Report Type Not Found. 4007- Error Processing Report. Cause: An internal processing and/or hardware error occurred during report generation. Action: Contact your service representative if you continue to receive this error message. 4008- Report requested on sample file with no data points.
Page 321 Appendix B ASAP 2020 Confirm 4011- Analysis gas in sample file does not match any gas in unit. Cause: You attempted to start an analysis using a sample information file in which the analysis gas specified does not match the analysis gas entered in the unit configuration.
Page 322 ASAP 2020 Confirm Appendix B 4015- Error creating export file for sample <sample file name>. Cause: A file error occurred during creation of an export output file. Action: The output file name may be invalid. Ensure that the target directory exists.
Page 323 Appendix B ASAP 2020 Confirm 4020- Disabling this option may damage the instrument. Are you sure that the sample should not be backfilled? Cause: You did not select Backfill sample at start of analysis on the Sample Backfill Options dialog. The sample tube is normally at atmospheric pressure when an analysis is started;...
Page 324 ASAP 2020 Confirm Appendix B 4023- The file (sample file) cannot be prepared for analysis. It is open for editing and contains errors. Cause: You attempted an analysis using a sample file that is being edited and has invalid values in one or more of its fields.
Page 325 Appendix B ASAP 2020 Confirm 4028- Dubinin calculations cannot be performed because the affinity coefficient of the analysis gas is zero. Cause: Dubinin values could not be calculated because the affinity coefficient of the analysis gas is zero. Action: Access the Dubinin Report Adsorptive options in the sample file and enter an appropriate value for the analysis gas.
Page 326 ASAP 2020 Confirm Appendix B 4033- Not enough points to generate Dubinin Tabular Report. Cause: There are fewer than two data points selected for the Dubinin tabular reports. Action: Examine the calculation assignments in the Collected Data dialog of the sample file. You must have at least two micropore pressures selected for inclusion in the Dubinin report.
Page 327 Appendix B ASAP 2020 Confirm 4037- Computations failed while processing the primary data set. No reports will be produced. Cause: The preparation of data for reporting could not be successfully com- pleted. No Horvath-Kawazoe reports will be produced. This message will always be preceded with another one containing additional infor- mation.
Page 328 ASAP 2020 Confirm Appendix B 4040- The value of Qm computed from the Langmuir equation is too low. The pore size will not be computed for all data points. Cause: The Cheng/Yang correction to the Horvath-Kawazoe equation requires the value of the monolayer volume as calculated from the Langmuir equation.
Page 329 Appendix B ASAP 2020 Confirm 4043- 1.0 cannot be a starting or ending pressure for a geometric progression toward saturation. Cause: You selected to generate a pressure table from a geometrically pro- gressing range. Action: Change the 1.0 entered value.
Page 330 ASAP 2020 Confirm Appendix B 4048- Warning: An error occurred while restoring the heat of adsorption report editor. Cause: The state of the heat of adsorption report editor could not be restored. Default settings will be used. Action: No action.
Page 331 Appendix B ASAP 2020 Confirm 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 332 ASAP 2020 Confirm Appendix B 4056- The Langmuir surface area could not be calculated. Cause: Fewer than two points were assigned to the requested surface area cal- culation in the collected data table. Action A: Assign more points to the surface area calculation.
Page 333 4062- Error during report generation. Cause: An internal processing error has occurred. Action: Contact your Micromeritics service representative. 4063- The data requested on this report are not available. Cause: There is no information in the sample log to report. Action: You selected a sample file for which no instrument operations have been used.
Page 334 ASAP 2020 Confirm Appendix B 4067- No data points are within the range of pressures in the reference isotherm. Cause: Thre are no collected data points within the range of pressures in the reference isotherm. Action: Select data points that are in the range of the reference isotherm, or select a more appropriate reference isotherm.
Page 335 Appendix B ASAP 2020 Confirm 4071- The selected pressures points do not form a valid set for deconvolution. Cause: The data points selected for analysis do not contain enough informa- tion to allow a DFT Plus data reduction. Action A: Edit data points in the table of the Collected Data dialog, or select another sample file.
