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Micromeritics ASAP 2460, Operator'S Manual

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ASAP 2460 Operator’s Manual

Table of Contents 

246-42800-01 - Nov 2013                                

v 

Checking and Cleaning the Analysis Port Dewars. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-5
Replacing Analysis Port Filters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-5
Replacing a Sample Tube O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-7
Inspecting and Changing Vacuum Pump Fluid . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-9

Inspecting Fluid . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-9
Changing Fluid . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-10

Replacing the Alumina in the Oil Vapor Traps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-13
Cleaning the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-16
Checking the Analysis Manifold Outgassing Rate  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-17
Testing the Analyzer for Leaks  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-19
Replacing the Vacuum Pump Exhaust Filter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-19

Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-21

Changing Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-21

Guidelines for Connecting Gases to the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-21
Connecting a Gas Regulator to the Gas Supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-21
Connecting the Gas Delivery Tubing to the Analyzer   . . . . . . . . . . . . . . . . . . . . . . . .  7-23
Specifying Gas Ports  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-24

Cleaning and Verifying the Gas Line. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-25

Calibrating the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-27

Performing a Reference Material Analysis  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-27

8.

ORDERING INFORMATION

Analysis System Components and Accessories. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  8-1
Sample Tubes and Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  8-4

A. FORMS

Sample Data Worksheet. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  A-3

B. ERROR MESSAGES

2200 and 2400 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  B-1
2500 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  B-10
4000 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  B-17
6100 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  B-33
6200 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  B-34
6500 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  B-41

C. CALCULATIONS

Saturation Pressure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  C-1
Relative Pressure Calculations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  C-2
Equation of State  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  C-2
Quantity Adsorbed Calculations  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3

Free Space  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  C-4

Measured  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  C-4
Calculated. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-5

Summary of Contents for ASAP 2460

Page 1: ...ASAP 2460 Accelerated Surface Area and Porosimetry System Operator s Manual V2 01 246 42800 01 Jan 2014...

Page 2: ...ary form must reproduce the above copyright notice definition disclaimer and this list of conditions in documentation and or other materials provided with the distribution 3 Altered versions including...

Page 3: ...the following conditions 1 Certain products sold by MICROMERITICS are the products of reputable manufacturers sold under their respective brand names or trade names We therefore make no express or imp...

Page 4: ......

Page 5: ...re 1 11 Shortcut Menus 1 11 Shortcut Keys 1 11 Files 1 12 File Status and Description 1 12 File Name Conventions 1 13 Libraries 1 14 Menu Structure 1 15 Main Menu Bar 1 15 Window Menu 1 16 Help Menu 1...

Page 6: ...ing Sample Tubes 2 33 Filling Dewars 2 34 Precautions 2 34 Filling an Analysis Dewar 2 35 Performing an Analysis 2 39 Standard Analysis 2 39 Krypton Analysis 2 42 High Throughput Analysis 2 44 Micropo...

Page 7: ...ubinin Report Options 3 63 Tabular Report Options 3 64 Transformed Isotherm Plot Options 3 64 Pore Volume Options 3 66 MP Method Report Options 3 67 Tabular Report Options 3 68 Plot Options 3 69 User...

Page 8: ...ort Shortcut Menus 5 20 Report Header Shortcuts 5 20 Tabular Reports Shortcuts 5 21 Graph Shortcuts 5 22 Other On Screen Features 5 26 Zoom Feature 5 26 Axis Cross Hair 5 26 Report Examples 5 27 Isoth...

Page 9: ...uidelines for Connecting Gases to the Analyzer 7 21 Connecting a Gas Regulator to the Gas Supply 7 21 Connecting the Gas Delivery Tubing to the Analyzer 7 23 Specifying Gas Ports 7 24 Cleaning and Ver...

Page 10: ...phere Pore Geometry Cheng Yang C 28 Cheng Yang Correction C 29 Interaction Parameter C 30 Additional Calculations C 31 Interaction Parameter Components C 32 DFT Density Functional Theory C 34 The Inte...

Page 11: ...F 2 Density Functional Formulation F 3 Models Included F 7 Non Local Density Functional Theory with Density Independent Weights F 7 Non Local Density Functional Theory with Density Dependent Weights F...

Page 12: ...Table of Contents ASAP 2460 Operator s Manual viii 246 42800 01 Nov 2013...

Page 13: ...d instrument interface Chapter 2 OPERATIONAL PROCEDURES Provides step by step procedures for operating the system Chapter 3 FILE MENU Provides a description of the File menu options and field and butt...

Page 14: ...ons used in reports Appendix D FREE SPACE CORRECTION Provides a discussion of the free space measurements for the analyzer Appendix E MAINTAINING HIGH PURITY GASES Provides information on the importan...

Page 15: ...icons to identify notes of importance warnings and cautions Notes contain important information pertinent to the subject matter Warnings contain information to help prevent actions that may cause per...

Page 16: ...or concurrently and can perform analyses of at least 50 hours without refilling the dewars Each port can accept a range of sample tube neck diameters 1 4 3 8 or 1 2 in OD Analysis operations can be m...

Page 17: ...is started no other samples can be started until the set is complete Each analysis port is equipped with an elevator that raises and lowers the analysis bath fluid dewar automatically A removable shi...

Page 18: ...tion The FlowPrep is an independent unit and not controlled by the analysis program VacPrep 061 The VacPrep offers two methods for removing contaminants In addition to flowing gas it provides vacuum t...

Page 19: ...e with the computer Once communications are established it remains solid green ASAP 2460 Operator s Manual Controls Indicators and Connectors 246 42800 01 Aug 2013 1 7 Side Panel The side panel of the...

Page 20: ...may be used for helium Controls Indicators and Connectors ASAP 2460 Operator s Manual 1 8 246 42800 01 Aug 2013 Back Panel The back panel of the Master Unit contains the connectors described below Au...

Page 21: ...ined If power is lost to the instrument any data collected which is not transferred to the computer will be lost 3 Place the computer monitor and printer ON OFF switches in the OFF position 4 Place th...

Page 22: ...l pore volume From this window numerous reports are accessible from a dropdown menu including BET Surface Area Langmuir Surface Area t Plot Alpha S Method BJH Adsorption BJH Desorption Dollimore Heal...

Page 23: ...isted to the right of the menu item Another shortcut method of accessing a menu or function is to use the Alt key plus the underlined let ter in the menu command For example to access the File menu pr...

Page 24: ...F7 Tiles open windows F8 Opens the File Selector allowing you to start a report from a selected SMP file F9 Closes all open reports Alt F4 Exits the program If files are open with unsaved changes a pr...

Page 25: ...rogram Prepared Sample information files that have been used in a degassing operation but have not been used in an analysis This status is applicable only if using the SmartPrep degasser Preparing Sam...

Page 26: ...ple Information library folder on the left Then select the SMP file on the right and click Open The File Selector has powerful Windows features Windows can be resized by dragging the window border col...

Page 27: ...al information on each item Methods 2460 Data MTH Report Options 2460 Param RPO Sample Information 2460 Data SMP Sample Tube 2460 Param STB Menu Item Description File Use to create or open files Refer...

Page 28: ...windows Refer to Window Menu page 1 16 Help Use to access this operator s manual Micromeritics web page and tutorials Refer to Help Menu page 1 16 Window Menu Option Description Cascade Stacks open wi...

Page 29: ...des access to instructional tutorials Micromeritics on the Web Provides a link to the Micromeritics web page www Micromeritics com ASAP 2460 on the Web Provides an Internet link to additional 2460 inf...

Page 30: ...Using the Software ASAP 2460 Operator s Manual 1 18 246 42800 01 Aug 2013...

Page 31: ...to the screen printer or file and listing file statistics generating graph overlays Working with Interactive Reports When opening a sample file that contains data from a complete or in progress analy...

Page 32: ...at the bottom of the window shows Isotherm as the current choice To view another report or to view the sample information file click the dropdown arrow The choices in this list allow you to display th...

Page 33: ...ons are Drag the blue bars to increase or decrease the range of data included in the plot Press CTRL then left click the mouse on a data point in the Isotherm Linear Plot to include or omit the data p...

Page 34: ...lled with the values in the default method They can then be edited if necessary You can edit the default method to meet your laboratory s needs as described below 1 Go to Options Option Presentation a...

Page 35: ...available in the Sample tube dropdown list 8 In the Mass group box indicate if mass is to be manually entered by the operator Enter or calculated by the system Calculate Refer to Mass group box page...

Page 36: ...o the default method you can create methods to be used when creating a new sample file as described below 1 Go to File New and create a new Sample Information file 2 Go to File Save As Enter a new fil...

Page 37: ...5 If the file sequence numbers for this Method will differ from other Methods select the Use separate sequence number checkbox and enter the new sequence number in the text box 6 In the Sample file n...

Page 38: ...ation and parameter files Navigate to parameter windows by selecting the tabs across the top of the window Basic Displays the entire sample information file in a single window with no tabs across the...

Page 39: ...ox fields may have been renamed or may not display if modified in Options Default Method 6 In the Sample Tube dropdown list select a sample tube from the list or click Edit to specify a sample tube de...

Page 40: ...information in the User Parameters group box These are user definable parameters that can be entered and tracked along with other statistical process control data 10 Enter any pertinent information ab...

Page 41: ...ed format parameter files cannot be edited 1 Ensure that the Basic or Restricted option is checked in the Options Option Presentation menu 2 Go to File New Sample 3 Select a Method from the dropdown l...

Page 42: ...ns the desired parameters Select the file and click Replace 9 Click the Add Log Entry button to enter notes for the instrument log report Create entries that cannot be recorded automatically through t...

Page 43: ...the Sample Information library folder select a SMP file with a status of Complete Analyzing or Entered and click Open or double click the file name The interactive reporting window displays Refer to...

Page 44: ...s of Preparing Prepared or No Analysis 1 Go to File Open or use the F2 keyboard shortcut 2 From the Sample Information library folder select a SMP file with a status of Preparing Prepared or No Analys...

Page 45: ...or s Manual Defining Sample Information Files 246 42800 01 Aug 2013 2 15 3 The Sample Description window displays in the specified format Advanced Basic or Restricted The following window is shown in...

Page 46: ...ime an analysis is performed Predefined parameter files are included with the program and can be edited as needed or new parame ter files can be created The Replace button can be used to overwrite val...

Page 47: ...othermal jacket and or filler rod will be used by selecting the Use isothermal jacket checkbox and or User filler rod checkbox Filler rods help to ensure accuracy in samples with lower total surface a...

Page 48: ...Select the Degas Conditions library folder and enter a file name in the File name field 2 Click Open 3 Click OK when prompted to create a new file Degassing is a required step in preparation for the a...

Page 49: ...DEG file containing the new parameters and click Open 5 Use the Insert button to enter up to five stages of degassing soak temperature ramp rate and soak time When using the SmartPrep degasser the max...

