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Thermo Scientific
Sorptomatic Software For Sorptomatic 1990 Operating Manual PN 317 091 28, Revision June 2007
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Sorptomatic Software - Operating Manual June 2007 Edition Part Number 317 091 28 © 2007 Thermo Fisher Scientific Inc. All rights reserved. Printed in ITALY. Published by Thermo Electron S.p.A., Strada Rivoltana 20090 Rodano - Milan Tel: +39 02 950591 Fax: +39 02 95059388 Printing History: First Edition, released A1-0698 Second Edition, released January 2002 Third Edition, released April 2004 Fourth Edition, released June 2007 Disclaimer Technical Information contained in this publication is for reference purposes only and is subject to change without notice. Every effort has been made to supply complete and accurate information; however, Thermo Fisher Scientific assumes no responsibility and will not be liable for any errors, omissions, damage, or loss that might result from any use of this manual or the information contained therein (even if this information is properly followed and problems still arise). This publication is not part of the Agreement of Sale between Thermo Fisher Scientific and the purchaser of Thermo Fisher Scientific system. In the event of any conflict between the provisions of this document and those contained in Thermo Fisher Scientific Terms and Conditions, the provisions of the Terms and Conditions shall govern. Reference to System Configurations and Specifications supercede all previous information and are subject to change without notice. Trademarks Sorptomatic Software and Sorptomatic 1990 are trademarks of Thermo Fisher Scientific Inc., and its subsidiaries. Other brand and product names may be trademarks or registered trademarks of their respective companies.
Contents About This Manual.................................................................................................................................ix Overview ................................................................................................................................... ix Conventions Used in This Manual............................................................................................. x
Chapter 1 Software Overview............................................................................................................................. 11 Introduction .............................................................................................................................. 11 Software Sorptomatic 1990 Installation................................................................................... 12
Chapter 2 Getting Started................................................................................................................................... 15 Main Menu Overview .............................................................................................................. 16 Bar Pull-Down Menu .................................................................................................. 17 Remark Box ................................................................................................................ 17 Icons Bar ..................................................................................................................... 17 Software Version Area................................................................................................ 18 Main Menu Sections Dialog Windows ....................................................................... 18 Bottom Line ................................................................................................................ 18 File Menu ................................................................................................................................. 19 Open ............................................................................................................................ 19 Save............................................................................................................................. 19 New ............................................................................................................................. 20 Instrument (1-4) .......................................................................................................... 20 Last File (A-D)............................................................................................................ 20 Exit .............................................................................................................................. 21 View Menu............................................................................................................................... 22 View Results ............................................................................................................... 22 Pore Distribution Results ............................................................................................ 24 File ................................................................................................................. 25 Edit................................................................................................................. 25 Report Menu............................................................................................................................. 25 Menu Overview........................................................................................................... 26 Report Option Page Buttons ....................................................................................... 26 Report Options Page Sections..................................................................................... 27 Title Section ................................................................................................... 27 Parameters Section......................................................................................... 28 Results Section............................................................................................... 28 Pore Distribution Results Section .................................................................. 29
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Data Report Section....................................................................................... 29 Custom Report Section............................................................................................... 30 Graph(s) Section............................................................................................ 31 View Graphs Menu.................................................................................................................. 33 Graph Menu Overview ............................................................................................... 33 Graph Menu................................................................................................................ 35 Method Menu ............................................................................................................. 36 Scale Menu ................................................................................................................. 37 Results Menu .............................................................................................................. 37 The Pore Size Distribution Range Table ....................................................... 38 Regions Menu............................................................................................................. 39 Marker Menu .............................................................................................................. 40 Print Menu .................................................................................................................. 40 Overlay Menu ............................................................................................................. 41 Load Overlay ................................................................................................. 41 View Overlay................................................................................................. 42 Autoscaling.................................................................................................... 42 Edit Data Points Menu............................................................................................................. 43 Edit Row Data Point ................................................................................................... 43 Instruments Serial Ports Menu................................................................................................. 45 Instrument Serial Port Submenu................................................................................. 45 Acquire Points ......................................................................................................................... 46 Sorptomatic Control................................................................................................................. 47 Remark..................................................................................................................................... 47 Help Menu ............................................................................................................................... 47 Main Menu Sections ................................................................................................................ 47
Chapter 3 Main Menu Sections...........................................................................................................................49 Introduction.............................................................................................................................. 50 Sample Information ................................................................................................................. 51 General Information Group Boxes ............................................................................. 51 Sample Mass (g) ......................................................................................................... 52 Sample Density........................................................................................................... 52 Acquisition Parameters............................................................................................................ 53 Adsorption Group Boxes ............................................................................................ 53 Desired points................................................................................................ 53 Equilibrium deviation.................................................................................... 54
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Equilibrium Time........................................................................................... 54 P/P0 regions ................................................................................................... 54 Piston filling volume...................................................................................... 54 Max Ads pressure .......................................................................................... 54 Min Saturation pressure ................................................................................. 55 Initial load pressure........................................................................................ 55 Prep-run time (min)........................................................................................ 55 Desorption Group Boxes............................................................................................. 55 Desired points (Des) ...................................................................................... 55 Equilibrium deviation .................................................................................... 56 Equilibrium Time (min)................................................................................. 56 P/PO regions .................................................................................................. 56 Piston filling volume...................................................................................... 56 Last Des pressure ........................................................................................... 56 Analysis type Box ....................................................................................................... 56 Saturation pressure Box .............................................................................................. 56 Analytical Conditions............................................................................................................... 57 Fill with gas data ........................................................................................................ 58 Left Section and Gas used data Group Boxes............................................................. 59 Gas molecular weight .................................................................................... 59 Gas molecular area......................................................................................... 59 Liquid gas density .......................................................................................... 59 Liquid gas surface tension ............................................................................. 59 Monolayer thick. ............................................................................................ 59 2nd virial coefficent burette temperature....................................................... 59 2nd virial piston temperature ......................................................................... 59 Righ Section Group Boxes.......................................................................................... 60 Blank slope..................................................................................................... 60 Blank intercept ............................................................................................... 60 Instrument hysteresis ..................................................................................... 60 Bottom Section Group Boxes ..................................................................................... 60 Burette temperature (°C)................................................................................ 60 Correct slope/Intercept................................................................................... 61 Instrument Parameters.............................................................................................................. 61 Stroke Volume Group Boxes ...................................................................................... 62 Total stroke Volume ...................................................................................... 62 ½ stroke Volume............................................................................................ 62 ¼ stroke Volume........................................................................................... 62