Page 336 ASAP 2020 Confirm Appendix B 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 337: 6200 Series
Appendix B ASAP 2020 Confirm 6200 Series 6201- ‘GetOpenFile()’ reports error code (number). File selection cannot be made. Cause: You specified a file name which does not exist. Action: Confirm that the file name used is valid and that the file exists.
Page 338 An error occurred creating the ROA data file (file name). The error code was (n). Cause: A software error occurred when the file was being created. Action: Contact your Micromeritics service representative. 6209- Analysis startup failed. (Secondary message number and text.) Cause: The ASAP 2020 Program was unable to start an analysis with the indi- cated unit.
Page 339 Appendix B ASAP 2020 Confirm 6235- (Unit [number]) Analysis canceled: Time limit exceeded while dosing Psat tube to 925 mmHg. Cause A: A pressure of 925 mmHg was not attained within the allowed time. The Psat gas regulator may be set too low or turned off.
Page 340 ASAP 2020 Confirm Appendix B 6241- (Unit [number]) Analysis canceled: Maximum time exceeded before the elevator reached the UP (or DOWN) position. Cause A: The maximum time for the analysis was exceeded before the elevator reached the UP (or DOWN) position. Ice may be present in the bottom or the neck of the Dewar.
Page 341: 6500 Series
The Pressure Gauge Calibration operation showed the transducer offset exceeds the recommended limit. Action: Repeat the Pressure Gauge Calibration operation, if this message occurs again contact a Micromeritics service representative. 6502- The 10 mmHg transducer offset exceeds recommended limits: (number) Cause: The Pressure Gauge Calibration operation showed the transducer offset exceeds the recommended limit.
Page 342 The Pressure Gauge Calibration operation showed the transducer offset exceeds the recommended limit. Action: Repeat the Pressure Gauge Calibration operation, if this message occurs again contact a Micromeritics service representative. 6504- Unable to write the calibration file (name). Cause: A Save to File operation failed.
Page 343 Dosing during an analysis did not come within the allowed range of the target. Action: Check that the outlet stage of the gas regulator is within specification. If the problem occurs frequently contact a Micromeritics service rep- resentative. 202-42811-01 - Mar 2011 B-49...
Page 344 ASAP 2020 Confirm Appendix B 6516- (Unit [number]) Analysis canceled: Sample pressure greater than (pressure) mmHg is not allowed. Cause: An absolute pressure greater than (pressure) mmHg was attained dur- ing Low pressure dosing (either fixed dose mode or incremental dose mode).
Page 345 Appendix B ASAP 2020 Confirm 6519- (Unit [number]) Analysis canceled: Psat gas is not condensing. Cause A: The working Dewar does not contain enough bath liquid. Action A: Retry the operation after filling the Dewar. Cause B: The Psat gas is contaminated.
Page 346 Cause: A manifold pressure over 1000 mmHg was detected. Action: Observe caution when operating the analyzer manually. If the problem persists contact a Micromeritics service representative. 6522- (Unit [number]) Analysis canceled: Time limit exceeded while evacuating man- ifold. Cause A: Maximum manifold evacuation time was exceeded before the vacuum set point was achieved.
Page 347 Appendix B ASAP 2020 Confirm 6524- (Unit [number]) Analysis canceled: Time limit exceeded while evacuating sam- ple (restricted). 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 348 A check of the 1000 mmHg gauge’s offset during an automatic oper- ation indicated it was too high. Action: If this message occurs repeatedly, contact a Micromeritics service rep- resentative 6529- Master pressure gauge offset is too high - [PR1] [PR-U].
Page 349 Evacuation during the manifold dosing operation did not come within the allowed range of the target. Action: Check that the outlet stage of the gas regulator is within specification. If the problem occurs frequently, contact a Micromeritics service rep- resentative. 202-42811-01 - Mar 2011 B-55...
Page 350 Allow the heating mantle to cool down (approximately 15- 30 minutes). Then exit the analysis program and turn off the analyzer. Wait a couple of minutes, then turn the instrument on and restart the program. If the problem recurs, contact your Micromeritics service representative. B-56...