Page 50: ...s page 2 21 and Analysis Conditions Files page 3 15 6 Use the Insert Range button to enter starting and ending relative pressure points 7 Select the Absolute pressure dosing checkbox to specify pressu...

Page 51: ...e analysis 1 Go to File Open Select the Adsorptive Properties library folder and enter a file name in the File name field 2 Click Open 3 Click OK when prompted to create a new file 4 Enter a descripti...

Page 52: ...pt the defaults in the following fields Maximum manifold pressure Non ideality factor Density conversion factor Thermal transpiration hard sphere diameter Molecular cross sectional area Adsorbate mole...

Page 53: ...s Report options files may contain tabular reports plots or both as well as user defined report tables Report Options files may be defined to include overlay options The system allows the overlay of u...

Page 54: ...the report title in the text box 6 To display a graphic on the report header select the Show report title checkbox and enter the report title in the text box Click the Browse button to locate a BMP o...

Page 55: ...kPa Absolute Pressure mbar Quantity Adsorbed mmol g Quantity Adsorbed cm g STP Quantity Adsorbed cm3 g STP Sample ASCII text file To import the ASCII text file 1 Go to File New Sample and open a new s...

Page 56: ...Open The isotherm data from the original sample file is imported and displays in the new sample file If an error message appears instead verify that the TXT file format listed above is correct Copying...

Page 57: ...open a new sample information file 5 On the Sample Description window select Manually entered in the Type of Data group box 6 In the dropdown list at the bottom of the window select Isotherm 7 Resize...

Page 58: ...iller rods if used Ensure the detergent is dissolved before placing the sample tubes and filler rods into the water If too much detergent is used it may be difficult to rinse from the sample tubes Tas...

Page 59: ...d filler rods from the unit 6 Clean the interior of the sample tubes with the brush supplied with the system 7 Rinse the sample tubes and filler rods thoroughly with hot water Then rinse again with is...

Page 60: ...or TranSeal before degas weigh the Sample Tube Set with sample before degas and subtract from the weight of the empty Sample Tube Set weigh the Sample Tube Set with sample after degas and subtract fr...

Page 61: ...mple Data Worksheet as B Sample tube set plus sample mass Before Degas 10 Subtract the A Mass for empty sample tube set from the B Mass of sample tube set plus sample and record this value as the C Sa...

Page 62: ...igh the sample tube set containing the sample and record the weight on the Sample Data Worksheet as B Sample tube set plus sample mass After Degas 2 Subtract the A Mass for empty sample tube set Befor...

Page 63: ...d slowly into the sample tube 2 Slide an isothermal jacket down over the sample tube stem until it touches the sample tube bulb 3 Place the connector nut ferrule and O ring onto the sample tube stem 4...

Page 64: ...ock 2 pour the liquefied gas slowly to prevent splashing and 3 vent the receiving container to the atmosphere Use a plastic stirring rod when stirring substances in a dewar containing liquefied gases...

Page 65: ...ng Dewars 246 42800 01 Aug 2013 2 35 Filling an Analysis Dewar 1 Fill the analysis dewar with the analysis bath fluid to about 5 cm 2 inches from the top Incorrect fluid levels can lead to measurement...

Page 66: ...Dewar has not been used for a while allow approximately 30 minutes for the temperature of the Dewar to stabilize with the bath liquid then recheck the level of the bath liquid Add additional liquid i...

Page 67: ...ASAP 2460 Operator s Manual Filling Dewars 246 42800 01 Aug 2013 2 37 5 Place the dewar on the elevator under the sample tube...

Page 68: ...ars ASAP 2460 Operator s Manual 2 38 246 42800 01 Aug 2013 6 Attach the safety shield to the two hooks on the front panel to enclose the sample tube and dewar 7 Begin the analysis as described in the...

Page 69: ...be performed if a high throughput or krypton analysis is in progress One analysis can be started at a time A sample can be added to any idle port and an analysis started without disturbing the analys...

Page 70: ...o the sample identification Density Mass Sample Tube and Empty Tube fields This information is pulled from the selected or newly created file The Density value is applicable only if using the Calculat...

Page 71: ...encountered before the port status at the bottom of the window changes from the Idle state 8 If you wish to view an analysis report click the appropriate Report Port button 9 When the analysis is com...

Page 72: ...n analysis must specify the Dosing Method From last port in the Adsorptive Properties Samples cannot be removed from or added to ports until the full set of analyses has completed The data collection...

Page 73: ...ation populated into the sample identification Density Mass Sample Tube and Empty Tube fields This information is pulled from the selected or newly created file The Density value is applicable only if...

Page 74: ...st view of the Analysis dialog is displayed High Throughput Analysis When you select this option the High Throughput Analysis dialog is displayed This dialog enables you to start up to six analyses at...

Page 75: ...Manual Performing an Analysis 246 42800 01 Aug 2013 2 45 1 Select Unit Start High Throughput Analysis The High Throughput Analysis dialog is displayed 2 Perform steps 3 through 9 in the topic Krypton...

Page 76: ...started together Once a set is started no other samples can be started until the set is complete 1 Select Unit Start Micropore Analysis The Micropore Analysis dialog is displayed 2 Perform steps 3 thr...

Page 77: ...lect a SMP file from the library The selected report name appears in the File name text box To select more than one file hold down the Ctrl key on the keyboard while selecting the files or hold down t...

Page 78: ...nly one file was selected in Step 1 the Select Reports window displays Verify the reports to generate and select additional reports if necessary Click OK If multiple files were selected this window do...

Page 79: ...2 Select a file from the library To select more than one file hold down the Ctrl key on the keyboard while selecting the files or hold down the Shift key to select a range of files 3 Click List The Re...

Page 80: ...t the destination directory Enter a new file name in the File name field or accept the default Select to save the file as a report system REP a spreadsheet XLS or an ASCII text TXT file format 4 Click...

Page 81: ...type of data to include or exclude during the export process When exported to a file the data can be imported into other applications that read TXT or XLS file formats 1 Select File Export 2 Select a...

Page 82: ...Destination section of the window Preview to send the file to the screen Print to send the file to the default printer Copies select the number of copies to print This field is only enabled when Prin...

Page 83: ...H Adsorption Desorption DFT Pore Size Surface Energy Dollimore Heal Adsorption Desorption Horvath Kawazoe M P Method Only the Advanced format can be used to generate overlays Go to Options Options Pre...

Page 84: ...s window select a plot in the Selected Reports group box then click the Options button to the right of the selected plot c On the Plot Options window select Plot curve and or Plot points if they are t...

Page 85: ...plot Verify other fields Click OK to return to the Report Options tab c Continue with Step 4 BJH Adsorption BJH Desorption Dollimore Heal Adsorption Dollimore Heal Desorption MP Method a In the Select...

Page 86: ...in the Selected Files box and click the Remove button To select more than one file hold down the Ctrl key on the keyboard while selecting the files or hold down the Shift key to select a range of fil...

Page 87: ...Operator s Manual Generating Graph Overlays 246 42800 01 Aug 2013 2 57 8 The report screen displays with tabs across the top of the screen Click each tab to view the reports Refer to Report Tool Bar...

Page 88: ...one line to include title two unit specifications and distribution type Accepted pore dimension units are A nm um Accepted pore volume units are cm3 g cm3 g ml g Accepted distribution types are cumula...

Page 89: ...f other samples To select more than one file hold down the Ctrl key on the keyboard while selecting the files or hold down the Shift key to select a range of files Click Open If a file with a status o...

Page 90: ...en Header information from the ASCII text file will then appear in the Select Imported Overlays window If an error message appears instead verify that the TXT file format listed above is correct Selec...

Page 91: ...n arrow at the Variable field and select a variable to overlay Then click the dropdown arrow of the Overlay field and select the Imported Data entry Click OK to return to the Report Options window 5 C...

Page 92: ...ey on the keyboard while selecting the files or hold down the Shift key to select a range of files Choose the report destination on the Report Settings window and click OK If only one file was selecte...

Page 93: ...ASAP 2460 Operator s Manual Generating Graph Overlays 246 42800 01 Aug 2013 2 63...

Page 94: ...Generating Graph Overlays ASAP 2460 Operator s Manual 2 64 246 42800 01 Aug 2013...

Page 95: ...respective sections Common field and button descriptions are listed in a Common table at the beginning of their respective chapters Field and button descriptions not listed in the Common table are lis...

Page 96: ...ed in error Destination group box Preview sends the file to the screen Click Print on the report screen to send the file to the printer Print sends the file to the default printer Copies select the nu...

Page 97: ...ose the active window Open button Click to open the selected file or double click the file name in the Name column to open the file Preview button Click to preview predefined reports Click the tabs ac...

Page 98: ...New Sample ASAP 2460 Operator s Manual 3 4 246 42800 01 Aug 2013 New Sample Provides the option to create a new sample file or parameter file Refer to Sample Information Files page 3 10...

Page 99: ...xt box contains an asterisk and a default file extension depending on the type of parameter file selected Default file extensions are ADP Adsorptive Properties ANC Analysis Conditions DEG Degas Condit...

Page 100: ...l 3 6 246 42800 01 Aug 2013 file go to File Save As select the Analysis Conditions folder in the application Library and enter a file name in the File name field Click Save Save All Saves all active w...

Page 101: ...ow No closes the window without saving the changes Cancel cancels the Close command Close All Closes all active windows If changes were made and not yet saved a prompt displays for each changed file p...

Page 102: ...data in a sample information file as a REP TXT or XLS file When saved to a file the data can be imported into other applications Convert Allows you to convert sample information files created with an...

Page 103: ...ogram If a file is open with unsaved changes a prompt displays providing the option to save the changes and exit or to exit the program without saving the changes Yes saves the changes then closes the...

Page 104: ...rring conditions When the sample file is created select the Analysis Conditions file for the analysis conditions Once it becomes part of the new sample file edit the new file as needed without affecti...

Page 105: ...ick to edit the sample tube parameters To save the sample tube parameters as a file go to File Save As Select STB as the File Type and enter a File name Description enter a description of the sample t...

Page 106: ...used for the Calculated free space method only Use 0 000 for a blank analysis Type of Data group box Automatically collected select if the type of data will be automatically collected by the system w...

Page 107: ...sser Add Log Entry button Use to enter information to appear in the sample log report that cannot be recorded automatically through the application Click the button again to enter multiple log entries...

Page 108: ...ers to be used in the analysis Heating Phase table Enter up to five stages of degas conditions Temperature soaking temperature with flowing gas Temperature Ramp Rate rate at which the temperature is t...

Page 109: ...d shortcut The Analysis Conditions tab provides details for setting up the sample analysis conditions file Field or Button Description Description dropdown list Use to select an ANC file that contains...

Page 110: ...ty at STP to liquid density Therm tran hard sphere diameter an estimate of molecular size used in calculating the thermal transpiration correction Molecular cross sectional area the area that a single...