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Piston Group Boxes .................................................................................................... 62 Piston dead Volume....................................................................................... 62 Piston temperature ......................................................................................... 62 Calculation Parameters ............................................................................................................ 63 Surface Area calculation method................................................................................ 63 B.E.T.............................................................................................................. 63 Dubinin .......................................................................................................... 64 Initial and Final (P/P0) .................................................................................. 64 Initial and Final log²(P0/P) ............................................................................ 64 Pore size calculation method ...................................................................................... 64 Smoothing Pore distribution convolution points........................................... 64 Pore specific volume at P/P0 ...................................................................................... 64 Pore Distribution Range ............................................................................................ 65 Buttons........................................................................................................... 65 Report Selection....................................................................................................................... 67 Report From Group Box............................................................................................. 68 Pore size distribution range from................................................................................ 68 How to Use the Memorize Button.............................................................................. 68 Digital Status Display .............................................................................................................. 70 Introduction ................................................................................................................ 70 File Menu.................................................................................................................... 72 Instrument Serial Port................................................................................................. 73 Run Menu ................................................................................................................... 73 Start................................................................................................................ 73 Stop................................................................................................................ 73 Reset .............................................................................................................. 73 Calibration Menu........................................................................................................ 73 Transducer Calibration using pressure of today ............................................ 73 Transducer Calibration using CPU 1990 ID Number ................................... 74 Calibration P0 Saturation .............................................................................. 74 Display the data during transducer calib. ...................................................... 74 Load from disk a modification inside prg. to SO1990 .................................. 74 Acquisition Parameters Menu .................................................................................... 75 Other Menu................................................................................................................. 76 Leak test......................................................................................................... 76 Change gas..................................................................................................... 77 Menu Menu................................................................................................................. 77 Command Buttons ...................................................................................................... 77
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Chapter 4 Running Analyses ............................................................................................................................. 81 Sorptomatic Main Menu .................................................................................................................... 6 File Menu ...................................................................................................................................... 9 View Menu ...................................................................................................................................... 12 Report Table ...................................................................................................................................... 12 Pore Size Distribution Results Window ............................................................................................ 14 Report Menu ...................................................................................................................................... 15 Report Options Page .......................................................................................................................... 15 Custom Report Dialog Window ........................................................................................................ 20 Graph Menu ...................................................................................................................................... 23 View Graphs Page ............................................................................................................................. 23 Load Overlay Window ...................................................................................................................... 31 Edit Data Points Page ........................................................................................................................ 34 Sample Information Dialog Window. ............................................................................................... 41 Acquisition Parameters Dialog Window ........................................................................................... 43 Analytical Conditions Dialog Window ............................................................................................. 48 Gas Used Data Page .......................................................................................................................... 49 Instrument Parameters Dialog Window ............................................................................................ 52 Calculation Parameters Dialog Window ........................................................................................... 54 Pore Distribution Range Table Page ................................................................................................. 56 Report Selection Dialog Window ..................................................................................................... 58 The Digital Status Display Dialog Window ...................................................................................... 61 Example of Mesoporous Page ........................................................................................................... 66
Operating Procedures Running the Blank and Sample Analysis .......................................................................................... 82
Figures Sorptomatic Main Menu .................................................................................................................... 16 File Menu ...................................................................................................................................... 19 View Menu ...................................................................................................................................... 22 Report Table ...................................................................................................................................... 22 Pore Size Distribution Results Window ............................................................................................ 24 Report Menu ...................................................................................................................................... 25 Report Options Page .......................................................................................................................... 25 Custom Report Dialog Window ........................................................................................................ 30 Graph Menu ...................................................................................................................................... 33
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View Graphs Page ............................................................................................................................. 33 Load Overlay Window ....................................................................................................................... 41 Edit Data Points Page ........................................................................................................................ 43 Sample Information Dialog Window. ................................................................................................ 51 Acquisition Parameters Dialog Window ........................................................................................... 53 Analytical Conditions Dialog Window .............................................................................................. 57 Gas Used Data Page ........................................................................................................................... 58 Instrument Parameters Dialog Window ............................................................................................. 61 Calculation Parameters Dialog Window ............................................................................................ 63 Pore Distribution Range Table Page .................................................................................................. 65 Report Selection Dialog Window ...................................................................................................... 67 The Digital Status Display Dialog Window ......................................................................................70 Example of Mesoporous Page ........................................................................................................... 75
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About This Manual Overview This manual is organized as follows: Chapter 1, Software Overview, contains the instruction to install the software for Sorptomatic 1990. Chapter 2,Getting Started, contains general informations and the description of the active items amd menu commands. Chapter 3, Main Menu Sections, contains the description of the active items and commands of the Main Menu Sections and Digital Status Display (DSD). Chapter 4, Running Analyses, contains the operating sequence to running the blank and sample analysis by using the software for Sorptiomatic 1990.
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About This Manual
Conventions Used in This Manual
Conventions Used in This Manual The following symbols and typographical conventions are used throughout this manual. Bold
Bold text indicates names of windows, menus, dialog boxes, buttons, and fields.
Italic
Italic indicates cross references, first references to important terms defined in the glossary, and special emphasis.
Monospace
Monospace, or Courier, indicates filenames and filepaths, or to indicate text the user should enter with the keyboard.
Monospace Bold
Monospace Bold indicates messages or prompts displayed on the computer screen or on a digital display.
»
This symbol illustrates menu paths to select, such as File»Open…. CAUTION
This symbol alerts you to an action or procedure that, if performed improperly, could damage the instrument.
NOTE
This symbol alerts you to important information related to the text in the previous paragraph.
This symbol alerts you to an action or sequence that, if WARNING! improperly performed, could result in damage to the instrument or possible physical harm to the user. This symbol may be followed by icons indicating special precautions that should be taken to avoid injury.
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1 Software Overview This chapter contains the instruction to install the software for Sorptomatic 1990.
Chapter at a Glance… Introduction .......................................................................................................... 11 Software Sorptomatic 1990 Installation ............................................................... 12
Introduction Please take into consideration the following remarks and specifications: •
The Sorptomatic 1990 software is designed to run under Windows® 2000/XP operative system
•
All printers supported by operative system can be used for report printout
•
Minimum computer specifications: - processor Pentium III or better - 256 Mb ram memory - 40 Gb hard disk memory - 1 serial port availability for each instrument connected (maximum 4).
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Chapter 1 Software Overview
Software Sorptomatic 1990 Installation
Software Sorptomatic 1990 Installation The Software Sorptomatic 1990 is dedicated to the acquisition and processing of data obtained with the Sorptomatic 1990; the software (Post-Run Calculations only) provides all information related to the porosity of an analyzed solid sample. To install the software, introduce the CD in the PC drive. Through the Windows commands Start-Run, start the program Setup that is in the CD. The Setup program requests disk/directory to transfer files: if the Next key is pressed, the program will create a directory \Thermo\Sorptomatic.
At the end of the installation, an icon will appear in the list ‘Programmes’ of the ‘Start’ menu. Clicking on this icon the program Sorptomatic can be started. The icon may be easily moved using the ‘Application bar...’ of the menu ‘Setup’ in the menu ‘Start’. Setup also creates a subdirectory \Data, where some example analyses can be found. The program to run Sorptomatic 1990 is SorptWin.exe. The other files used by the software are : •
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HorvKaw.def - table for the Horvath/Kawazoe calculation
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•
Sorpt.hlp - help file
•
Sorpt_it.hlp - help file (Italy)
•
Logo.bmp - bitmap file of the Thermo logo
•
Setup also transfers into the directory \Windows\System the following drivers:
•
VCF132.ocx
•
MFCANS32.dll
•
OC30.dll
•
MSVCRT20.dll
Then the software creates a subdirectory \TMP, where the data of the four analyses in memory are saved (Tmp_1.tmp, Tmp_2.tmp,...). It also generates two files of setup and configuration, SorptW.ini and ReportSo.ini, in the \Sorptomatic directory.
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Software Sorptomatic 1990 Installation
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2 Getting Started This chapter contains general informations and the description of the active items amd menu commands.
Chapter at a Glance… File Menu.............................................................................................................. 19 File Menu.............................................................................................................. 19 View Menu ........................................................................................................... 22 Report Menu......................................................................................................... 25 View Graphs Menu...............................................................................................33 Edit Data Points Menu.......................................................................................... 43 Edit Data Points Menu.......................................................................................... 43 Instruments Serial Ports Menu .............................................................................45 Help Menu ............................................................................................................ 47 Help Menu ............................................................................................................ 47 Main Menu Sections............................................................................................. 47
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Chapter 2 Getting Started
Main Menu Overview
Main Menu Overview The Main Menu includes all options for processing the data acquired with the instrument Sorptomatic 1990 (files xxx.199). The heading of the Main Menu window also reports the software version and, between brackets, the original file name of the data in memory.
Figure 2-1. Sorptomatic Main Menu Main Menu is the starting point to enter all menu and relevant functions. It consists of the following sections:
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•
Bar Pull-Down Menus
•
Remark Box
•
Icons Bar
•
Software Version Area
•
Main Menu Dialog Windows
•
Button Line
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Main Menu Overview
Bar Pull-Down Menu It allows to access the following pull-down menus: Menu
Refer To:
Menu
Refer To:
File
File Menu on page 19
Edit Data Points
Edit Data Points Menu on page 43
View
View Menu on page 22
Instrument Serial Port
Edit Data Points Menu on page 43
Report
Report Menu on page 25
Help
Help Menu on page 47
Graphs
View Graphs Menu on page 33
Remark Box It displays a comment to the analysis. •
To enter a test Press the mouse left button with the cursor inside the textbox, write the desired comment and then press ENTER ot the mouse button again. The entered command will be saved with the parameters of the analysis and it will be displayed each time the analysis is loaded
Icons Bar It allow to activate a function by clicking on the correspondent icon. Icon
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Description
Refer To:
Open (Load Analysis)
page 19
Save (Analysis)
page 19
Results (View Results)
page 22
Pore Distribution Results
page 24
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Main Menu Overview
Icon
Description
Refer To:
Report
page 25
View Graphs
page 33
Instrument (1-4)
page 20
Acquire Points
Instruments Serial Ports Menu on page 45
Sorptomatic Control
Help Menu on page 47
Software Version Area It reports the software version and, between brackets, the original file name of the data in memory.