Page 351 Appendix B ASAP 2020 Confirm 6540- Error thermocouple unplugged. Current= (no.), Target = (no.) Cause: The heater was enabled, but the thermocouple was unplugged. Action: Plug in the thermocouple and try again. 6541- Error: SmartVac is not in a valid state to check degas.
Page 353: Calculations
Appendix C ASAP 2020 Confirm C. CALCULATIONS Saturation Pressure (Po) Po method is selected by the user on the Po and Temperature Options dialog. It may be entered, measured, or calculated from temperature. If entered, Po = user entered value...
Page 354 ASAP 2020 Confirm Appendix C where saturation pressure for the I data point (mmHg) most previous measured saturation pressure before I data point (mmHg) first measured saturation pressure after the I data point (mmHg) calculated Po entered saturation pressure (mmHg)
Page 355: Free Space
Appendix C ASAP 2020 Confirm Free Space Free-space volumes are calculated using the following equations: ----------- -  ----- 1 –  ----------- -  ----- 1 –  – ----------------------- - ---------- – where: system manifold pressure before dosing helium onto sample (mmHg)
Page 356: Equations Of State
ASAP 2020 Confirm Appendix C Equations of State The ideal gas law relates pressure, volume, temperature, and quantity of gas. ------ - where = pressure = volume = temperature = a constant that depends on the units of n. For n in cm STP, R = P For n in moles, R = 8.3145 J mol...
Page 357: Quantity Adsorbed
Appendix C ASAP 2020 Confirm Quantity Adsorbed For the I dose, the quantity dosed is:     n P     – dosed i   dosed i 1 – The real gas equation of state is used to calculate n if compressibility information is available.
Page 358: Equilibration
ASAP 2020 Confirm Appendix C 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 pressure are calculated using the Savitzky-Golay convolution method for polynomial functions.
Page 359: Thermal Transpiration Correction
Appendix C ASAP 2020 Confirm Thermal Transpiration Correction During data reduction, thermal transpiration correction is applied to the data if the user selected Thermal transpiration correction from the Report Options dialog. Starting with the first collected pressure, the following calculations are performed until the pressure ratio (PC/ P) is greater than or equal to 0.99.
Page 360: Bet Surface Area
ASAP 2020 Confirm Appendix C BET Surface Area For each point designated for surface area calculations, the BET transformation is calculated as follows: --------------------------------------------- -   N  1.0 P – where B is in units of g/cm STP.
Page 361: Langmuir Surface Area
Appendix C ASAP 2020 Confirm Volume of the Monolayer (cm /g STP): ------------------- - ------------------ -  Error of the BET Surface Area (m /g):    -------------------------------------------------------------------- - Langmuir Surface Area For each point designated for surface area calculations, the Langmuir...
Page 362 ASAP 2020 Confirm Appendix C Langmuir Surface Area (m /g):     6.023 -----------------------------------------------------------------------------------------------      S  22414 cm where analysis gas molecular cross-sectional area (nm ), user-entered on the Adsorptive Properties dialog Volume of the Monolayer (cm...
Page 363: T-Plot
Appendix C ASAP 2020 Confirm t-Plot For each point designated for t-Plot calculations, the following calculations are done: Thickness for the I point (Å):  ------------------- - (Halsey   HJP1 HJP3 ------------------------------------------ - (Harkins and Jura   HJP2 –...
Page 364 ASAP 2020 Confirm Appendix C KJS1 = Kruk-Jaroniec-Sayari parameter #1 KJS2 = Kruk-Jaroniec-Sayari parameter #2 KJS3 = Kruk-Jaroniec-Sayari parameter #3 = relative pressure for the Ith point A least-squares analysis fit is performed on the (t ) data pairs where t...
Page 365: Bjh Pore Volume And Area Distribution
Appendix C ASAP 2020 Confirm BJH Pore Volume and Area Distribution For adsorption data, the relative pressure and volume adsorbed data point pairs collected dur- ing an analysis must be arranged in reverse order from which the points were collected during analysis.
Page 366: Calculations
ASAP 2020 Confirm Appendix C c. The walls of the cylindrical pore - the diameter of the empty pore is required to determine the pore volume and pore area. End area is neglected. pore wall Insignificant compared to core length...