Page 111: ...essures Select this option to enable the Pressures and Options buttons Pressures button click to edit the Entered Pressures table Use this window to manually enter the pressures A pressure table consi...

Page 112: ...essure the number of points to insert within the specified range and whether to have linear or geometric progression Linear select to insert evenly spaced points into the table Geometric from low pres...

Page 113: ...sure table point is low and the gas uptake of the sample is expected to be high choosing this mode can shorten the time required to reach the first point on the pressure table Maximum volume increment...

Page 114: ...of points so wider tolerances may be used Unnecessarily tight tolerances lengthen the analysis Low Pressure incremental dose mode Choose this option when you are performing an analysis of microporous...

Page 115: ...ay cause the instrument to wait an excessive length of time for equilibration Dose Increments option The sample is dosed repeatedly with a fixed amount of gas and isotherm points are collected after e...

Page 116: ...pressure table value is reached Incremental Dose Mode is disabled and points are recorded in accordance with the specified pressure table Because the data points recorded during Incremental Dose Mode...

Page 117: ...pace measurement or sample analysis if free space is to be Entered or Calculated Leak test enables the system to check for system leaks or sample outgassing before the analysis The leak test seals the...

Page 118: ...e rises more than 0 025 mmHg within the time specified in the Outgas test duration field outgassing is present If outgassing is found the test repeats up to nine times with a 30 minute evacuation time...

Page 119: ...the measurement of each data point without slowing the analysis 2 Analysis bath temperature not used for krypton analyses Measures the po on a continuous basis and over the sample then adjusts the me...

Page 120: ...e and an estimate for the initial po not used for krypton analyses Measures the po over the sample After the po is measured the value is reapplied to all data points 6 Analysis bath temperature This m...

Page 121: ...reading of the pressure changes Long equilibration intervals tend to lengthen analyses but improve data integrity Short equilibration intervals produce a faster analysis but may reduce the accuracy of...

Page 122: ...reading of the pressure changes Long equilibration intervals tend to lengthen analyses but improve data integrity Short equilibration intervals produce a faster analysis but may reduce the accuracy of...

Page 123: ...ling the sample tube Indicate if the sample should be backfilled at the start and or end of the analysis Click the dropdown arrow and select the backfill gas to be used Cancel button Close button OK b...

Page 124: ...he minimum and maximum pressures to be included in the pressure table Include All button include all pressures in the table Exclude All button exclude all pressures in the table Use Interpolation chec...

Page 125: ...EPORTS MENU page 5 1 Customized report options files can be created then loaded into a sample file allowing quick and easy generation of reports Field or Button Description Report Options dropdown lis...

Page 126: ...ranspiration Always use thermal transpiration when performing micropore analyses Refer to CALCULATIONS page C 1 for additional information on thermal transpiration Inside diameter of sample tube text...

Page 127: ...ed on the Collected Data window the isotherm is interpo lated to the value in the p po fields and the point is used for the total pore volume calculation Otherwise the point selected with calculation...

Page 128: ...ions window for selection of pass fail criteria Upper Lower options and text boxes specify upper and lower limits for the selected parameter A range can be left open by not selecting the limit In the...

Page 129: ...lick Edit Field or Button Description Select Reports group box Select the checkbox to the left of each option to include on the final report Options buttons Click to display related linear plot option...

Page 130: ...Time between points time elapsed between points during the analysis Plot Options group box Select the types of isotherm to plot adsorption desorption overlays Quantity Adsorbed group box Select how t...

Page 131: ...rea 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...

Page 132: ...is the y axis field shows BET Langmuir transformation BET or Langmuir Isotherm plot Uses the BET Langmuir monolayer volume and constant to produce an isotherm Overlay samples checkbox use to overlay s...

Page 133: ...hen click Edit Field or Button Description Specify monolayer capacity checkbox and text box Select and enter the monolayer capacity of the sample Tabular report checkbox Use to have a report of the pr...

Page 134: ...overlay sample files on the Freundlich isotherm plot Autoscale x axis linear x axes begin at zero The x axis field shows the absolute pressure Autoscale y axis y axes begin at zero The y axis field s...

Page 135: ...the monolayer capacity of the sample Specify differential heat of adsorption checkbox and text box Select and enter the differential heat of adsorption at zero surface coverage This allows inclusion...

Page 136: ...files on the isotherm plot Autoscale x axis linear x axes begin at zero The x axis field shows the absolute pressure Autoscale y axis y axes begin at zero The y axis field shows the quantity of gas a...

Page 137: ...ed materials In the Selected Reports list box highlight t Plot then click Edit Field or Button Description Thickness Curve group box Select the thickness curve and click Edit to modify the values in t...

Page 138: ...the first column and the thickness values in the second column Columns must be separated by a space or a tab Refer to Table buttons page 3 3 for a description of the Insert Delete Clear and Append but...

Page 139: ...curve Go to Options Units to specify default units Refer to UNIT MENU page 4 1 Tabular report checkbox Use to have a tabular report of data generated t Plot checkbox Use to have a graphical representa...

Page 140: ...rectory Use the table to enter relative pressure and the alpha s values Field or Button Description Open button To import values from an existing thickness curve ALS file click Open and select the fil...

Page 141: ...heckbox Use to have a tabular report of data generated Alpha S plot checkbox Use to plot data in graph format Overlay samples checkbox use to overlay sample files on the plot Autoscale x axis the x ax...

Page 142: ...ple of the same material as the current sample When the referenced file is selected the file name appears to the left of the Browse button Tabular report checkbox Select to have a tabular report of da...

Page 143: ...ed Reports list box highlight BJH Adsorption or BJH Desorption then click Edit An incomplete pore distribution may be generated if a thickness curve selection is not a good match for the sample being...

Page 144: ...o compensate for this error Cumulative Reports options Larger use to report the total volume found in pores larger than the current pore size Smaller use to report the total volume found in pores smal...

Page 145: ...ields and Buttons File Menu Options page 3 1 Field or Button Description Fixed pore size table Use to specify exact pore sizes for volume or area data Click the Table button to modify the fixed pore s...

Page 146: ...utton The fixed pore size table must contain a minimum of two points The points must be strictly decreasing Enabled only when Fixed pore size table is selected Cancel button OK button Refer to Common...

Page 147: ...box in the BJH Report Options window and click Edit Field or Button Description Plot curve Plot points checkboxes Refer to Isotherm Report Options page 3 35 X Axis Use to have the x axis on a logarith...

Page 148: ...tes Dollimore Heal reports from both adsorption and desorption data In the Selected Reports list box highlight Dollimore Heal Adsorption or Dollimore Heal Desorption then click Edit Dollimore Heal Ads...

Page 149: ...ometry of the micropores in the sample material When Sphere is selected options in the Interaction Parameter group box are disabled Interaction Parameter group box Use to determine which interaction p...

Page 150: ...ter and Diameter at zero energy text fields may be edited Description select the name of the sample used in the analysis Diameter enter the diameter of the sample atom Diameter at zero energy enter th...

Page 151: ...n atom at zero interaction energy 2 5 1 6 diameter Polarizability enter the polarizability of the adsorptive Magnetic susceptibility enter the magnetic susceptibility of the adsorptive Density enter t...

Page 152: ...s window and click Edit Select the data types to include in the report Column n indicates the column order and data contents for the report Plot Options Highlight a plot option in the Selected Reports...

Page 153: ...nanometers Y Axis the y axis field shows the quantity of gas adsorbed Variable dropdown list select a y axis variable for the report Overlay dropdown list select an option to overlay on the current re...

Page 154: ...based on the density functional theory Classical model based on the Kelvin equation and thickness for determining the pore size distribution Refer to DFT MODELS page F 1 for further discussion on mode...

Page 155: ...Edit The Log Goodness of Fit and Goodness of Fit graphs cannot be edited Plot Type group box select the method for data display Autoscale Options group box use to autoscale the x axis and or y axes Ov...

Page 156: ...eport Options The DFT Surface Energy report contains the results of surface energy distribution analyses In the Selected Reports list box highlight DFT Surface Energy then click Edit DFT Surface Energ...

Page 157: ...escription Report Type group box Select report types If Astakhov is selected either select the Optimize exponent checkbox or enter an appropriate exponent value in the text box Fitted Relative Pressur...

Page 158: ...cted on the Dubinin Report Options window If not then the value for n is the entered exponent value Transformed Isotherm Plot Options Highlight Transformed Isotherm in the Selected Reports list box in...

Page 159: ...Use to overlay sample files on the plot Autoscale x axis Autoscale y axis checkboxes Select an option to have the x and or y axes scaled automatically Both axes begin at 0 the system uses the highest...

Page 160: ...urve Plot points checkboxes Use to plot curves and or points Overlay samples checkbox Use to overlay sample files on the plot Autoscale x axis Autoscale y axis checkboxes Select an option to have the...

Page 161: ...ighlight MP Method then click the Edit button Pore size can be expressed in angstroms or nanometers Go to Options Units to specify the unit Refer to UNIT MENU page 4 1 Field or Button Description Thic...

Page 162: ...Report Options window highlight MP Tabular Report in the Selected Reports list box and click Edit Column n indicates the column order and data contents for the report The MP Method reports hydraulic r...

Page 163: ...scription Plot curve Plot points checkboxes Use to plot a curve and or points X Axis Use to have the x axis autoscaled or enter beginning and ending values Y Axis Variable dropdown list select a varia...

Page 164: ...s 10 tabular reports and 10 graphical reports In order to use this feature you must create a file containing a Python script that imports a mic python module Appendix G provides an example of python s...

Page 165: ...ists to select currently defined functions used to define the report calculations and output Edit button Use to edit a function Overlay samples checkbox Use to overlay samples as defined by the functi...

Page 166: ...nformation Manual control operations performed during analysis Information entered using Add Log Entry on the sample file editor Warnings and or errors which occurred during analysis Validation Report...

Page 167: ...This chapter provides details of Unit menu options and descriptions of commonly used functions and buttons The title bar of the main window displays as Unit n for each attached unit Each unit has a st...

Page 168: ...r a file Select a file from either the Name column or from the application Library and click Open or double click the file name to open the file Cancel button Discards any changes made to the screen o...

Page 169: ...the active window Report after analysis button Preview sends the file to the screen Click Print on the report screen to send the file to the printer Print sends the file to the default printer Copies...

Page 170: ...rom any of the six ports without disturbing the analyses being performed on other ports The sample dosing method should be Normal All analyses must use the same gas If saturation pressure is being mea...

Page 171: ...be selected at a time Sample text field Displays the sample s file name Mass group box continued Calculate enables the Empty tube and Sample tube fields Enter the values necessary to calculate the sam...

Page 172: ...alysis button Refer to Common Fields and Buttons Unit Menu Options page 4 2 Start button Begins the analysis Suspend button Click to suspend an analysis in progress Select the ports containing the ana...