Main Menu Sections Dialog Windows In the middle of the window there are five main sections that contain the major information of the analysis in memory. Refer to Main Menu Sections on page 47.
Bottom Line It reports the number of points acquired in the Adsorption and Desorption stage, and also the run time of the analysis.
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File Menu
File Menu This menu, shown in Figure 2-2, allows to access the following functions:
Figure 2-2. File Menu
Open This function loads an analysis previously stored on disk. If no analysis has yet been acquired, load one from the subdirectory\Data in the directory chosen during the software installation. When an analysis is loaded, the data of the analysis in memory are replaced, and therefore lost, if one or more parameters have been changed, first execute a Save command to save the data memorized on disk.
Save To save the data memorized on disk. The disk should be organized by preparing specific directories, named according to the operator’s convenience (by \Month or by \Type of sample or by \Name etc...). This will allow to find useful analyses even after a long time.
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File Menu
When Save is executed, the currently active The Pore Size Distribution Range Table is saved with the analytical data.
New To create a new set of analytical parameters starting from the data currently in memory. The unnecessary data can be deleted; i.e., in the displayed window, click on the section Sample Information and click on Delete Ads/Des points; this will cause all data of Sample Information and all points (Ads/Des) to be deleted, whereas the data of Acquisition parameters and Analytical conditions are maintained. When New is exited by pressing OK, the file name to be saved on disk will be requested; after the confirmation, the new data will be saved. The Sample information and the points acquired from the instrument can be completed later on.
Instrument (1-4) When more than one instrument is available, a different number should be assigned to each instrument, and that number should be used for the data processing and acquisition in the Main Menu as well as for the software controlling the instrument (Refer to Digital Status Display). The Sorptomatic 1990 software can control 4 instruments, and it can simultaneously keep in memory 4 different analyses related to each instrument. To shift from one analysis to the other, move the cursor to the corresponding number on the buttons bar of the Main Menu and press the mouse left button. Alternatively, in the File menu, move the cursor to one of the rows numbered 1-4 and press the mouse left button. The file name from which all data in memory are drawn is reported in the heading at the top of the Main Menu.
Last File (A-D) List of the 4 last files loaded in memory independently of the instrument selection. Click on the row of a file to load it in memory. NOTE
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By selecting one of the rows numbered 1 to 4, one of the analyses in memory is activated, whereas by selecting one of the rows A to D, the file from disk is loaded.
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File Menu
Exit To exit the Sorptomatic 1990 software. When Sorptomatic 1990 is closed, the data of the 4 analyses in memory are saved in 4 temporary files (Tmp_1.TMP, Tmp_2. Tmp,..) in the directory TMP. When Pascal is started again, the data are relocated in memory. CAUTION
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The original file of the data (see the file path and name in the header line of the Main Menu) is not updated. To save permanently the data on disk, use the function ‘Save’ in the File Menu.
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View Menu
View Menu This menu, shown in Figure 2-3, allows to access the following functions:
Figure 2-3. View Menu
View Results Selecting this function, the following table is displayed.
Figure 2-4. Report Table
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View Menu
Results
Description
Calculation Method
Initial P/P0 - Final P/P0 Monolayer volume (cm³/g) Specific surface area (m²/g) C value of BET equation Correlation factor Pore specific volume (cm³/g) Pore specific volume at P/P0 Total Adsorbed volume (cm³/g)
Calculation Method
Initial Log²(P0/P) - Final Log²(P0/P) Monolayer volume (cm³/g) Specific surface area (m²/g) Correlation factor Micropore volume (cm³/g) Total Adsorbed volume (cm³/g)
Pore size calculation method
Dol./Heal B.J.H. Horv./Kaw. Cumulative area max. (m²/g) Pore volume max. (cm³/g)
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View Menu
Pore Distribution Results Selecting this function, the following window is displayed:
Figure 2-5. Pore Size Distribution Results Window The window displays the following results for the ranges set in the The Pore Size Distribution Range Table saved with the analytical data when Report from=None has been set in Report Selection. •
Pore Range
•
Radius or Diameter
•
Relative % Volume
•
Comulative Volume%
•
Relative Volume
•
Comulative Volume
If in Report selection a Report from other than None is set and the option Pore size from... is ticked, the table used is the one memorized in that kind of report.
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Report Menu
File The File command can be used to save (Save as...) the report in a text file (nnnn.TXT) or Excel file (nnnn.XLS). Choose the desired format in the save menu displayed selecting from the pulldown menu of the Save as… function.
Edit To use the Edit function in the sheet, first select the cells to be edited with the comands: Cut, Copy, Paste, Format cells.
Report Menu This menu, shown in Figure 2-6, allows to create a report.
Figure 2-6. Report Menu Selecting Creation, the following page is displayed.
Figure 2-7. Report Options Page
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Report Menu
Menu Overview Here you select and set the different options to print a report. If the settings have to be saved, first select one of the 20 reports in Report Selection of the Main Menu, create the report with Report Options, then press Memorize in the Report selection section of the Main Menu. In the window heading, after Report Options, the type of report, which contains the selected or set options is displayed between brackets. Report Options page consists of eight sections and a series of active buttons. Refer to Report Option Page Buttons on page 26 and Report Options Page Sections on page 27.
Report Option Page Buttons The following active button are present: Button
Description
PREVIEW
To display, in the window below the PREVIEW button, a print preview of a page of the report. The graph displayed in the print preview is complete with the curve only if Report Options opened from the View Graphs page. In this case it is still possible to print a report only showing the same graph displayed on the screen. When Report Options is opened from the Main Menu, the graphs in the print preview are displayed only with scales and profile. The curve in any case will be completely plotted during printing. In this case the report can contain all the graphs that can be selected. The print preview is updated only when pressing PREVIEW. If, after the print preview selection, a parameter for the report printing is changed, it will be necessary to press the PREVIEW button again to see the report updated with the new entry.
ZOOM
Zoom + : magnifies the print preview to make the report text readable; use the vertical and horizontal scroll bars to move inside the magnified preview. Zoom - : shows the report full page in the window below the Zoom button.
NEXT
The print preview can display only one report page at a time.
BACK
To go back to the previous page in the print preview
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Report Menu
Button SHEET
Description To create the report (not the graphs) in an Excel type sheet. To use the Edit function in the sheet, first select the cells to be edited with the commands Cut, Copy, Paste, Format cells. The File command can be used to save (Save as...) the report in a text file (nnnn.TXT) or Excel file (nnnn.XLS) to choose in the save menu displayed, the desired format using the pulldown menu of the Save as.. function.
FONT
It allows to choose the Font, the size and style of characters to be used in the report print. By the option Print Preview, it is possible to check how the report appears with the selected Font. If with certain fonts the Print Preview appears
PRINT
To send the report to the selected printer after all print options have been set in the displayed menu.
EXIT
To exit Report Options. If you want to save the settings of Report Options for future operations, select one of the 20 reports and press the MEMORIZE button in the section Report Menu.
Report Options Page Sections Report Option page contains eight sections:
Title Section The title is printed at the beginning of the Report and may consist of a logo, file information, type of instrument, sample name and a comment. Function
Description
Logo
Click on this check box to print the logo.
Instrument type
In the heading choose one or more parameters among those displayed by clicking on the corresponding check box. If Comment has been selected, enter your text in the textbox below.
Sample name Filename Software version Date Comment
Use these buttons to define the position in the report
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Report Menu
Function LOAD
Description Use this button to load the logo previously saved in a BMP. File.