Page 367 Appendix C ASAP 2020 Confirm The thickness of the remaining adsorbed layer at this relative pressure is calculated: ------------------   where HP1, HP2, and HP3 are Halsey Parameters 1, 2, and 3 (respectively) from the Halsey Thick- ness Equation dialog.
Page 368 ASAP 2020 Confirm Appendix C The annular cross-sectional area of the wall layer desorbed is calculated for all pre- viously opened pores: –  Rc   Tw   10   – The total volume of gas desorbed from walls of previously opened pores is calculated: ...
Page 369 Appendix C ASAP 2020 Confirm The Kelvin radius for the end of the interval is calculated as follows: – ---------------------------------------------- -       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.
Page 370 ASAP 2020 Confirm Appendix C c. 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 follows: 2 Td...
Page 371 Appendix C ASAP 2020 Confirm 3) Incremental Surface Area (SA /g): 2 – –  LP   10   D   10   m/cm 4) Cumulative Surface Area (SA /g): CUM(I)   for J 1...
Page 372 ASAP 2020 Confirm Appendix C 2) Cumulative Pore volume (VpF , cm /g): CUMI   INTERP DpF where INTERP(x) is the value interpolated from the function X = Dp and Y = , using an AKIMA semi-spline interpolation. CUMJ...
Page 373: Compendium Of Variables
Appendix C ASAP 2020 Confirm 8) dA/dD pore area (dA/dDpF /g-A):   dA/dDpF INTERP DpF where INTERP(x) is the value interpolated from the function X = D and Y = avgJ dA/dD 9) dA/dlog(D) pore area [dA/dlog(DpF ), m /g]: ...
Page 374: Horvath-Kawazoe
ASAP 2020 Confirm Appendix C Horvath-Kawazoe A relative pressure lower limit is determined such that L-d never equals zero. All pressure points less than this limit are discarded. For each collected relative pressure point, values of L are chosen in an iterative manner, and the relative pressure (P/Po) determined by solving one of the following equations: •...
Page 375: Cylinder Pore Geometry (Saito/Foley
Appendix C ASAP 2020 Confirm A   ----------------------------- - where: = molecular diameter (Å) from the Horvath-Kawazoe Physical Properties dialog = diameter of sample atom (Å) from the Horvath-Kawazoe Physical dialog pore width (nucleus to nucleus) (Å) equilibrium pressure (mmHg)
Page 376: Sphere Pore Geometry (Cheng/Yang
ASAP 2020 Confirm Appendix C – –    ------------------- -  ,   – – –     ------------------- - ,   – -- - radius of the cylindrical pore, Sphere Pore Geometry (Cheng/Yang) When you use the Cheng/Yang method, the following equation is solved for each value of P.
Page 377 Appendix C ASAP 2020 Confirm      * ------------- - -------------------------------------------- - , where ------------------ - ------------------ - –     – ------------------ - ------------------ - –     – ------------------ - ------------------ - –...
Page 378: Interaction Parameter
ASAP 2020 Confirm Appendix C Interaction Parameter The interaction parameter (IP) results from the following calculations: The Kirkwood-Muller dispersion coefficients -      6 MC -------------------------------------------- -   ----- ----- -     ...
Page 379: Additional Calculations
Appendix C ASAP 2020 Confirm Additional Calculations Based on the previous calculations, the following can be calculated: Adjusted Pore Width (Å): (Shell to Shell) – Cumulative Pore Volume (cm /g):  where density conversion factor (cm liquid/cm STP) on the Adsorptive...
Page 380: Interaction Parameter Components
ASAP 2020 Confirm Appendix C Interaction Parameter Components Table C-1. Interaction Parameters Interaction Bath Parameter Temperature Calculated Sample Type 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 381 Appendix C ASAP 2020 Confirm Carbon Dioxide = 3.23 = 4.567 x 10 (25 ºC) 5.45 x 10 (0 ºC) 7.697 x 10 (-78 ºC)  = 5.0 x 10  = 2.7 x 10 values are from van der Waal’s constant.