Page 173: ...nted to the screen only Live Graph Settings button Allows you to select Thermal transpiration X axis Quantity relative or absolute pressure and the X Axis Scale linear or logarithmic Status window Dis...

Page 174: ...order to start an analysis All analyses must use krypton gas From one to five analyses can be started at the same time using ports 1 through 5 Port 6 is reserved for dosing A blank tube must be instal...

Page 175: ...ables the Empty tube and Sample tube fields Enter the values necessary to calculate the sample mass Equation used to calculate sample mass Masssample Masssample tube Masstube Density value is used for...

Page 176: ...button Click to skip to the next step This button is visible only when an analysis is in progress Select the ports containing the step to skip Use the Skip function with caution the ASAP 2460 performs...

Page 177: ...ogarithmic Status window Displays the last point pressure and relative pressure for each port with varying numbers of digits after the decimal if 10 mmHg and 0 1 mmHg transducers are present on that p...

Page 178: ...put analyses All ports must be idle in order to start an analysis All analyses must use the same analysis gas All analyses that measure Psat must use the same Psat gas which may be different from the...

Page 179: ...All ports must be idle in order to start an analysis All analyses must use the same analysis gas All analyses that measure Psat must use the same Psat gas which may be different from the analysis gas...

Page 180: ...ter to select a component A component is selected when it is surrounded by a thin line Each component has a shortcut menu displaying the operations available for that particular com ponent These menus...

Page 181: ...P 2460 Operator s Manual Start Micropore Analysis 246 42800 01 Aug 2013 4 15 Double click on the valve or elevator symbol Select the valve or elevator symbol and press the Spacebar Transducers Each sa...

Page 182: ...ansducer readings and the vacuum gauge pressure The 1000 mmHg transducer is present in all ASAP 2460 systems The 10 mmHg transducer is shown only on units containing the Krypton or Micropore option Th...

Page 183: ...n Enable Manual Control Select this option to display a schematic of the ASAP 2460 analysis system The schematic is a graph ical representation of the analysis system including system valves analysis...

Page 184: ...Show Instrument Schematic ASAP 2460 Operator s Manual 4 18 246 42800 01 Aug 2013 Four port Instrument Schematic Six port Instrument Schematic...

Page 185: ...Dashboard The dashboard displays the following Number of analyses started and the number completed Number of days until roughing pump maintenance is due Manifold outgas rate Nitrogen po statistics Dat...

Page 186: ...early maintenance is recommended The number of days until the anniversary of the last pump maintenance are shown The displayed value is updated at least once per day and when the maintenance time is r...

Page 187: ...ratures The mean two sigma minimum and maximum values display The gauge is updated when a po is logged with nitrogen as the adsorptive To reset these numbers right click on the window then click the R...

Page 188: ...246 42800 01 Aug 2013 Show Status Unit n Show Status Use to show the current status for each port If there are multiple units attached to the computer Select Show Status on each unit menu and have th...

Page 189: ...and calibrations Field or Button Description Analysis Calibration Message Select which logs to display Include Message Number Use to generate a log report containing all the instances of one message n...

Page 190: ...rint This field is only enabled when Print is selected File saves the report as a file Click the Browse icon to the right of the text field to select the directory where the new report file will be st...

Page 191: ...ASAP 2460 Operator s Manual Degas 246 42800 01 Aug 2013 4 25 Degas Unit Degas If a SmartPrep is not connected to the analyzer the menu options in this section are disabled...

Page 192: ...and stop gas flow after samples are degassed Field or Button Description Skip button Use to skip the degassing of the selected sample Cancel button Use to cancel the degassing of the selected sample...

Page 193: ...Prep heating stations are represented by row numbers on the Automatic Degas window Field or Button Description Browse button Use to locate a sample file to degas Clear button Clears the entry of the s...

Page 194: ...Degas ASAP 2460 Operator s Manual 4 28 246 42800 01 Aug 2013 SmartPrep Configuration Unit Degas SmartPrep Configuration Displays the SmartPrep configuration and software versions ASAP 2460...

Page 195: ...r of the selected analyzer Change IP click to display the Unit IP Setup window The IP address and Subnet mask assigned during installation display Do not edit these fields unless instructed by a Micro...

Page 196: ...Unit Configuration ASAP 2460 Operator s Manual 4 30 246 42800 01 Aug 2013 Calibrations button Displays calibration information for instrument components Field or Button Description continued...

Page 197: ...ASAP 2460 Operator s Manual Show All Readings 246 42800 01 Aug 2013 4 31 Show All Readings The Show All Readings screen displays the calibrated and nominal readings of all sensors in the system...

Page 198: ...ag directory assuming you used the default direc tory Your service representative will request that you E mail this file to him so that he may examine the data If E mail is unavailable you may print t...

Page 199: ...st Analysis Leak Test with Clean Leak Test all Manifolds Operator Enter information to identify the person running the service test Estimated time min Approximate time for test completion Repeat butto...

Page 200: ...tem is in Service Test mode Save to File Unit n Calibration Data Save to File Use to save the current calibration settings to a backup file which can later be reloaded using Unit n Calibration Load fr...

Page 201: ...tion file a backup of the current file is created and saved as SN last cal The backup file is overwritten each time a new one is created Service Test Unit n Service Test Use for service tests performe...

Page 202: ...Service Test ASAP 2460 Operator s Manual 4 36 246 42800 01 Aug 2013...

Page 203: ...ple currently being analyzed manually entered Common Fields and Buttons Reports Menu Options The following fields and buttons are common to many of the report files References are made to these fields...

Page 204: ...t box Select a file from either the Name column or from the application Library The file name displays in the File name text box Click Open or double click the file name to open the file Multiple file...

Page 205: ...Report Reports Start Report or use the F8 keyboard shortcut Use to generate a report on a sample analysis Close Reports Reports Close Reports or use the F9 keyboard shortcut Use to close all open repo...

Page 206: ...Open Report 2460 Operator s Manual 5 4 246 42800 01 Aug 2013 Open Report Reports Open Report file Use to open a saved report...

Page 207: ...s All selected variables must be computed for each sample file used in an SPC report therefore it is more efficient to select only the necessary variables The selected items appear as options on the R...

Page 208: ...eport Options 2460 Operator s Manual 5 6 246 42800 01 Aug 2013 The selected items also appear as options on the Reports Control Chart screen Click the Graph n button then click the Statistic dropdown...

Page 209: ...ext box Use to show a graphic on the report header Click the Browse button to locate the graphic Height Width enter the height and width of the selected graphic These values determine the graphic appe...

Page 210: ...s selected the following message displays Saving the recalculated SPC data may render some files unreadable by the original application Saving the SPC data speeds up future SPC reports Do not show me...

Page 211: ...the Available Files list box and click Add to move the file to the Selected Files list box Or select a file in the Selected Files list box and click Remove to move the file back to the Available File...

Page 212: ...statistic Field or Button Description Show report title text box Select and enter a report title to appear on the report header Show graphic text box Use to show a graphic on the report header Click t...

Page 213: ...e sorts in alphanumeric order Date sorts by the date the files were analyzed Minutes sorts by the minutes elapsed from the first file placed on the list which is the earliest analyzed file Days sorts...

Page 214: ...ields Center Line group box displays placement options for the center line in the graph Choose Entered to specify placement of the line Limit Lines group box displays limiting lines options Lines can...

Page 215: ...he adsorbent and the adsorption capacity Multiple adsorption isotherms are obtained on the same sample using the same adsorptive but at different temperatures to obtain the heat of adsorption Field or...

Page 216: ...adsorbed and number of points to insert Insert button insert a row above the selected row Delete button deletes the selected row Clear button clears the entire table of all entries except one Append b...

Page 217: ...bed versus the temperature Heat of adsorption plot checkbox Select to generate the Heat of Adsorption data in a graphical format Open button Click to select and open a Heat of Adsorption file Browse b...

Page 218: ...he report header can also contain a graphic and a title Tabular and graphical reports contain sample and instrument statistics such as analysis date time analysis conditions etc The headers contain no...

Page 219: ...l generated reports The same reports display as tabs across the top of the report header unless the report has been hidden using the Hide button Show button Jumps to the selected report in the Reports...

Page 220: ...ects all reports in the Reports list box Shown button selects only the reports not hidden Clear button clears all selections OK button prints the selected report to the printer indicated Cancel button...

Page 221: ...ck to specify default report parameters for fonts and curve properties Font group box Font Type list box allows font type and attributes to be edited for the selected item Select an item in the list c...

Page 222: ...ogram Fill dropdown list select a histogram fill option from the list Graph border line thickness text box enter a thickness number for the graph border Load button click to load the last saved defaul...

Page 223: ...the move Align column Right click on the column to be aligned Select Align Column on the shortcut menu and select Left Right or Center Show column Displays a list of all columns Click a column to add...

Page 224: ...ther document Option Description Autoscale all axes Returns the report to full view after using the zoom feature Reset axis limits to initial setting Removes the cross hair and returns the graph back...

Page 225: ...selected curve Color button click to change the curve color Use default thickness checkbox select to use the default curve thickness Deselect the checkbox and enter a new thickness number in the Thick...

Page 226: ...ox use to change the graph display Linear Logarithmic select the option to scale the graph as linear or logarithmic Autoscale minimum maximum select the Autoscale checkbox to enable the option To manu...

Page 227: ...efault font to enable font options Edit title Use to change the graph title and font Deselect the Use default font to enable font options Copy Graph Copies the graph to the clipboard It can then be pa...

Page 228: ...e mouse button The enlarged area fills the graph area To return to normal view right click in the graph area and select Autoscale all axes or Reset all axes to initial setting on the shortcut menu Axi...

Page 229: ...2460 Operator s Manual Report Examples 246 42800 01 Aug 2013 5 27 Report Examples This section of the manual contains samples of some of the available reports Most of the reports can be customized...

Page 230: ...Report Examples 2460 Operator s Manual 5 28 246 42800 01 Aug 2013 Isotherm Linear Plot...

Page 231: ...2460 Operator s Manual Report Examples 246 42800 01 Aug 2013 5 29 BET Surface Area Report...

Page 232: ...Report Examples 2460 Operator s Manual 5 30 246 42800 01 Aug 2013 BET Surface Area Plot...

Page 233: ...2460 Operator s Manual Report Examples 246 42800 01 Aug 2013 5 31 t Plot Report...

Page 234: ...Report Examples 2460 Operator s Manual 5 32 246 42800 01 Aug 2013 BJH Adsorption Cumulative Pore Volume...

Page 235: ...2460 Operator s Manual Report Examples 246 42800 01 Aug 2013 5 33 BJH Desorption Cumulative Pore Volume...

Page 236: ...Report Examples 2460 Operator s Manual 5 34 246 42800 01 Aug 2013...