Parameters Section It allows to print the parameters set in the 5 sections of the Main Menu. Function
Description
Sample information Acquisition Parameters Analytical Conditions Instruments Parameters Calculation Parameters
NONE/ALL
Tick (v) the sections to be printed. The alignment of parameters is automatic. The Sorptomatic program centers in the middle of the page as many parameters as possible, according to the number of sections required and to the Font selected. Select this button to simultaneously select all the functions.
Results Section Select the check boxes of the results that have to be printed. Function
Description Click the revelant check box to select the results that have to be printed.
Use these buttons to define the position in the report
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Report Menu
Function NONE/ALL
Description Select this button to simultaneously select all the functions.
Pore Distribution Results Section It prints the results of the check boxes ticked: Function Relative volume % Cumulative Volume%
Description Click the relevant check box to select the function required.
Relative Volume Cumulative Volume
Use these buttons to define the position of the results. NONE/ALL
Select this button to simultaneously select all the functions.
Data Report Section It prints the data of Adsorption and Desorption for all the points acquired. Function
Description Click the relevant check box to select the data to print.
Use these buttons to define the position of the data. NONE/ALL
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Select this button to simultaneously select all the functions.
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Report Menu
Custom Report Section Selecting this section, the following dialog window is displayed
Figure 2-8. Custom Report Dialog Window In the report up to 5 sets of data can be printed in 5 columns, each with Type of parameter, Label, Unit, Format number and Derive set. To have the Custom report printed, tick the box Custom report enabled. Using the alignment buttons, arrange the position of the columns (left, middle, right). Option
30
Description
12345
Use these buttons to select the column to be edited. It is recommended to always select the first free column.
Type of parameters
To choose the datum for which the value has to be printed; select one of those available in the box.
Label
Name of the column heading. To change the name, enter in the box a new one.
Unit
Unit of measure in the column heading. To change the unit, enter in the box the desired one.
Format number
To set the number of figures to be printed for the datum (e.g. Format number = 4 to print 4 decimals, 0 to print integers).
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Report Menu
Option
Description The result of the parameter selected for the active column is summed to and/or multiplied by the values entered in the boxes and then printed in the report; to enable this option tick the box Derive.
Derive
Printed value = [( Result + Value1) * (Value2) + (Value3) * (Value4)] Custom Report enabled
Click this check box to enable custom report.
Default
The columns are edited with preset parameters. Use these buttons to define the position of the data
Graph(s) Section Through Report Options in the Main Menu, it is possible to print one or more graphs in the report. Select the graphs to be printed by ticking the corresponding check box in the Graph required option. Option
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Description
Compressed graphs
It is always enabled; by ticking this box the required graphs are printed in a reduced format.
Graph Required
Select the graphs to be printed by ticking the corresponding check box.
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Report Menu
Option Set scale
Description The scale used for graphs may be chosen between: - Autoscale
To use the scales calculated by the software to have the complete curve displayed in the graph. - Selected Regions
To use the memorized scales using the STORE GRAPH REGIONS button in the View graphs Menu. When Report Options is opened from the View Graphs page, the small boxes in Graph required are disabled, because the graph printed in the report is the same as that displayed in the View Graphs page. Refer to View Graphs Menu. PREVIEW
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Using this button, the graph displayed in the print preview is complete with the curve only if Report Options is opened from the View Graph page.
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View Graphs Menu
View Graphs Menu This menu, shown in Figure 2-9, allows allows to see a graph chosen among the four available ones.
Figure 2-9. Graph Menu Selecting View Graphs, the following page is displayed:
Figure 2-10. View Graphs Page
Graph Menu Overview Different options for the scale, the type of graph and the type of print can be found in the Menus and/or in the Buttons bar in the upper section of the window.
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•
All values of initial and full scale can be changed from the keyboard: Move the arrow cursor on the value that has to be changed and press the mouse left button. The box (Edit) to enter the new value will appear, then press ENTER to confirm.
•
A portion of the graph can always be magnified: Move the arrow cursor inside the drawing to the upper left point of the graph portion to be magnified. Keeping it depressed, drag the angle of the rectangle that appears downwards to the right as far as the desired point then release the
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View Graphs Menu
mouse button. The software draws the graph again magnifying the selected portion. •
To restore the graph original size (Home graph) press the right button of the three Buttons displayed at the right upper angle of the graph.
•
The values with relevant units of measure reported on the top of the graph refer to the position of the arrow cursor when the latter is inside the graph.
•
The methods and ranges to be used for the calculation of the surface area. The method of calculation of pore size distribution can be selected in this page. If one or more parameters are changed, before closing View Graphs, the software asks whether changes have to be accepted. If confirmed, changes will be reported in the corresponding boxes in the sections of the Main Menu.
•
The settings of Grid and Point marker are maintained also for printing graphs in the Report.
•
It is possible to overlay different analyses in the graph using the option View Overlay; the overlay menu allows to choose the analyses to be displayed, the color of the curve and the result required for each superposed analysis.
•
When analyses are overlaid, two currently not visible boxes appear in the page. The top box reports, in the color chosen for that analysis, the path and file name of the analysis. Two arrows (Up/Down) next to the box allow to scroll the loaded analyses. If the path and file name exceed the extent of the box, move the cursor inside the box using the arrow keys Left/Right on the keyboard.
•
The box at the bottom of the page reports the type of result and the calculated value referred to the analysis identified in the box at the top of the page.
The View Graph page contains the following pull-down menus and relevant icons and buttons. Menu
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Refer To:
Graph
Graph Menu on page 35
Method
Method Menu on page 36
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View Graphs Menu
Menu
Refer To:
Scale
Scale Menu on page 37
Results
Results Menu on page 37
Regions
Regions Menu on page 39
Marker
Marker Menu on page 40
Print
Print Menu on page 40
Overlay
on page 41
Graph Menu Choose the graph to be displayed among: Submenu
Icon
Description
Ads/Des Isotherm
Graph of the adsoption and desorption isotherm plotted using the equilibrium pressures acquired from the instrument.
B.E.T.or Dubinin plot
The graph is plotted using the pressures of relative equilibrium and the corresponding values calculated with the B.E.T or Dubinin equation. The graph also shows a straight line plotted with the linear regression of the points ranging within the limits chosen by the operator. The points used for the calculation are highlighted in a different color.
Cumulative area
Cumulative area calculated according to the required method : Dollimore/Heal, B.J.H. or Horvath/Kawazoe.
Pore distribution curve
Pore size distribution calculated according to the required method: Dollimore/ Heal, B.J.H. or Horvath/Kawazoe using DV/DR.
Pore distribution histog.
Pore size distribution calculated according to the required method: Dollimore/ Heal, B.J.H. or Horvath/Kawazoe using the histograms selected in Pore size distribution range.
Edit data point
To display the values of volume and pressure for each acquired point (see Edit Data Points Menu).
Exit
To exit View graphs and go back to the Main Menu.
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View Graphs Menu
Method Menu Choose the desired method between the following options: Option
Icon
Description
B.E.T.method for surface area calc.
To use the B.E.T. equation for plotting the graph. Define the area where the linear regression must be applied by magnifying the concerned region or by directly entering the initial and full scale, then activate the option Use actual scale for surf.area calc..
Dubinin method for surface area calc.
To use the Dubinin equation for plotting the graph. Define the area where the linear regression must be applied by magnifying the concerned region or by directly entering the initial and full scale, then tick the option Use actual scale for surf.area calc..
Use actual scale for surf. area calc.
To use the actual scale of the graph as area for the B.E.T. or Dubinin calculations. The scale may be changed either by magnifying a portion of the graph or by directly entering the initial and full scale after having moved the cursor on the value and pressed the mouse left button.
Restore original limits for surf. area calc.
To restore the values of the original limits of the area used for the B.E.T. or Dubinin calculations.
Dollim./Heal method for pore dist.
To plot the graph of the cumulative area and pore distribution using the Dollimore/Heal method for the calculations.
B.J.H method for pore dist. calc.
To plot the graph of the cumulative area and pore distribution using the B.J.H method for the calculations. Choose in the submenu the C coefficient to be used.