Page 382: Dubinin-Radushkevich
ASAP 2020 Confirm Appendix C Dubinin-Radushkevich The Dubinin-Radushkevich equation is as follows:  V      -------------- - – ------ -  where: volume adsorbed at equilibrium pressure (cm /g STP) the micropore capacity (cm /g STP)
Page 383 Appendix C ASAP 2020 Confirm Using the results of the above calculations, the following can be calculated: Monolayer Capacity (cm /g STP): Vo = 10 Error of Monolayer Capacity (cm /g STP): = Vo x (10 - 1.0) Micropore surface area (m /g): ...
Page 384: Dubinin-Astakhov
ASAP 2020 Confirm Appendix C Dubinin-Astakhov The Dubinin-Astakhov equation is a follows: V     -------- -  – ------ - E where volume adsorbed at equilibrium pressure (cm /g STP) the micropore capacity (cm /g STP) saturation vapor pressure of gas at temperature T (mmHg)
Page 385 Appendix C ASAP 2020 Confirm Using the results of the above calculations, the following can be calculated: Monolayer Capacity (cm /g STP): = 10 Micropore Volume (cm /g): = (V x D) where density conversion factor (cm liquid/cm STP) from the Adsorptive...
Page 386 ASAP 2020 Confirm Appendix C Maximum Differential Pore Volume (cm /g-nm): This value is also known as frequency of the mode 1/3N          --------------- - Max --------------- - ----- --------------- - –...
Page 387 Appendix C ASAP 2020 Confirm Equivalent Pore Width (nm): 1/3N   ---- - –    ---------------------------------------- -     – dV/dw Pore Volume (cm /g-nm):   – –      ...
Page 388: Mp-Method
ASAP 2020 Confirm Appendix C MP-Method For each point designated for MP-method calculations, the following calculations are done: Thickness for the I point (Å):  ------------------- -   (Halsey HJP1 HJP3 ------------------------------------------ -   HJP2 – (Harkins and Jura...
Page 389 Appendix C ASAP 2020 Confirm Remaining pore surface area for the I point (m /g): 6 –       – D 10 – ------------------------------------------------------------------------------ - –   10  – – where density conversion factor (cm...
Page 390: Freundlich Isotherm
ASAP 2020 Confirm Appendix C Freundlich Isotherm The Freundlich isotherm has the form: ----- - where quantity of gas adsorbed quantity of gas in a monolayer temperature-dependent constant temperature-dependent constant The pressure is absolute; typically, m > 1. In terms of quantity adsorbed,...
Page 391: Temkin Isotherm
Appendix C ASAP 2020 Confirm Temkin Isotherm The Temkin isotherm has the form,   ----- - -------- -  where quantity of gas adsorbed quantity of gas in a monolayer the differential heat of adsorption at zero surface coverage /RT}, where ...
Page 392: Dft (Density Functional Theory
ASAP 2020 Confirm Appendix C DFT (Density Functional Theory) The adsorption isotherm is known to convey a great deal of information about the energetic heterogeneity and geometric topology of the sample under study. The data of physical adsorp- tion have been used for many years as the basis for methods to characterize the surface area and porosity of adsorbents.
Page 393: Application To Surface Energy Distribution
Appendix C ASAP 2020 Confirm Application to Surface Energy Distribution Under certain conditions, an energetically heterogeneous surface may be characterized by a distribution of adsorptive energies. The conditions are that the sample is not microporous, i.e., that adsorption is taking place on essentially a free surface with no pore filling processes at least to about 0.2 relative pressure.
Page 394: Performing The Deconvolution
ASAP 2020 Confirm Appendix C 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,e) and q(p,H), which we call the kernel functions, are con- tained in numeric form as model isotherms.
Page 395: Heat Of Adsorption
Appendix C ASAP 2020 Confirm Heat of Adsorption The adsorption isostere is represented by   ----- ------ -   where = isosteric heat of adsorption = unknown constant The isosteric heat of adsorption, q, is determined by finding the slope of ln (P/P ) as a func- tion of 1/RT for a set of isotherms measured at different temperatures.