Page 237: ...ntation Use to change the default editing format of sample files Restricted Basic or Advanced Each format type displays sample information and options differently For descriptions of the presentation...

Page 238: ...hod Use to specify default parameters for sample information files Manage Libraries Options Manage Libraries The application Library allows access to sample and parameter files The library gathers fil...

Page 239: ...ns Manage Libraries Select the library to modify then click the Manage button 2 To add a folder click Add to browse and locate a folder Select the folder and click the Include Folder button 3 To remov...

Page 240: ...Options Graph Grid Lines Use to select how grid lines appear on reports This menu option is not available if using Restricted format Field or Button Description X Axis Y Axis options Select major and...

Page 241: ...vice Test mode is a password protected option used to perform certain service tests with the assis tance of a trained Micromeritics service representative The password is supplied by your service repr...

Page 242: ...Service Test Mode 2460 Operator s Manual 6 6 246 42800 01 Aug 2013...

Page 243: ...ring at the analysis port Sample weighing errors Use of too much analysis bath fluid in the dewar at the start of an analysis Entry of incorrect system volume for analysis Always check these first whe...

Page 244: ...ug or empty sample tube on the port Enable manual control then use the instrument schematic to close the gas inlet valve Refer to Enable Manual Control page 6 20 Vacuum gauge shows reading above 20 mH...

Page 245: ...Alumina in the Oil Vapor Traps page 7 13 Oil Free Pump Only Filter in the port being used is dirty Replace the port filter Refer to Replacing Analysis Port Filters page 7 5 High vacuum pump may have t...

Page 246: ...um pump fluid page 7 9 As required or every 3 months Replace alumina in oil vapor traps page 7 13 As required or every 3 months Clean the outside of the analyzer page 7 16 As required or every 6 month...

Page 247: ...nsure problems do not develop due to ice accumulation check the dewar after each use Clean dewars on a weekly basis as follows 1 Remove the dewars and pour the liquid nitrogen from the dewars into an...

Page 248: ...from the analyzer Sample tube fitting 2 Remove the filter and O ring 3 Replace the filter and the O ring 4 Reinstall the analysis port fitting securely tighten with a wrench to prevent leaks during e...

Page 249: ...dure applies to both degas and analysis ports 1 Holding the sample tube firmly with one hand loosen and remove the sample tube connector nut by turning it counterclockwise Carefully pull the sample tu...

Page 250: ...lide a new O ring over the sample tube about 1 4 in 5 mm from the top of the tube 4 After the new O ring is in place insert the sample tube back into the sample port until it is fully seated 5 Turn th...

Page 251: ...h vacuum levels The fluid can first be inspected to determine if a change is necessary Use oil supplied by Micromeritics or refer to the vacuum pump manual for other acceptable oils Inspecting Fluid 1...

Page 252: ...g the vacuum pump from the power source 2 Loosen the wing nut on the clamp at the top of the oil vapor trap Swing the clamp open and remove the trap from the hose Always drain the vacuum pump while th...

Page 253: ...Replace the drain plug 4 Remove the oil fill plug 5 Add fresh fluid to the oil fill port until the level is midway between the two indicator lines in the oil level window 6 Check the washer or O ring...

Page 254: ...plug from the drain spout e Allow the oil to drain into the waste container f Reinstall the drain plug g Add fresh fluid to the oil fill port until the level is midway between the two indicator lines...

Page 255: ...or a three month period Most of the alumina pellets are no longer white 1 Prepare fresh alumina as follows a Heat an oven between 250 C and 350 C b Pour about 180 grams of alumina into a glass or meta...

Page 256: ...Remove the used alumina from the trap body and dispose of it in an appropriate manner 5 If the trap body interior appears oily or dirty wash it with isopropyl alcohol or ethyl alcohol and dry it thoro...

Page 257: ...ure the centering ring is in place on the intake port 8 Place the trap on the centering ring 9 Open the clamp and place it around the flange of the intake port and the flange of the trap Swing the cla...

Page 258: ...be cleaned every six months or sooner if required Clean the outside casing of the analyzer including the shields with a clean cloth dampened with iso propyl alcohol IPA a mild detergent in water or a...

Page 259: ...in unused gas inlet ports 3 If the analysis system schematic in manual control mode is not displayed on the computer screen select Unit Enable Manual Control then Unit Show Analysis Schematic 4 Open...

Page 260: ...through 26 13 Record the pressure as the Initial Reading then begin timing as soon as you complete the next step 14 Gas inlet valves 21 through 26 must remain closed during this procedure Pressurize...

Page 261: ...he filter minimizes the release of oil vapor and should be replaced when it becomes so saturated with oil that it is ineffective This procedure applies to oil based vacuum pumps only Exhaust filters a...

Page 262: ...filter 3 Retain the centering ring clamp and wing nut 4 Remove the dust cover from the new filter 5 Make sure the centering ring is on the exhaust port 6 Place the new filter on the centering ring 7 O...

Page 263: ...Label both ends of the gas lines before connecting for ease in identification and maintenance Ensure that all gas bottles are closed before connecting them to the analyzer The instructions below desc...

Page 264: ...tor as follows a Close the regulator shut off valve by turning it fully clockwise b Turn the pressure regulator control knob fully counterclockwise c Slowly open the gas bottle valve by turning it cou...

Page 265: ...1 through 4 for each gas supply bottle to be attached to the analyzer 6 Proceed to the next section to connect the copper delivery tubing to the analyzer Connecting the Gas Delivery Tubing to the Ana...

Page 266: ...you must enter the change in the analysis program as follows 1 Select Unit n Unit Configuration from the main menu The Unit Configuration dialog is displayed 2 Click on the down arrow at the port to...

Page 267: ...failed Causes and corrective action for a failure are provided Before beginning confirm that the state for valves and the low pressure gauge are as follows 1 To start diagnostic testing go to Unit n D...

Page 268: ...operation If any test shows a Failed reading refer to the following table for the location of the gas leak Tab Test If Failed status then Gas Line to Inlet Port n Test 1 Gas Line to Gas Bottle Test T...

Page 269: ...ur accessories If your system needs recalibration contact your Micromeritics service representative The calibration procedures under the Calibrate Analysis com mand on the Unit menu are accessible by...

Page 270: ...Calibrating the System ASAP 2460 Operator s Manual 7 28 246 42800 01 Aug 2013...

Page 271: ...samples with both heat and flowing gas 060 00030 00 FlowPrep 060 degasses up to six samples at up to 400 C with flowing gas 061 00030 00 VacPrep 061 degasses up to six samples at up to 400 C with eit...

Page 272: ...not to be used with noxious gases 004 62230 32 Gas pressure regulator CGA 320 fitting CO2 30 psig 004 16821 00 Reference material high surface area 004 16816 00 Reference material low surface area kry...

Page 273: ...00001 11 Vacuum pump oil based with built in anti suckback valve 100 120 VAC includes hose kit and alumina oil vapor trap 062 00001 23 260 25896 00 004 25626 08 Vacuum pump oil based with built in an...

Page 274: ...a computer other than the one controlling the analyzer or to compare data from another instrument 202 20827 00 MicroActive software 202 42827 00 MicroActive Operator s manual Part Number Item and Des...

Page 275: ...300 25862 00 M TranSeal assembly for use with 1 2 in sample tubes only 202 25901 00 N Isothermal jacket 1 4 in 240 61001 00 O Sample tube 1 4 in 240 61014 00 P Filler rod 1 4 in 202 25902 00 Q Isother...

Page 276: ...Ordering Information ASAP 2460 Operator s Manual 8 6 246 42800 01 Aug 2013...

Page 277: ...ASAP 2460 Operator s Manual Appendix A 246 42800 01 Aug 2013 A 1 A FORMS This appendix contains the following form Sample Data Worksheet Copy and use this form as needed...

Page 278: ......

Page 279: ...__________________________________________________ _________________________________________________________________________________ Sample Mass g NOTE Record all values in grams Before Degas After De...

Page 280: ......

Page 281: ...roblem occurred Action A Check the performance of your computer devices or network Cause B A software error occurred when the file was accessed Action B Contact a Micromeritics service representative...

Page 282: ...te Select No if you do not want to spend the time updating the directory information This option may be feasible if a large number of files have been copied into the directory and you know the name of...

Page 283: ...field does not contain a valid file specification Cause You entered an invalid file name Action See the description of file naming conventions in your Windows man ual and re enter the name 2450 Sampl...

Page 284: ...then restart the application If this error persists contact your service representative 2461 No instruments are in operation This application will unconditionally terminate Cause At least one analyze...

Page 285: ...port assigned to this program 2475 Unit number Communications port COM port number specified in the pro gram control files cannot be accessed Unit cannot initialize Cause The operating system has pre...

Page 286: ...from the proper application 2480 File file name cannot be analyzed It is currently being edited Cause You attempted an analysis using a sample file that is being edited Action Save the changes and cl...

Page 287: ...window containing the file correct the errors and save it 2484 The edit session for file name must be saved before the analysis Save changes and continue with the analysis Cause You attempted an anal...

Page 288: ...you specified is being used in another edit operation Action Check the Windows list to locate the other edit session 2489 File file name cannot be opened for writing It is already in use Cause The fil...

Page 289: ...is required for this field Cause This field requires a valid entry for you to proceed Action Enter or select an appropriate value 2494 Value is out of the valid range 2495 Value is out of the valid r...

Page 290: ...es 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...

Page 291: ...me Cause You selected an invalid calibration file or one that cannot be read Action Be sure the media containing the calibration file has no problems 2514 Unable to write the calibration file file nam...

Page 292: ...erformed Action If the calibration operation was successful press Accept 2520 No data points available for reporting Cause No analysis file Action Choose another file 2521 Unable to program controller...

Page 293: ...f software operat ing in the analyzer Action If there are no analyzers other than the ASAP 2460 connected to the computer select Yes and allow the updated software to load 2533 Analyzer initialization...

Page 294: ...at the analyzer is turned on and that the status light is not blinking If these checks are okay exit the analysis program and then restart the application If this error persists contact your service r...

Page 295: ...longer exists Action If the directory was deleted renamed or moved in error restore the directory Action Select a different set of files for SPC reporting 2560 File filename cannot be created or opene...

Page 296: ...name has no dose incremental table entries 2599 The selected file has an extension that is not supported by this operation Cause This message is triggered on application start up if any of the library...

Page 297: ...report generation Action Contact your service representative if you continue to receive this error message 4005 Pressures were not smoothed Not enough pressures below 0 10 P Po Cause The Smooth pressu...

Page 298: ...elect only files that have been created by MICMOS 2400 or 2405 programs 4015 Error creating export file for sample filename Cause A file error occurred during creation of an export output file Action...

Page 299: ...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 w...

Page 300: ...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 Action Enter valid values into the fields that have errors...

Page 301: ...es 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 analy...