Horv.Kaw. method for pore dist. calc.
To plot the graph of the cumulative area and pore distribution using the Horvath/Kawazoe method for the calculations.
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View Graphs Menu
Option
Icon
Description
Smoothing Pore
It is enabled when the Pore Distribution curve is displayed. Allows to smooth noisy DV/DR curve
New Value Pore
It is enabled when the Adsorption/Desorption curve is displayed.. Allows to select the pore specific volume at P/P0 on the curve. Refer also to Pore specific volume at P/P0.
Scale Menu To plot the scale of the graph of the cumulative area and pore distribution as: Option
Icon
Description
Logarithmic
Logarithmic scale
Linear
Linear scale
Results Menu Choose between the following options: Option Edit Pore distribution range
Icon
Description Enter in the boxes of the table displayed the values of the pore ranges for which Pore Distribution Results are required. The measuring unit used is Angstrom. For details see The Pore Size Distribution Range Table on page 38
View Pore size results
See Pore Distribution Results on page 24
View Results
See View Results on page 22
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View Graphs Menu
The Pore Size Distribution Range Table
The Pore size distribution range table will be saved with all the other parameters of the analysis by using the function Save. If the table has to be used as matrix for future analyses, select one of the 20 reports in Report Options Page Sections. Edit the table and then press the button MEMORIZE. NOTE
By using MEMORIZE, also the settings of the report as they are in Report Options are saved. When Pore size distribution range Table is opened, the values found in the cells are those of the file of the analysis if Report from.. in Report Selection is set to None. Whereas the values are those of the selected report model (1-20), if Report from... is set other than None. Pore size distribution range Table includes the following active buttons: Button
38
Description
CLEAR TABLE
To clear the table and edit a new one.
SORT
To arrange the values in the cells.
CANCEL
After new entries or changes in the cells have been made press this button to exit Pore size distribution range without saving the changes.
UPDATE
To accept in memory the new settings and then exit the Pore size distribution range table.
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View Graphs Menu
Button AUTOFILL
Description Press this button to fill automatically the table. The software divides the pore distribution (press CLEAR TABLE first) or portion of curve of pore size distribution into histograms of the same extent. The number of subdivisor is defined by the value entered in the box Numbers of intervals on the left of this button.
Regions Menu Choose between the following options: Option
Icon
Description
Store graph regions
To memorize the values of the initial and full scale of the X and Y axes of the graph as it appears on the display. The graph can be seen later in the scale memorized with View store graph regions. These values are also used when printing the Report from the Main Menu if the option Selected regions is selected in printing graphs. Refer to Graph(s) Section on page 31.
View store graph regions
To display the graph with the values of initial scale of the X and Y axes memorized with Store graph regions.
Home graph
To restore the original size of the graph after the magnification of portions thereof.
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View Graphs Menu
Marker Menu Each point used to trace the graph curve can be highlighted with a surrounding square by using the following options: Option
Icon
Description
Pointer Marker +
The square size increases each time the corresponding button or Pointer marker + is pressed.
Pointer Marker -
The square size decreases each time the corresponding button or Pointer marker - is pressed.
Grid(+)
To draw (+) / Not to draw (-) a more or less thick grid inside the graph.
NOTE
In the printout the square may be smaller than the size displayed on the screen.
Print Menu Choose between the following options: Option
Icon
Print graph drawn on the screen
NOTE
The software uses the logo Thermo Fisher Scientific as heading derived from the Thermo logo.bmp file, which is in the directory of installation of the Sorptomatic 1990 software, or the logo selected in Title Section on page 27 of Report Menu. The type of instrument, the sample name, the file name (path and name of the file of the analysis) are also printed.
When more overlaid curves (Overlay) are on the screen, the software prints the file name, the type of result and, below the graph, the value of the result required for each overlaid curve.
Print the graph + report
40
Description
To print the graph as it appears on the screen with the report set in Report Menu.
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View Graphs Menu
Option NOTE
Icon
When more overlaid curves (Overlay) are on the screen, the software prints the file name, the type of result and the value of the result required for each overlaid curve, all the remaining report refers to the data of the main analysis in memory.
Print font dialog
NOTE
Description
To choose the type of ‘Font’ to be used for printing.
The Font used for the graph name, the values, the name and the units of the scale is defined by the software (Courier New).
Overlay Menu It consist of the following submenus.
Load Overlay It allows to choose the analyses, the colors to be used for the overlaid curves and the result that is required for each analysis.
Figure 2-11. Load Overlay Window
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View Graphs Menu
The menu displayed, shown in is subdivided into two sections : Option Overlay file
Description Press ADD to choose the file name of the analysis to be overlaid in the graph. Select a row in the list, then press COLOR to choose the color to be used for the graph of the analysis that has been selected in the list. Select a row in the list and press the button DELETE to eliminate an analysis to be overlaid.
Results to print
Select one of the results in the list; the value of the result for each overlaid analysis will be displayed in a box below the graph and it will be printed when selecting Print graph drawn on the screen or Print the graph + report . Refer to Print Menu on page 40. Press OK to go back to the View Graphs page and make the settings active. Press CANCEL to go back to the View Graph page aborting all settings.
View Overlay To enable/disable the superimposition of the curves. When View Overlay is enabled for the first time, the menu Load Overlay automatically appears to set the curves to be superposed.
Autoscaling To calculate the graph scale in a way to display all points of all curves.
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Edit Data Points Menu
Edit Data Points Menu This menu displays the values and the graphs of the raw points acquired by the instrument, and allows to modify the data of Pressure for each point.
Edit Row Data Point Selecting this submenu the page of Figure 2-12 is displayed.
Figure 2-12. Edit Data Points Page
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To completely change a datum Select a box and press once the mouse left button. The datum in the box is highlighted and will be replaced by a new entry.
•
To partially modify a datum, Select a box and press twice the mouse left button. The cursor appears in the box thus allowing to change the value.
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Edit Data Points Menu
•
When changing a value Press the button REDRAW to update the graph.
•
If you want to restore the data as at the opening of the Edit Data Points submenu Press the button RESTORE. When a box is selected, the corresponding point in the graph is highlighted by a rectangle.
•
The commands Delete and Insert Can act on more points simultaneously. To do this, select more boxes using Shift+arrow key (up or down).
In Edit row data points page, the following active button are present: Button
44
Description
ADSORPTION
To display the data of Volume/Pressure of the points acquired during ‘Adsorption’ phase.
DESORPTION
To display the data of Volume/Pressure of the points acquired during ‘Desorption’ phase.
DELETE
It eliminates the values Volume/Pressure in the selected box. To eliminate more data at a time, use the Shift+arrow keys (up or down) and select more boxes.
INSERT
To insert an empty row for adding a value of Volume/ Pressure. To insert more than one row, select a number of boxes corresponding to the desired number to be added.
RESTORE
To restore data as at the opening of the Edit Data Points submenu. When the command CUT BELOW is used, the decrease data are cancelled; to restore them, repeat the comand ‘Restore’ after pressing the DESORPTION button.
EXIT
To exit Edit Data Points. If points have been changed, the software will ask whether changes have to be saved. To save the changes on disk, use function Save in the File menu of the Main Menu.
REDRAW
This command allows to redraw the graph, when a Volume/ Pressure value has been changed.
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Instruments Serial Ports Menu
Button ZOOM
Description o magnify a section of a graph; the point preceding the selected one is used as starting point for the scale, the following one is used to define the full scale. To restore the complete graph, press the button REDRAW.
Instruments Serial Ports Menu This menu allows to set the instruments serial ports. The Sorptomatic 1990 software can accept analyses from 4 instruments and can keep in memory 4 different analyses at the same time. This menu allows to inform the software of which port the instrument is connected to. For each instrument a submenu is opened.
Instrument Serial Port Submenu Select in the sub-menu of each instrument (1-4), the required serial port Com 1-4. Option
Description
Com 1-4
Serial port at which the instrument is connected. The ACQUIRE POINTS button will be enabled.
None
Select it when the instrument is not connected. The ACQUIRE POINTS button will be disabled.