Page 396 ASAP 2020 Confirm Appendix C e. Micropore Volume See t-Plot calculations. Horvath-Kawazoe Maximum Pore Volume See Horvath-Kawazoe Calculations g. Horvath-Kawazoe Median Pore Diameter See Horvath-Kawazoe Calculations h. Dubinin-Radushkevich Micropore Surface Area See Dubinin-Radushkevich Calculations Dubinin-Radushkevich Monolayer Capacity See Dubinin-Radushkevich Calculations...
Page 397: Spc Report Variables
Appendix C ASAP 2020 Confirm SPC Report Variables Regressions 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 398: Control Chart Variables
ASAP 2020 Confirm Appendix C Control Chart Variables  y -------- - Mean  y Mean   – StdDev ----------------------------------- - – StdDev ------------------ - CoefVar Mean  PlusNSig Mean n StdDev  MinusNSig Mean n StdDev – C-46...
Page 399: Testing For Leaks
Appendix D ASAP 2020 Confirm D. TESTING FOR LEAKS This appendix contains general instructions for testing the ASAP 2020 and the SmartVac degasser (if installed) for leaks. If the analyzer successfully performs a blank tube analysis using nitrogen, you do not need to test for leaks.
Page 400 ASAP 2020 Confirm Appendix D 6. Select Show Instrument Schematic, then Enable Manual Control from the Unit menu. (For clarity, this illustration shows only the valve portion of the schematic.) Table D-1 lists descriptions of the analysis valves. Table D-1. Analysis Valve Descriptions...
Page 401 Appendix D ASAP 2020 Confirm 12. Open valves 10 and 11. 13. Open valve 8. 14. Open valve PV. 15. Allow the system to evacuate for a minimum of one hour; a four-hour or overnight evacuation is preferred. 16. Obtain the manifold outgassing rate: Use the pressure transducer with the lowest range.
Page 402: Valves 3 And P1 Through P6
ASAP 2020 Confirm Appendix D Valves 3 and P1 through P6 1. Open the regulator outlet valve for the gas connected to port 3. 2. Take a pressure reading; record it as P1 for valve 3. 3. Wait 10 minutes and take another pressure reading; record it as P2 for valve 3.
Page 403: Valves 1, 2, 8, 9, 10, 11, And Pv
Appendix D ASAP 2020 Confirm Valves 1, 2, 8, 9, 10, 11, and PV Valves 10 and 11 1. Open valve PV; wait 5 minutes (Valves PS and 5 should be open.). 2. Open valve 7; allow the system to evacuate to 10 mHg.
Page 404 ASAP 2020 Confirm Appendix D Valves 1, 2, and PV 18. Open valves 1 and 2. 19. Open valves 4, 5, and PS. 20. Allow the system to evacuate for 15 minutes. 21. Close valves 1 and 2. Valve PV should be closed; if not, close it.
Page 405: Degas Valves
Appendix D ASAP 2020 Confirm Degas Valves Perform the following steps to measure the degas manifold outgas rate. 1. Ensure that the degas system is idle. 2. Close the regulator outlet valve for the backfill gas. 3. Insert a plug (or attach a clean, empty sample tube) into each degas port.
Page 406: What To Do If You Detect A Leaking Valve
ASAP 2020 Confirm Appendix D What To Do If You Detect a Leaking Valve If you determine that a specific valve is leaking, remove differential pressure from the valve and continue testing the remaining valves for leaks. As an alternative, you may repair or replace the leaking valve after removing the differential pressure on the valve.
Page 407 Appendix D ASAP 2020 Confirm 3. Closely inspect the valve seat area for any debris which may cause another leak. Gasket Plunger 4. Reassemble the valve. • Reopen the helium supply if you are repairing the helium inlet valve. • Turn on the vacuum pump system if you are repairing a vacuum valve.
Page 408: Replacing Valves On The Degas And Gas Inlet Manifold
ASAP 2020 Confirm Appendix D Replacing Valves on the Degas and Gas Inlet Manifold 1. Backfill the manifold with nitrogen to approximately 800 mmHg. 2. Turn off the gas supply for the inlet valves. 3. Turn off the vacuum pump system for degas valves D5 and D6.