Page 302: ...the Dubinin report 4034 Fewer than 2 points available for Dubinin calculations Cause There are fewer than two valid data points available for Dubinin reports in one of the sample files selected for ov...

Page 303: ...duced This message will always be preceded with another one containing additional infor mation Action Refer to the number of the error message which preceded this one for an explanation 4038 Fewer tha...

Page 304: ...the Horvath Kawazoe report If the Langmuir correlation coefficient can be brought above 0 98 by removing some points at high relative pres sure remove them and reproduce the Horvath Kawazoe reports 40...

Page 305: ...ptions so that the Cheng Yang correction is not applied 4042 0 0 cannot be a starting or ending pressure for a geometric progression from low pressure Cause You selected to generate a pressure table f...

Page 306: ...ntegrity check using ScanDisk 4047 Warning An error occurred while reading file name Cause An error happened during a read operation of a thickness curve file Action If the problem persists restart yo...

Page 307: ...ess range for the t Plot calculations Action A Edit the calculation assignments for the t Plot report Action B Edit the fitted thickness range in the t Plot report editor 4055 A positive BET surface a...

Page 308: ...culation assignments are not being used edit the Temkin Report options Abso lute pressure range in the sample file Cause You have selected at least one point with a negative pressure value to include...

Page 309: ...ed but none of the subreports for that report were selected meaning nothing will be done for that report Action A If the report was selected in error remove the selection 4067 No data points are withi...

Page 310: ...are then try again 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 data reduc...

Page 311: ...y These are placed in the directory during software installa tion Action Reinstall the software to place the DFT models in the MOELS direc tory 4076 Invalid sample file Adsorptive Properties Non conde...

Page 312: ...remove the named overlay file from the list 4078 Slope and Y Intercept cannot be determined from the selected points Cause The Langmuir report cannot be generated from the selected points Action Edit...

Page 313: ...rn on the analyzer and restart the 2460 application If the problem persists con tact your Micromeritics representative 6101 Configured serial number does not match instrument Cause The serial number o...

Page 314: ...his action must be completed before the application exits Cause The unit is calibrating Action Do not exit the application until the calibration is complete 6213 Error overheating on port number Curre...

Page 315: ...name that is already in use Action Enter a unique file name 6220 There are currently no available ports to start a degas operation Cause All degas ports are in use Action Wait until the degas operati...

Page 316: ...analysis can be started 6227 File name cannot be analyzed It is currently being edited Cause You tried to start an analysis using a sample information file that is cur rently being edited Action Close...

Page 317: ...rm a Krypton analysis with Normal selected as the dosing method Action Choose From last port for Dosing Method in the Adsorptive Proper ties dialog then start the analysis 6232 Po gas in sample file d...

Page 318: ...ded before the port port number 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 i...

Page 319: ...ected to the analyzer Action A Check the helium gas connections Cause B A valve transducer or elevator has failed Action B Contact your Micromeritics representative 6249 Zeroing of a transducer failed...

Page 320: ...rvice representative 6264 Krypton gas is not condensing in sample port 6 pressure Cause A The krypton gas may be contaminated Action A Evacuate the krypton gas inlet line Action B Manually verify the...

Page 321: ...um manifold pressure Action The analysis was canceled All previously collected data were stored 6517 Unit number Total volume dosed greater than volume cm3 is not allowed Cause A More than volume cm3...

Page 322: ...s not contain enough bath liquid Action A Retry the operation after filling the Dewar Cause B The Psat tubing from the regulator to the instrument is contaminated Action B Pump out the tubing Cause C...

Page 323: ...old is contaminated or leaking Action C Correct the problem Refer to Appendix D TESTING THE ANA LYZER FOR LEAKS 6523 Analysis suspended Time limit exceeded while evacuating sample unrestricted Cause T...

Page 324: ...ck the sample tube and the sample tube fitting ensure that the tube is securely attached to the port Verify that the sample is properly degassed then resume the analysis 6525 Time limit exceeded while...

Page 325: ...pressure measured over the dosing source Note that the Adsorptive Properties must specify dosing from Psat tube Sample port 3 or Vapor source 5 The saturation pressure of a gas is measured in the Po...

Page 326: ...calculate relative pressure for that point Equation of State The ideal gas law relates pressure volume temperature and quantity of gas where P pressure R a constant that depends on the units of n For...

Page 327: ...n the free space is with the real gas equation of state Here Ps is the sample pressure where Tamb approximate room temperature 298 K Tbath analysis bath temperature K Vfc volume of free space cold cm3...

Page 328: ...re after raising dewar and equilibrating with helium Tamb approximate room temperature 298 K Tbath analysis bath temperature K Tman system manifold temperature before dosing helium onto sample K TSTD...

Page 329: ...he sample from the measured free space of the empty tube where Tamb approximate room temperature 298 K Tbath analysis bath temperature K TSTD standard temperature 273 15 K Vcb cold free space of the e...

Page 330: ...oint window where the numerical constants are from the Savitzky Golay convolution arrays and Pavg average pressure Pchg change in pressure Ppcp i percent change per interval Pi ith pressure reading ta...

Page 331: ...equal to 0 99 where Weber s coefficient 0 033 Weber s coefficient 0 245 F Y intermediate values for subsequent calculations G Weber s coefficient 2 5 H Weber s coefficient 2 MD thermal transpiration h...

Page 332: ...e following are calculated a Slope S g cm3 STP b Y intercept Yint g cm3 STP c Error of the slope Serr g cm3 STP d Error of the y intercept YIerr g cm3 STP e Correlation coefficient Using the results o...

Page 333: ...ndent variable and L is the dependent variable The following are calculated a Slope S g cm3 STP b Y intercept Yint g cm3 STP c Error of the slope Serr g cm3 STP d Error of the y intercept YIerr g cm3...

Page 334: ...m has the form where C temperature dependent constant m temperature dependent constant P equilibrated collected pressure measured by gauge at temp Tamb Q quantity of gas adsorbed Qm quantity of gas in...

Page 335: ...mp Tamb q0 the differential heat of adsorption at zero surface coverage Q quantity of gas adsorbed Qm quantity of gas in a monolayer R molar gas constant T bath temperature In terms of quantity adsorb...

Page 336: ...nt Using the results of the above calculations the following can be calculated External Surface Area m2 g where 104 unit conversions F surface area correction factor user entered on the t Plot Report...

Page 337: ...t squares analysis fit is performed on the i Qads i data pairs where i is the independent vari able and Qads i is the dependent variable The following are calculated a Slope S cm g STP b Y intercept Q...

Page 338: ...ach data pair represents an interval boundary or desorption step boundary for intervals i 1 to i n 1 where n total number of P Q pairs Generally the desorption branch of an isotherm is used to relate...

Page 339: ...s and the critical pressure is defined by the Kelvin equation b The adsorbed layer composed of adsorbed gas that is stripped off a bit at a time with each pressure step the relationship between the th...

Page 340: ...pores open at both ends from the BJH Adsorption Report Options window or the BJH Desorption Report Options window assumed to be zero for desorption Rc Kelvin radius of core This radius will be adjust...

Page 341: ...are no previously opened pores so the volume of liquid desorbed from walls of previously opened pores is zero Vd1 0 and the remainder of Step a is skipped The change in thickness of the wall layer du...

Page 342: ...hus no ending Kelvin radius and average pore diameter are calculated for this inter val Note that this means the report may have fewer tabulated intervals on the collected data report than experimenta...

Page 343: ...nd Rck 1 if its length was the mean of the lengths at those radii The relative pressure corresponding to Davg k is calculated as The thickness of the adsorbed layer at this pressure is calculated as T...

Page 344: ...o the ends of the pressure intervals as for all except Rck 1 Steps a to c are repeated for each pressure interval After the above calculations have been performed the diameters corresponding to the en...

Page 345: ...Area SAcum i m2 g 5 dV dD pore volume dV dDi cm3 g A 6 dV dlog D pore volume dV dlog D i cm3g 7 dA dD pore area dA dDi m2 g A 8 dA dlog D pore area dA dlog D i m2 g SAi LPi 10 2 m cm Davg i 10 10 m S...

Page 346: ...diameter 2 Cumulative Pore volume VpFcum i cm3 g where INTERP x is the value interpolated from the function X Dpj i and Y VPcum i using an AKIMA semi spline interpolation 3 Incremental Pore Volume VpF...

Page 347: ...ere INTERP x is the value interpolated from the function X Davg j and Y dV dlog D j 8 dA dD pore area dA dDpFi m2 g A where INTERP x is the value interpolated from the function X Davg j and Y dA dDj 9...

Page 348: ...of opening of newly opened pores cm2 Davg average pore diameter Dp pore or core diameter F fraction of pores open at both ends from the BJH Adsorption Report Options window or the BJH Desorption Repor...

Page 349: ...a tion of average pore diameter and pore length Pore Diameter Pore diameter is determined from the Kelvin radius and thickness equation The average pore diameter is the arithmetic mean of the diameter...

Page 350: ...ned by solving one of the following equations Slit Pore Geometry original Horvath Kawazoe Cylinder Pore Geometry Saito Foley Sphere Pore Geometry Cheng Yang Slit Pore Geometry original HK When you use...

Page 351: ...th Kawazoe Physical Properties window Cylinder Pore Geometry Saito Foley When you use the Saito Foley10 method the following equation is solved for each value of P The value of L is determined when th...

Page 352: ...e pressure where 1032 the number of cm4 that are equal to 4 12 where 22 where d0 where DA molecular diameter from the Horvath Kawazoe Physical Properties window DS diameter of sample atom from the Hor...

Page 353: ...G L one of the Horvath Kawazoe equations given above degree of void filling is estimated by first computing the monolayer capac ity Qm with the Langmuir equation over the range of data points from re...

Page 354: ...ple atoms cm3 mc2 kinetic energy of electron 0 8183 10 6 erg A diamagnetic susceptibility of gas molecule cm3 where NA number of gas molecules cm2 at monolayer from the Horvath Kawa zoe Physical Prope...

Page 355: ...n Pore Width where Dl pore width Li that corresponds to Vl Dg pore width Li that corresponds to Vg Vcum n total cumulative pore volume Vcum i for points designated for Horvath Kawazoe calculations Vg...

Page 356: ...e 298 15 Carbon Ross Olivier value Carbon Horvath Kawazoe value Zeolite 4 20 9 20 5 08 273 15 Carbon Ross Olivier value Carbon Horvath Kawazoe value Zeolite 4 34 9 35 5 22 194 65 Carbon Ross Olivier v...

Page 357: ...Saito Foley are Carbon Graphite Zeolite DS 3 40 DS 3 04 NS 3 845 1015 NS 3 75 1015 S 1 05 10 29 Ross Olivier S 1 94 10 29 13 5 10 29 Horvath Kawazoe implicit S 0 85 10 24 S 1 02 10 24 Nitrogen Argon...