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Acquire Points
Acquire Points This command allows to acquire points from the instrument. This function is enabled only when the software has been informed of the serial port in use (see Edit Data Points Menu on page 43). Before starting the acquisition, the software asks where the data have to be saved on disk through the window Directory / File Name. In choosing the path and the file name, select: 1. New, when the file does not exist on disk. The software uses all the parameters of the analysis in memory + the acquired points and saves them on disk in the file. 2. Existing, when the file already exists on disk. The software loads from the existing file the analysis parameters, cancels the points existing on file, adds the points acquired and saves on disk. 3. The same, when the file is the same as the analysis in memory. The software uses all parameters of the analysis in memory, cancels the existing points, adds the points acquired and then saves on disk. Once the file for saving the data is chosen, the page summarizing the parameters of the analysis is displayed, and the acquired points are added. Check that the parameters are the desired ones and press CONTINUE to go on with the acquisition. To abort the operation, press ESCAPE; the parameters can be modified later. NOTE
46
If during the acquisition the message Communication error ... is displayed, repeat the acquisition. If during the data acquisition, the D.S.D Panel is open and positioned on the same instrument, the communication between the D.S.D Panel and the computer is cut out until the end of the acquisition. If the message Communication error ... is still present, repeat the acquisition after closing the D.S.D Panel.
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Sorptomatic Control
Sorptomatic Control This command allows to access Digital Status Display (D.S.D.). For details refer to Digital Status Display.
Remark To add a comment to the analysis. To enter a text, press the mouse left button with the cursor inside the textbox, write the desired text and then press ENTER or the mouse left button again. The entered comment will be saved with the parameters of the analysis and it will be retrieved any time the analysis is loaded.
Help Menu This function permits to access the help system of Sorptomatic 1990 software. The Help is divided in many modules and each has been designed to cover specific arguments of the modules currently in use.
Main Menu Sections Main Menu has six sections and an specific dialog window for the Sorptomatic 1990 control named Digital Status Display. The following table lists the available sections. You may find the instructions to operate in Chapter 3.
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Sample Information
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Acquisition Parameters
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Analytical Conditions
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Instrument Parameters
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Calculation Parameters
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Report Selection
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Main Menu Sections
•
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Digital Status Display
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3 Main Menu Sections This chapter contains the description of the active items and commands of the Main Menu Sections and Digital Status Display (DSD).
Chapter at a Glance… Introduction .......................................................................................................... 50 Sample Information .............................................................................................. 51 Acquisition Parameters......................................................................................... 53 Calculation Parameters......................................................................................... 63 Report Selection ................................................................................................... 67 Report Selection ................................................................................................... 67 Digital Status Display........................................................................................... 70
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Chapter 3 Main Menu Sections
Introduction
Introduction The following table lists the available sections and the relevant paragraph where you may find the instructions to operate. Main Menu Sections and DSD
50
Refer To:
Sample Information
Sample Information on page 51.
Acquisition Parameters
Acquisition Parameters on page 53.
Analytical Conditions
Analytical Conditions on page 57.
Instrument Parameters
Instrument Parameters on page 61.
Calculation Parameters
Calculation Parameters on page 63.
Report Selection
Report Selection on page 67.
Digital Status Display (DSD)
Digital Status Display on page 70.
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Chapter 3 Main Menu Sections
Sample Information
Sample Information Pressing SAMPLE INFORMATION the following dialog window is displayed where you set the required sample information parameters.
Figure 3-1. Sample Information Dialog Window.
General Information Group Boxes Information Company Name Operator
Description Enter in the boxes the texts referring to the analysis. These data are not used for the calculations.
Data Sample name Preparation
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Sample Information
Preparation Button The button next to Preparation allows to load a file containing a temperature program (file name.Rat) previously saved (with D.S.D panel) and corresponding to the sample treatment before the analysis. The loaded data will be entered in the box Preparation. The format of the entered text is as follows: XXX-YYY (°C) RR (°C/min) TT (hours) where : XXX = Initial temperature YYY = Final temperature RR = Increment TT = Time during which the sample is kept at the final temperature.
Sample Mass (g) Enter in this test box the weight of the sample expressed in grams. Sample mass is a very important value, because it is used for many calculations (see View Results on page 22) and to draw graphs. Set Sample mass = 0 when a blank analysis is run.
Sample Density Enter in this test box the real density of the sample in g/cm³. If the value is unknown, enter 1. This parameter is used together with Sample Mass in the calculation of Slope/Intercept for the blank correction.
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Acquisition Parameters
Acquisition Parameters Pressing ACQUISITION PARAMETERS the following dialog window is displayed where you set the required acquisition parameters.
Figure 3-2. Acquisition Parameters Dialog Window The parameters in this section simply summarize the analytical conditions set for the analysis. They are not used for the calculations. These data are automatically loaded via RS232 when acquiring points from a Sorptomatic 1990 (see Instruments Serial Ports Menu on page 45).
Adsorption Group Boxes The following parameters refer to the adsorption stage. This stage can be subdivided into three sections with different acquisition parameters.
Desired points Enter in the boxes the number of points to be acquired for each region. The program in the instrument, while analyzing, calculates the loading pressure and the piston volume as a function of the number of points acquired for each region and of the sample adsorption rate (A.G.I.S.).
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Acquisition Parameters
It is possible to select a fixed volume dosing for all the three pressure ranges selected by the user. To select the fixed dose routine click on the side arrow and select FixVol on the line identified by Desired points. NOTE
The sum of the points of the three regions must not exceed 500.
Equilibrium deviation Maximum variation limit of pressure recorded during a time interval (Equilibrium Time). If the equilibrium pressure variation is below the value set in the box, the system goes on with the following injection; otherwise it waits for a further time interval. Enter a value for each of the three regions.
Equilibrium Time Time interval (in minutes) where pressure must not exceed the value of Equilibrium deviation to allow the subsequent injection. Enter a value for each of the three regions.
P/P0 regions Set a value between 0 and 1. •
If 0 is set, the region is cancelled and the value of the following one is considered.
•
If 1 is set, the subsequent regions are cancelled.
Piston filling volume When Desired points selected is FixVol, to select the piston volume in use to inject the gas dose, select full (1/1), half (1/2) or quarter stroke (1/4). If the fixed volume is selected, in the relevant pressure range the instrument will inject the measuring gas using the selected volume and the loading pressure indicated in the box Initial load pressure.
Max Ads pressure Enter in this box the maximum value of pressure to be reached at the end of the adsorption cycle.
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In any case the instrument ends the adsorption cycle when the Max Ads pressure is reached, even if it is lower than the real saturation pressure. This parameter can be useful when a quick adsorption cycle is required. Once the value set in this box is reached, the system immediately switches to the desorption cycle if Ads + Des is set, or it stops the measurement if only Ads is set. See Analysis type Box.
Min Saturation pressure Enter in this box the value of the minimum pressure at which the instrument starts to consider a possible saturation for the actual Physisorption cycle. The value is set to 10-20 Torr (with nitrogen) below the actual atmospheric pressure of that day. This parameter avoids that the Sorptomatic 1990 finds the saturation pressure at a lower P/P0; this often occurs when the sample is a mesoporous material causing a phenomenon of capillary condensation.
Initial load pressure Enter in the box the loading pressure of the first gas injection only; the pressure required for the acquisition of the other points is calculated by the instrument (A.G.I.S.). The recommended value is 200 for non porous materials, 300 for mesoporous materials, 400 for microporous solids.
Prep-run time (min) When starting an experiment, the instrument will wait the selected delay time keeping the sample holder under vacuum conditions before starting the experiment.
Desorption Group Boxes The following parameters refer to the desorption stage. The cycle starts from the saturation up to the value set in Last Des pressure (15< 500). This stage can be subdivided into two sections with different acquisition parameters.
Desired points (Des) Enter in this box the number of points to be acquired during the desorption cycle.
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Acquisition Parameters
Equilibrium deviation Maximum variation limit of pressure recorded during a time interval (Equilibrium Time). If the equilibrium pressure variation is below the value set in the box, the system goes on with gas removal, otherwise it waits for a further time interval.