Page 409: Valve Data Test Sheet
Appendix D ASAP 2020 Confirm Valve Data Test Sheet Make a copy of this form to record pressure readings and outgassing rates when leak-testing system valves. VALVE(s) (1st pressure reading) (2nd pressure reading) OUTGASSING RATE Analysis Valves Manifold Gas inlet valve...
Page 411: Calculating Free-Space Values For Micropore Analyses
Appendix E ASAP 2020 Confirm E. CALCULATING FREE-SPACE VALUES FOR MICROPORE ANALYSES Many microporous materials, such as zeolites and activated carbons, trap and hold helium in their complex pore structures for many hours after being exposed to helium. Helium trapped in micropores can interfere with the analysis at low pressures, causing an “S”-shaped curve at...
Page 412 ASAP 2020 Confirm Appendix E To correct cold free space: where = calculated cold free space with sample present (in standard cm = cold free space measured for the empty tube (in standard cm = mass of the sample to be analyzed (in grams)
Page 413: Dft Models
ASAP 2020 Confirm Appendix F F. DFT MODELS Theories are developed by scientists in an attempt to explain a class of observed behavior. In the experimental physical sciences, theories are often expressed in terms of a model that can be visualized and described mathematically. Early models of physical adsorption were quite simple, both conceptually and mathematically, for very practical reasons —...
Page 414: Molecular Simulation Methods
Appendix F ASAP 2020 Confirm If the equilibrium distribution of the gas atoms near the surface could be described as a func- tion of pressure and the molecular properties of the components of the system, then a model could be constructed for the adsorption isotherm for the system. Modern physical chemistry provides several ways to calculate this distribution.
Page 415: Density Functional Formulation
ASAP 2020 Confirm Appendix F If the move results in a configuration of higher energy, a probability for that event is calcu- lated, and a random number between zero and one is generated. If the generated number is smaller than the probability of the event, then the move is accepted; otherwise, another par- ticle is selected and the process is repeated.
Page 416 Appendix F ASAP 2020 Confirm Figure F-1 shows the density profile for argon at a carbon surface as calculated by density functional theory for a temperature of 87.3 K and a relative pressure of about 0.5. Figure F-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.
Page 417 ASAP 2020 Confirm Appendix F Figure F-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 418 Appendix F ASAP 2020 Confirm Figure F-3. Model Isotherms for Some Larger Pore Widths Argon on Carbon at 87.3 K Figure F-4 shows model isotherms for pores in the micropore size range. Note the logarithmic scale for pressure. Figure F-4. Model Isotherms in the Micropore Size Range of Pore Width Argon on Carbon at 87.3 K...
Page 419: Models Included
ASAP 2020 Confirm Appendix F Pores of 4 Å width, barely larger than the argon atom (3.38 Å), fill at pressures below 1 mil- litorr. Pores below 15 Å fill before a monolayer is completed on the surface of the larger pores.
Page 420 Appendix F ASAP 2020 Confirm The surface energy is reported in terms of the effective Lennard-Jones interaction parameter, e, for the adsorptive/adsorbent pair divided by Boltzmann’s constant. The units are therefore Kelvins. N2 - Cylindrical Pores - Oxide Surface AR - Cylindrical Pores - Oxide Surface...
Page 421 ASAP 2020 Confirm Appendix F References: Mietec Jaroniec, Michal Kruk, James P. Olivier and Stefan Koch, “A 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 422 Appendix F ASAP 2020 Confirm N2 - Tarazona NLDFT, Esf = 30.0K Geometry: Cylinder Substrate: Oxide Category: Porosity Method: Nitrogen at 77 K 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, typ- ical for a silica or alumina surface.
Page 423 ASAP 2020 Confirm Appendix F This model is particularly useful for microporous carbon materials. The reported pore size range is from 3.5 to 250 angstroms. Reference: Jacek Jagiello and James P. Olivier. “A simple two-dimensional NLDFT model of gas adsorption in finite carbon pores. Application to pore structure analysis.,”...
Page 424 Appendix F ASAP 2020 Confirm Carbon Cylinder, multi-wall nanotube by NLDFT N2 - Argon Cylinder, multi-wall nanotube by NLDFT Ar - Geometry: Cylinder Substrate: Carbon Category: Porosity Method: Nitrogen at 77 K; Argon at 87K Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting functions and cylindrical pore geometry.