Page 358: ...therefore the convolution of an adsorption process with the distribution of one or more properties which affect that process This was first stated mathematically by Ross and Olivier12 for the case of...

Page 359: ...p on an ideal free surface of energy and f the total area of surface of energy in the sample The exact form of the energy dependent term depends on the form of the model isotherms expressed in the ke...

Page 360: ...ns window as a selection of tables or graphs Regularization DFT allows a selectable regularization also referred to as smoothing constraint to be applied during the deconvolution process to avoid over...

Page 361: ...ed for Dubinin Radushkevich calculations the following calculations are done The intercept log Vo can be found by performing a least squares fit on the LP LV designated pairs where LP is the independe...

Page 362: ...lative to the Po gas from the Dubinin Adsorptive Options window E0 characteristic energy kj mol N Astakhov exponent may be optimized or user entered from the Dubinin Report Options window P equilibriu...

Page 363: ...ing the value of N that gives the smallest standard error of the y intercept The exponent N is optimized to within 10 4 If the optimum value for N is not found in this range an exponent of 2 is used T...

Page 364: ...rgy KJ mol Modal Equivalent Pore Diameter where affinity coefficient of the analysis gas relative to the Po gas from the Dubinin Adsorptive Options window Maximum Differential Pore Volume cm3 g This v...

Page 365: ...the domain 0 1 where b1 0 57719 1652 b2 0 98820 5891 b3 0 89705 6937 b4 0 91820 6857 b5 0 75670 4078 b6 0 48219 9394 b7 0 19352 7818 b8 0 03586 8343 and where Equivalent Pore Diameter Dmean 2 10 3 nm...

Page 366: ...f the line defined by two consecutive interpolated points The slopes of each pair of consecutive points from the origin to the last point must be monotonically decreasing and non negative With the int...

Page 367: ...ace area for the ith point m2 g Incremental pore volume occluded for the ith point cm3 g Cumulative pore volume occluded for the ith point cm3 g dV dR pore volume for the ith point cm3 g dA dRi Sinci...

Page 368: ...rve calculations C1 parameter 1 C2 parameter 2 C3 parameter 3 Prel i relative pressure for the ith point mmHg ti thickness for ith point Kruk Jaroniec Sayari Halsey Halsey5 Harkins and Jura Harkins an...

Page 369: ...E Publications McGraw Hill p 16 If there is only a single point or all N points have the same x value there can be no line of best fit in the standard form Slope The coefficient of Correlation for thi...

Page 370: ...gle point Surface Area m2 g where P pressure closest to 0 3 of the relative pressure points designated for surface area calculations Q quantity adsorbed corresponding to P b Multi point Surface Area S...

Page 371: ...t Plot Micropore Pore Volume See t Plot calculations k Freundlich See Freundlich calculations l Temkin See Temkin calculations m Alpha S See Alpha S calculations n DFT Pore Size and DFT Surface Energ...

Page 372: ...total Scum i see MP method Calculations for the last collected data point used in the MP method Calculations and the range of hydraulic pore radii over which the cumulative surface area was computed u...

Page 373: ...2 1871 8 Barrett E P Joyner L S and Halenda P P J Am Chem Soc 73 373 380 1951 9 Horvath G and Kawazoe K J Chem Eng Japan 16 6 470 1983 10 Saito A and Foley H C AlChE Journal 37 3 429 1991 11 Cheng Lin...

Page 374: ...Appendix C ASAP 2460 Operator s Manual C 50 246 42800 01 Aug 2013...

Page 375: ...tity of gas The total quantity of gas in the partly immersed sample holder cannot simply be determined using n PV RT because temperature is not constant over the total volume but instead is distribute...

Page 376: ...e file Enter the analysis bath temperature found on the po and Temperature dialog Enter the sample mass and density found on the Sample Information dialog Enter This method allows you to enter predete...

Page 377: ...trument Use metal gas lines only Remove trapped air from the regulator and gas lines Using Metal Gas Lines You should always use metal gas lines which have been carefully cleaned of any oils and greas...

Page 378: ...ing trapped air 1 Go to Unit Enable Manual Control if the instrument schematic is not displayed select Show Instrument Schematic 2 Close all valves by right clicking on each valve and selecting Close...

Page 379: ...02 MPa then tighten the fitting 7 Repeat steps 4 5 and 6 three times 8 Briefly open the gas bottle valve then using the Pressure Control knob reset the regulator output pressure to 15 psig 9 After th...

Page 380: ...d fall close to zero 5 Close valves 6 7 and 10 The regulator is filled with gas Close the gas bottle valve Open the regulator Shut off valve Loosen the helium inlet fitting or nut on the rear panel of...

Page 381: ...ateral interaction of adsorbed molecules with each other Other theo ries such as the Dubinin Astakhov approach also include parameters for the effect of adsorbent porosity Instead of this classical ki...

Page 382: ...ervals This method takes into account both the forces acting between the gas particles themselves and those acting between the gas particles and the atoms of the simulated surface As the simulated par...

Page 383: ...d The bulk fluid is a homogenous system of constant den sity its chemical potential is determined by the pressure of the system using well known equations The fluid near the walls is not of constant d...

Page 384: ...adsorption iso therm for the model If the value of H is very large the isotherm obtained corresponds to that of an external or free surface If H is smaller a range of pressures is reached where two m...

Page 385: ...the critical pore filling pressure In inset c the profile shows the density decreasing to near zero actually the bulk gas density at 4 or 5 molecular diameters from the surface Inset d shows the profi...

Page 386: ...Model Isotherms for Some Larger Pore Widths Argon on Carbon at 87 3 K Figure D 4 shows model isotherms for pores in the micropore size range Note the logarithmic scale for pressure Figure D 4 Model Is...

Page 387: ...near 1 00 relative pressure These models are identical to those supplied with the original DOS version of DFT software Some slight difference from the DOS results may be noted when they are applied t...

Page 388: ...s Pillared Clay Surface Montmorillionite Model isotherms were calculated using a combination of statistical thermodynamic Non Local Density Functional Theory NLDFT calculations and experimental isothe...

Page 389: ...a Pillared Interlayered Clay PILC from a Hybrid Density Functional Theory DFT Method The Journal of Physical Chemistry B 2001 105 3 623 629 M L Occelli J P Olivier J A Perdigon Melon and A Auroux Surf...

Page 390: ...ng functions and a slit like pore geometry These models are slightly different from N2 DFT and Ar DFT models that were calculated using NLDFT with density independent weighting functions The reported...

Page 391: ...n microscopy HRTEM and or X ray diffraction XRD to obtain comprehensive information about the structure of studied carbon material N2 Carbon Cylinder single wall nanotube by NLDFT Ar Argon Cylinder si...

Page 392: ...n multi wall nanotubes The reported pore size range is from 3 5 to 1000 Ar Zeolites H Form by NLDFT Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting...

Page 393: ...ave the Hill de Boer equation and the Fowler Guggenheim equation All of these suffer from the fact that they only describe monolayer adsorption whereas the data may include contributions from multilay...

Page 394: ...traditional algorithm Kernel functions corresponding to various classical Kelvin based methods have been calculated for differing geometries and included in the list of models Models Included t 3 54...

Page 395: ...gen properties used in the Kelvin equation are N2 Harkins and Jura Thickness Curve The calculation is the same as above except that cylindrical geometry is assumed Geometry Slit Substrate Average Cate...

Page 396: ...that cylindrical geometry is assumed and the film thick ness depends on pore size see reference Geometry Slit Substrate Average Category Porosity Method Nitrogen at 77 K Surface tension 8 88 dynes cm...

Page 397: ...d Catalysts on Solids Kazimierz Dolny Poland July 1992 2 Classification of Adsorption Behavior Simple Fluids in Pores of Slit shaped Geometry Perla B Balbuena and Keith E Gubbins Fluid Phase Equilibri...

Page 398: ...Appendix F ASAP 2460 Operator s Manual F 18 246 42800 01 Aug 2013...

Page 399: ...rm rel Get the isotherm data 6 iso_abs mic isotherm abs 7 or as components 8 prel qads num_ads warm_fs cold_fs mass desc mic isotherm rel 9 pabs qads num_ads warm_fs cold_fs mass desc mic isotherm abs...

Page 400: ...32 mic table addcolumn Column B Big Bigger 33 Another tabular report 34 mic table Tabular Report Two Add another table 35 mic table addtable One 36 mic table addcolumn Column A Small Smaller 37 mic t...

Page 401: ...sc sample description mic overlay overlay_number 1 press_type rel Get overlay isotherm data Keyword arguments overlay_number the overlay number 1 through 8 press_type the pressure basis use rel for re...

Page 402: ...mic adsorptive_data sample_number 0 Get adsorptive data for each sample Keyword arguments sample_number Identifier for the adsorptive data to retrieve default 0 0 the current sample file 1 through 8 t...

Page 403: ...ker a graphtype both Add a curve to the last created graphical report Keyword arguments name the curve name x list of x values must be a list of floats or convertible and the same length as y y list o...

Page 404: ...e last created table Keyword arguments header column header must be a string or convertible values column values must be a list of strings or convertible mic summary title User Summary Create a new su...

Page 405: ...Ar Carbon Finite Pores As 6 2D NLDFT model F 10 Ar Carbon Slit Pores by NLDFT model F 10 AR Cylindrical Pores Oxide Surface model F 8 AR DFT model F 7 AR Modified Density Functional Model F 9 Argon C...

Page 406: ...t 3 54 Dosing Method From last sample port 2 22 Normal 2 22 3 16 Dubinin calculations C 37 report 3 63 tabular report options 3 64 transformed isotherm plot options 3 64 Dubinin Astakhov calculations...

Page 407: ...als 1 17 High throughput analysis 2 44 High Throughput Analysis dialog 2 45 Horvath Kawazoe Cylinder pore geometry Saito Foley calculations C 27 physical properties window 3 56 report 3 55 report calc...

Page 408: ...ity Functional F 7 N2 Tarazona NLDFT Esf 30 0K F 9 Zeolites H Form by NLDFT F 12 Molecular dynamics F 2 Molecular simulation methods F 2 Monolayer capacity 3 39 3 41 Monte Carlo F 2 Montmorillionite F...

Page 409: ...nscreen 5 22 header 5 16 Heat of Adsorption 5 13 Interactive 2 1 Isotherm 3 35 Langmuir surface area 3 37 Sample log 3 72 shortcut menus for 5 20 Statistical Process Control SPC 5 5 Summary 3 33 tabul...

Page 410: ...ostic 4 32 Text copy graph data as 5 25 Thermal transpiration correction 3 32 correction calculations C 7 Thermodynamic law F 2 Thickness curve Broekhoff de Boer 3 44 Carbon Black STSA 3 44 Halsey 3 4...