Equilibrium Time (min) Time interval (in minutes) during which the pressure must not exceed the value set in Equilibrium deviation to go to the following gas removal operation.
P/PO regions Set a value between 0.1 and 0.99. •
Set both regions otherwise the Last Des value will be not considered.
Piston filling volume When Desired points (Des) selected is FixVol, to select the piston volume in use to remove the gas dose, select full (1/1), half (1/2) or quarter stroke (1/4).
Last Des pressure Enter in the box the last value of pressure to be reached in the desorption cycle. This value represents the completion of the analytical cycle.
Analysis type Box Select Ads to perform only the adsorption cycle, select Ads+Des if the desorption cycle is also required.
Saturation pressure Box Select PT100 (or 0) to assign to each point the saturation pressure found on the basis of the temperature detected in the vicinity of the sample. Enter a value higher than 0 to assign the same value to all points. This is useful for chemisorption analyses, because due to the analytical conditions the gas will never reach the saturation pressure. This will allow the software to correctly calculate the graphs scale. Acquisition Parameters page includes the following active buttons
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Analytical Conditions
Button
Description LOAD ACQUISITION PARAMETERS To load the values of Acquisition parameters from a dedicated file previously saved on disk (extension .Cus). The loaded data will be entered in the corresponding boxes. SAVE ACQUISITION PARAMETERS To save the acquisition parameters in a dedicated file (extension .Cus).
Analytical Conditions Pressing ANALYTICAL CONDITIONS the following dialog window is displayed where you set the required parameters.
Figure 3-3. Analytical Conditions Dialog Window This page includes the following active buttons:
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Chapter 3 Main Menu Sections
Analytical Conditions
Button
Description FILL WITH GAS DATA Use this button to choose the gas to be used in the list of the menu displayed. Refer to Fill with gas data. CALCULATION Use this button to calculate Blank Slop, Blank intercept and Instrument isteresis. LOAD Use this button to choose a memorized blank analysis.
Fill with gas data Choose the gas to be used in the list of the menu displayed.
Figure 3-4. Gas Used Data Page All the parameters will also be shown. By pressing the UPDATE button, the values will be reported in the appropriate boxes.
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Analytical Conditions
Left Section and Gas used data Group Boxes The left section of Analytical Conditions page and the Gas used data page contains the following boxes:
Gas molecular weight Enter the molecular weight of the gas used for the measurement (g/mol); see references or use the option Fill with gas data.
Gas molecular area Enter the molecular area of the gas (A²) deposited on the sample porous walls. It is a feature of the gas used for the measurement; see references or use the option Fill with gas data.
Liquid gas density Enter the density of the gas used for the measurement (g/cm³). See references or use the option Fill with gas data.
Liquid gas surface tension Enter the value of the specific surface tension (Dyne/cm) of the liquid gas used for the measurement. See references or use the option Fill with gas data.
Monolayer thick. Thickness of the gas monolayer deposited on the sample porous walls (Å). It is a feature of the gas used for the measurement. See references or use the option Fill with gas data.
2nd virial coefficent burette temperature This value is used in the calculations to optimize the real state of the gas used as adsorbent.
2nd virial piston temperature This value is used in the calculations to optimize the real state of the gas used as adsorbent.
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Analytical Conditions
Righ Section Group Boxes The right section of Analytical Conditions page contains the following boxes:
Blank slope Correction value of the sample isotherm calculated from the equation of a blank analysis. If the analysis in memory is actually a blank analysis, press CALCULATION button to do the calculation of Blank slope, Blank intercept and Instrument hysteresi, otherwise press LOAD button to choose a blank analysis. The values of Blank slope, Blank intercept and Instrument hysteresis will be taken from this analysis and reported in the appropriate boxes.
Blank intercept Correction value of the sample isotherm calculated from the equation of a blank analysis. If the analysis in memory is actually a blank analysis, press CALCULATION button to do the calculation of Blank slope, Blank intercept and Instrument hysteresis, otherwise press LOAD button to choose a blank analysis. The values of Blank slope, Blank intercept and Instrument hysteresis will be taken from this analysis and reported in the appropriate boxes.
Instrument hysteresis This parameter is used to correct the slight difference in volume that occurs when switching from the adsorption cycle to the desorption cycle. This value is found with a blank analysis in both cycles. If the analysis in memory is actually a blank analysis, press CALCULATION button to do the calculation of Blank slope, Blank intercept and Instrument hysteresis, otherwise press LOAD button to choose a blank analysis. The values of Blank slope, Blank intercept and Instrument hysteresis will be taken from this analysis and reported in the appropriate boxes.
Bottom Section Group Boxes The bottom section of Analytical Conditions page contains the following boxes:
Burette temperature (°C) Enter the temperature of the burette containing the sample during the analytical cycle. If the refrigerating fluid of the burette is liquid nitrogen, enter in the box the nitrogen temperature.
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Instrument Parameters
Correct slope/Intercept To set the correction of Slope/Intercept when the blank has been run with an empty burette. This allows to take into consideration the volume occupied by the sample. To perform this correction, the real sample density must be known (see Sample Information). The blank could be run with a burette with sample using helium instead of nitrogen, because helium is not absorbed by the sample except microporous active carbons, in this case the correction must not be performed.
Instrument Parameters Pressing INSTRUMENT PARAMETERS the following dialog window is displayed where you set the required parameters.
Figure 3-5. Instrument Parameters Dialog Window
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Instrument Parameters
Stroke Volume Group Boxes Total stroke Volume Enter in the box the total volume of the piston (in cm³) used in the Sorptomatic 1990. The value is reported on a label applied on the piston.
½ stroke Volume Enter in the box the volume at half stroke (in cm³) of the piston used in the Sorptomatic 1990. The value is reported on a label applied on the piston.
¼ stroke Volume Enter in the box the volume at a quarter of stroke (in cm³) of the piston used in the Sorptomatic 1990. The value is reported on a label applied on the piston.
Piston Group Boxes Piston dead Volume Enter in the box the dead volume at the head of the piston (in cm³) used in the Sorptomatic 1990. The value is reported on a label applied on the piston.
Piston temperature Enter in the box the temperature of the piston (in °C). This temperature is normally 34 °C, but it can be measured using a thermocouple device applied in the inner part of the piston.
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Calculation Parameters
Calculation Parameters Pressing CALCULATION PARAMETERS the following dialog window is displayed where you set the required calculation parameters.
Figure 3-6. Calculation Parameters Dialog Window This dialog window includes the following active buttons. Buttons
Description PORE DISTRIBUTION RANGE
Refer To: Pore Distribution Range on page 65
Surface Area calculation method To choose the calculation method to determine the sample surface area.
B.E.T. Calculation of the sample surface area using the B.E.T. equation. Set the region of the linear regression by entering in the Initial and Final (P/P0).
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Calculation Parameters
Dubinin Calculation of the sample surface area using the Dubinin equation. Set the region of the linear regression by entering Initial and Final log²(P0/P).
Initial and Final (P/P0) Set in these boxes the region of the linear regression when the sample surface area is calculated using the B.E.T. equation. See B.E.T..
Initial and Final log²(P0/P) Set in these boxes the region of the linear regression when the sample surface area is calculated using the Dubinin equation. See Dubinin.
Pore size calculation method To choose one of the calculation methods to determine the pore size distribution; available methods are: •
Dollim./Heal
•
Horv./ Kaw.
•
B.J.H.
Smoothing Pore distribution convolution points To smooth the pore distribution curve by performing a weighted mean for a consecutive number of points entered in this box. See also View Graphs Menu.
Pore specific volume at P/P0 Enter in this box a value of relative pressure to be used for the calculation of the pore total volume according to the Kelvin factor, evaluated for the measuring gas. The relative pressure entered must be lower than the saturation pressure and higher than the pressure at which capillary condensation takes place (Isotherm of type 4). See also View Graphs Menu.
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Calculation Parameters
Pore Distribution Range When the relevant button is pressed, the following table page is displayed.
Figure 3-7. Pore Distribution Range Table Page Enter in the table cells the values (Radius or Diameter) of the pore ranges for which results, Pore size distribution results, are required. Refer to Pore Distribution Results on page 24. The measuring unit used is Angstrom.