Page 425: Models Based On Classical Theories
ASAP 2020 Confirm Appendix F Models Based on Classical Theories Both surface energy distribution and pore size distribution may be evaluated using classical approaches to model kernel functions for use with equation (1) of the DFT Theory in the cal- culations appendix.
Page 426: Models Included
Appendix F ASAP 2020 Confirm Models Included Kelvin Equation with Halsey Thickness Curve N2 - Halsey Thickness Curve Geometry: Slit Substrate: Average Category: Porosity Method: Nitrogen at 77 K The kernel function is calculated using the Halsey equation with standard parameters: –...
Page 427: Kelvin Equation With Broekhoff-De Boer Thickness Curve
ASAP 2020 Confirm Appendix F 13.99   -------------------------------------------- -     0.034 – P/Po The nitrogen properties used in the Kelvin equation are: Surface tension = 8.88 dynes cm Molar density = 0.02887 g cm N2 - Harkins and Jura Thickness Curve...
Page 428 1. “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 429 ASAP 2020 Confirm Index INDEX Ar Carbon Finite Pores, As=6, 2D-NLDFT model, F-10 Ar Carbon Slit Pores by NLDFT model, F-10 Add archive location command, 7-2 AR Cylindrical Pores - Oxide Surface model, F-8 Add Log Entry push button, 4-6...
Page 430 Index ASAP 2020 Confirm Calibrate Vacuum Gauge dialog box, 5-30 Cryogen, 1-6, 3-26 Calibration Cumulative Reports, 4-63 details, 5-16 Curve Properties dialog, 6-26 file, loading, 5-25 Load from File, 5-25 pressure offset, 5-21, 8-20 Data pressure scale, 5-22, 8-21 selecting display...
Page 431 ASAP 2020 Confirm Index Dollimore-Heal Adsorption/Desorption report, 4-69 Exit command, 4-110 Dosing Options dialog, 4-25 Export command, 4-106 Dubinin Adsorptive Options dialog, 4-81 Import command, 4-105 Dubinin report, 4-80 List command, 4-104 pore volume, 4-83 Log in command, 4-109 tabular, 4-82...
Page 432 Index ASAP 2020 Confirm Harkins and Jura equation, 4-53 removing differential pressure, D-8 Heat of Adsorption dialog box, 6-15 Valve 9, D-5 Heat of Adsorption report, 6-15 Valves 10 and 11, D-5 Heating mantle Valves P1 through P6, D-4 connector, 2-4...
Page 433 ASAP 2020 Confirm Index N2 Cylindrical Pores - Oxide Surface, F-8 generating, 3-34 N2 Cylindrical Pores - Pillared Clay Surface, F-8 N2 DFT model, F-7 N2 Halsey Thickness Curve, F-14 Parameter file, 4-3, 4-97 N2 Harkins and Jura Thickness Curve, F-14, F-15...
Page 434 Index ASAP 2020 Confirm Regression Report Options dialog, 6-8 density, 4-8 Regression Report Sample Selection dialog, 6-9 determining amount to use, 3-19 Regulators, gas, 1-4 determining weight, 3-19 Replace push button, 2-11 preparing, 3-14 Report Sample Analysis command, 5-3 closing, 2-9, 6-6...
Page 435 ASAP 2020 Confirm Index Service Test command, 5-31 displayed on schematic, 5-11 Servo valve Template calibrating (Degasser), 5-30 creating, 3-1 Shortcut keys, 2-9 listing statistics, 3-31, 4-104 list of, 2-9 opening, 4-96 Shortcut menu, 2-8 printing contents, 3-30 graphs, 6-25...
Page 436 Index ASAP 2020 Confirm calibration details, 5-16 pressure, 5-11 Vacuum pump exhaust filter, replacing, 8-8 fluid, changing, 8-9 fluid, inspecting, 8-9 panel, 2-2 placement, 2-7 Validation report, 4-90 Valves degassing, 5-27 description, D-2 opening and closing, 5-9 system, 5-10 testing for...

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