Page 411: ...ASAP 2460 Operator s Manual Index 246 42800 01 Aug 2013 Index 7 X X axis order by 5 11 Z Zeolites H Form by NLDFT model F 12 Zeolites Me Form by NLDFT model F 13 Zoom feature 5 26...

Page 412: ...Index ASAP 2460 Operator s Manual Index 8 246 42800 01 Aug 2013...

Page 413: ...ASAP 2460 Operator s Manual Appendix G Aug 2013 SVP 1 SVP Smart VacPrep Operator Manual...

Page 414: ...Appendix G ASAP 2460 Operator s Manual SVP 2 Aug 2013...

Page 415: ...OPERATOR MANUAL Smart VacPrep Operator Manual Nov 2013 SMART VACPREP INTELLIGENT VACUUM SAMPLE PREPARATION SYSTEM...

Page 416: ...egistered trademark of Micromeritics Instrument Corporation _____________________________________________________________________________________ Micromeritics Instrument Corporation 2013 All rights r...

Page 417: ...e made subject to factory inspection of returned parts MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications are made by persons other than its...

Page 418: ...actures a special product to the purchaser s specifications MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its products other than the liabi...

Page 419: ...lyzer or components WARNING Warnings contain information to help prevent actions that may cause personal injury For Chemisorption Indicates the marked item is applicable to chemisorption analyzers onl...

Page 420: ...sis Conditions etc Keyboard Commands Keyboard commands are represented as bold font weight and black letters Some examples are F2 Alt F4 etc Menu Instructions Menu instructions are represented as bold...

Page 421: ...e 770 662 3636 Fax 770 662 3696 www Micromeritics com U S Inquiries U S Sales 770 662 3633 ussales micromeritics com Quotes Orders and Customer Satisfaction Customer Service 770 662 3636 orders microm...

Page 422: ...Contact Us vi Smart VacPrep Operator Manual...

Page 423: ...Smart VacPrep 3 1 Backfill the Smart VacPrep Ports 3 1 Evacuate the Smart VacPrep Ports 3 1 QuickStart Degas Conditions 3 2 Load QuickStart Degas Conditions into a Sample File 3 4 Start Smart VacPrep...

Page 424: ...6 1 Replace the Smart VacPrep Fuse 6 2 Sample Tube Installation on the Smart VacPrep 6 2 Oil Based Vacuum Pump 6 3 Inspect and Change Vacuum Pump Oil 6 3 Replace the Alumina in the Oil Vapor Trap 6 7...

Page 425: ...eters is available A record of the sample preparation time and temperature can be recorded as part of the sample data file The degas program may be started or terminated by using the analyzer software...

Page 426: ...hen be started either by pressing the Select and Start buttons on the Smart VacPrep unit or by going to Smart VacPrep Unit n Degas Start Degas A Check Seal or TransSeal can be used to transfer air sen...

Page 427: ...Width 53 cm 20 75 in Depth 44 cm 17 in Weight 32 kg 70 lbs Evacuation Period Determined by selected elapsed time or achievement of selected low pres sure target Evacuation Rate Selectable evacuation r...

Page 428: ...driver to gently pry open the cover of the compartment 2 Firmly press down on the voltage indicator and roll the indicator to display the appropriate voltage for your environment Selections are 100 Va...

Page 429: ...n IP address will be assigned to the unit allowing the unit to connect automatically during startup Up to three additional degasser units can be installed Menu options for the Smart VacPrep are provid...

Page 430: ...n prompted enter the serial number of the unit being added Duplicate serial numbers are not allowed 2 Click Add Initialization begins REMOVE A SMART VACPREP UNIT Smart VacPrep Remove 1 Select the seri...

Page 431: ...o display the Unit IP Setup window The IP address and Subnet mask assigned during installation display Do not edit these fields unless instructed by a Micromeritics service representative OK Saves and...

Page 432: ...2 About the Software 2 4 Smart VacPrep Operator Manual...

Page 433: ...ckfill pressure in the Backfill pressure field 2 Select the ports to be backfilled 3 Click Start to start the process or Cancel to stop the process EVACUATE THE SMART VACPREP PORTS Unit n Smart VacPre...

Page 434: ...lity to enter commonly used degas conditions for each Smart VacPrep port without the need for a sample information file Degassing can then be easily started using the front panel buttons on the Smart...

Page 435: ...ator Manual 4 Click Save Repeat these steps for each port to be configured If multiple ports will have the same degas conditions parameters click Edit on the port and use the Copy QuickStart Degas Con...

Page 436: ...tions from the Smart VacPrep Unit Use to copy the degas conditions settings from the selected Smart VacPrep unit and port Degas Conditions Use to browse for a DEG file that contains degas condition pa...

Page 437: ...will stop and hold the sample temperature approximately constant until the pressure falls below the Hold pressure This prevents damage to the sample struc ture due to steaming and or elutriation due...

Page 438: ...ort 5 Attach the heating mantle using the metal clip If a straight wall tube is used heating mantles with elastic cords are available Refer to the Parts and Accessories section of the analyzer oper at...

Page 439: ...dashboard numbers right click on the dashboard setting then click Reset Field or Button Description Days until roughing pump service is due Annual maintenance is recommended The number of days until...

Page 440: ...escriptions Table continued SHOW SMART VACPREP LOG Smart VacPrep Unit n Show Log Use to display a log of recent analyses calibrations or messages Field Description Add Log Entry Use to enter informati...

Page 441: ...eadsheet XLS a portable document format PDF or an ASCII text TXT file format Analyzer Log Fields and Buttons Table continued SHOW SMART VACPREP SCHEMATIC Unit n Show Instrument Schematic Use to displa...

Page 442: ...access the shortcut menu hover the mouse pointer over the component and right click Schematic Shortcut Icon Available Options Valve options l Close Closes the selected valve l Open Opens the selected...

Page 443: ...e vacuum valves are closed and the vacuum level on the selected ports is monitored l The Status window indicates that the degassing operation is being checked and displays the outgassing rate as it be...

Page 444: ...r Button Description Sample The name of the sample file Skip Skips the current degas operation Status Indicates the current status of the degas Smart VacPrep Status Fields and Buttons Table continued...

Page 445: ...lated Topics See Smart VacPrep Pressure Offset below See Smart VacPrep Servo Valve Calibration on the next page SMART VACPREP PRESSURE OFFSET Smart VacPrep Unit n Calibration Pressure Offset Use to pe...

Page 446: ...ed before starting this calibration procedure 1 Go to Smart VacPrep Unit n Calibration Servo Valve 2 Click Start The window closes when the calibration is complete Click Cancel to stop the cal ibratio...

Page 447: ...ime or periodic running of a sequence of diagnostic tests A separate list of tests is saved for each of the possible test frequencies Tests are categorized and flagged as requiring intervention or not...

Page 448: ...if the instrument is idle at any time during the entered time frame Test Frequency Select how often the test is to run unattended Test Sequence Provides the test file identification and estimated run...

Page 449: ...s not immediately visible go to Unit n Show Instrument Schematic Schematic Components Description 1 6 Sample port valves 7 8 9 Vacuum and backfill valves Heating mantle con trols Sets the ramp rate an...

Page 450: ...flat head screwdriver to gently pry the fuses out of the holder 3 Insert a new fuse into each holder then push the holders back into the slot until snug 4 Press the compartment cover shut Ensure it cl...

Page 451: ...t the heating mantle thermocouple plug into the thermocouple connector 7 Insert the heating mantle power plug into the power connector and twist the power plug to lock securely 8 After installing the...

Page 452: ...on the oil level window when the pump is running Oil in good condition is clean clear or light in color and transparent Change the oil if it has darkened Change or Add Oil Drain the oil while the pump...

Page 453: ...ain plug and drain the oil into the waste container 6 Replace the drain plug 7 Remove the drain plug from the oil fill port on top of the pump 8 Slowly add oil to the port until the level is midway be...

Page 454: ...no longer white replace the alumina before reattaching the vacuum pump See Replace the Alu mina in the Oil Vapor Trap on the facing page 10 Reconnect the vacuum pump hose 11 Reconnect the power cord t...

Page 455: ...lumina pellets are no longer white Do not perform the following procedure on used alumina The resultant oil vapors may cause a fire 1 Disconnect the vacuum pump from the analyzer and place it on a wor...

Page 456: ...y Under normal circumstances these cracks will not cause problems or leaks Prepare fresh alumina 1 Preheat the oven to 300 C 2 Pour approximately 180 grams of fresh alumina into a glass or metal conta...

Page 457: ...of the trap body 9 Screw the other end fitting back onto the trap and tighten securely by hand 10 Lightly tap both ends of the trap body on the work surface to remove remaining dust from the pel lets...

Page 458: ...amp and place it around the flange of the intake port and the flange of the trap Swing the clamp fastening screw toward the intake port until it fits into the slot in the other half of the clamp Tight...

Page 459: ...usted by the oil filled vacuum pump The filter minimizes the release of oil vapor and should be replaced when it becomes so saturated with oil that it is ineffective Exhaust filters are used to minimi...

Page 460: ...it around the exhaust port flange and the exhaust filter flange Swing the clamp fastening screw toward the exhaust port until it fits into the slot in the other half of the clamp Tighten the wing nut...

Page 461: ...URO BUNA N for use with sample port dust frit 004 27041 00 Sample port dust frit 20 microns 067 33601 00 Operating supplies sample tube o rings 1 2 in and 12 mm sample port dust frit o rings for sampl...

Page 462: ...d alumina 500 grams for oil vapor trap 004 25491 02 Centering ring NW 40 BUNA N AL for use with hybrid turbo vacuum pump 004 25509 00 Clamp NW 10 16 004 25626 08 Flex tube 3 4 in OD x 48 in long NW 16...

Page 463: ...ng it to the preferred unit 4409 A free IP address on the same subnet as s could not be found Cause All IP addresses on the network for the Ethernet card specified during installation are in use by ot...

Page 464: ...ouple is unplugged or has malfunctioned Action Ensure the thermocouple is plugged in If the problem persists contact your Micro meritics service representative 4420 Communications error Cause The appl...

Page 465: ...pen by this or another application Cause The selected sample file is damaged Action Select another sample file 4425 The sample s on port d has an invalid status and cannot be used for degassing Cause...

Page 466: ...8 Error Messages 8 4 Smart VacPrep Operator Manual...

Page 467: ...B Backfill port Smart VacPrep 3 1 C Calibration Smart VacPrep 4 1 Smart VacPrep pressure offset 4 1 Smart VacPrep servo valve 4 2 Configuration Smart VacPrep 2 3 Contact Us v D Dashboard Smart VacPrep...

Page 468: ...unit 2 1 schedule diagnostic tests 5 1 schematic 3 9 show dashboard 3 7 show status 3 11 software about 2 1 specifications 1 3 start degas 3 5 troubleshooting and maintenance 6 1 use 3 1 Soak time de...

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