Buttons This Table page includes the following active buttons. Buttons
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Description
CLEAR TABLE
Press this button to clear the table in order to set a new one
SORT
Press this button to arrange the values in the cells.
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Buttons
Description
CANCEL
Press this button to exit the table when the modifications have to be aborted.
UPDATE
Press this button to exit the table when the new settings have to be stored in memory.
AUTOFILL
Press this button to fill automatically the table. The software divides the pore distribution (press CLEAR TABLE first) or portion of curve of pore size distribution into histograms of the same extent. The number of subdivisor is defined by the value entered in the box Numbers of intervals on the left of this button.
The Pore distribution rangetable will be saved with all the other parameters of the analysis using the function Save in File Menu. To use the table as a matrix for other analyses, select one of the 20 reports in Report Selection, edit the table and then press MEMORIZE. NOTE
Pressing MEMORIZE, also all the report settings selected in Report Options are saved. When the Pore distribution range table is opened, the values already found in the cells are derived from the file of the analysis if None has been set in Report From Group Box in Report selection section. Whereas the values come from the selected report model (1-20), if other than None is set.
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Report Selection
Report Selection Pressing REPORT SELECTION the following dialog window is displayed where you set the required parameters.
Figure 3-8. Report Selection Dialog Window This page includes the following active buttons. Buttons
Description
MEMORIZE
Use this button to memorize a report model. Refer to How to Use the Memorize Button on page 68.
CHANGE NAME
The twenty available reports are named by the software: Report 1, Report 2, .... By pressing this button, it is possible to enter another name in the textbox next to the button.
The following options allow to set Report Options Page Sections with the parameters previously defined in one of the twenty avilable reports.
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Report Selection
When None is selected, the parameters of Report Options are defined by the software when the page is first opened, then they keep the last setting until Sorptomatic 1990 is closed.
Report From Group Box The following options allow to set Report Options with the parameters previously defined in one of the twenty available reports. Option
Description
None
No preset report is used to define the Report Options. The Pore Distribution Range table used in the one loaded with the file of the analysis.
Report 1-20
It uses the parameters of the report in memory to set the Report Options, tick corresponding button to the report to be used. The report must have been previously defined setting the Report Options and then memorized (see MEMORIZE button).
Pore size distribution range from... When this box is ticked, the Pore Distribution Range table used to calculate the pore distribution is the one memorized with the selected report (see above Report 1-20). When the box is not ticked, the Pore size distribution range table used to calculate the pore distribution is the one saved with the parameters of the analysis.
How to Use the Memorize Button To memorize a report model Operate as follows: 1. Tick the button of one of the twenty available reports. 2. Set the Report Options, edit the Pore size distribution range table. 3. Enter in Report creation and modify all the report parameters according to your requirements.
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4. When the Report creation is complete, save the report set by pressing the button MEMORIZE. The parameters of the twenty report models are written in the Report.Ini file that can be found in the same directory as Sorptomatic 1990. NOTE
Operating Manual
By using MEMORIZE also the Pore size distribution range table is saved with the data of Report Options, even when the options Pore size distribution range from... is disabled. When a table of Pore size distribution range saved with an analysis has to be transferred into one of the twenty reports, operate as follows : 1 - choose one of the twenty report models by ticking the corresponding box 2 - untick the boxes ‘Pore size distribution range from...’ 3 - load from File menu the analysis reporting the required table 4 - press the button MEMORIZE.
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Digital Status Display
Digital Status Display Digital Status Display (D.S.D.), shown in Figure 3-9 is a window used as control panel of the Sorptomatic 1990, and it is activated from the Main Menu.
Figure 3-9. The Digital Status Display Dialog Window
Introduction From the Main Menu first select one of the 4 instruments (Instrument 1 2 3 4), previously connected to a serial port RS232 and configured in the menu ‘Instruments serial port’, then press the Pascal control icon. The D.S.D. panel is displayed, the software checks the presence of the instrument and displays the instrument status. It is possible to open four D.S.D panels, one for each of the 4 instruments in the Main Menu, provided that each instrument is connected to a different serial port
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COM (1-4). If the D.S.D panel of an already open instrument is requested, an error message is displayed: •
Error opening Com x, with the prompt message Abort and Retry. Select Abort and close the D.S.D panel erroneously opened.
It is also possible to open only one D.S.D. panel and switch from one instrument to the other by using the buttons 1 2 3 4. The box on the top of the window below the main menu shows the condition of the RS232 communication. The message may be one of the following : •
Communication Ok The instrument is connected and acknowledged.
•
Communication Error The instrument is not connected or not acknowledged (check the connection).
•
Serial Port not assigned The selection of ‘Instruments serial port’ in the Main Menu is not correct.
When the D.S.D panel is correctly connected to the instrument, it receives the following indications approximately every 0.5 seconds: — Pressure — Status — Number of points acquired — Solenoid status — Ovens conditions To actuate the solenoid valves, move the cursor on the button showing the concerned valve and press the mouse left key. When the instrument is running the acquisition, the solenoid valves are actuated only from the instrument.
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The solenoid valve V6 is automatically actuated when pressure exceeds 950 Torr. This is useful to protect the pressure transducer.
•
The solenoid valves V7 and V8 move the piston. The filling volume of the piston is defined by radio buttons 1/4, ½, 1/1 (a quarter, half, total volume of the piston).
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The button COOL activates the automatic system to keep the level of liquid nitrogen constant during the analytical cycle. WARNING! Never open the solenoid valve V4 without a measuring burette installed, or alternatively a plug. The vacuum pump, operating at atmospheric pressure, might be severely damaged. NOTE
The D.S.D panel is not closed when exiting the main menu of Sorptomatic 1990, but it must be closed separately. When running ‘Acquire Points’ from the Main Menu, the communication with the instrument is temporarily cut out. In Digital Status Display dialog window the following menus and command are available:
File Menu This menu allows to access the following functions.
Function Open
1-2-3-4
Description This function allows to load a memorized analysis. Through the menu Acquisition parameters, it is possible to see and send to the instrument the same analytical conditions as those used for the analysis in memory. When more than one instrument is available, it is convenient to assign a different number to each one and use the same number both for the data processing and acquisition in the Main Menu and for the software for the instrument control (D.S.D panel). The Sorptomatic 1990 software may simultaneously control 4 different instruments. To switch from one instrument to the other, place the cursor on the desired number in the top buttons and press the mouse left button. Alternatively, in the File submenu, select one of the rows numbered 1-4 and press the mouse left button. The software will close the communication with the current instrument and it will open the communication with the selected instrument (see also Instrument Serial Port on page 73).
Exit
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To exit the window of the D.S.D panel.
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Instrument Serial Port The software can acquire analyses from 4 instruments and keep in memory 4 different analyses at the same time. Instruments serial port allows to inform the software of the serial port to which the instrument is connected. In the submenu of each instrument (1-4), select the desired port Com 1- 4; the Edit Data Points Menu can also be found in the Main Menu.
Run Menu This menu includes the following commands
Start To send the command and start the analysis. First check the acquisition parameters set in the instrument (see Acquisition Parameters Menu, make sure that the vacuum is stable and nitrogen at the appropriate level.
Stop To interrupt the current analysis.
Reset To set to zero the instrument status when an analysis is over, thus allowing another analysis to be run. A message from the software prompts whether the data in memory in the instrument have to be saved on disk. For this purpose go to the Sorptomatic 1990 Main Menu and press the ACQUIRE POINTS button. See Instruments Serial Ports Menu.
Calibration Menu This menu includes the following options
Transducer Calibration using pressure of today To start the intrument internal procedure for the calibration of the transducer. If the actual atmospheric pressure is not exactly known, perform calibration with the following option, because this procedure requires the entry of this pressure.
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Transducer Calibration using CPU 1990 ID Number To start the instrument internal procedure for the calibration of the transducers. At the beginning of the procedure the software requires the ID number reported on the label of the CPU installed in the instrument.
This number is different for each instrument, and it is assigned during the instrument final test.
Calibration P0 Saturation To start the procedure of calibration of the saturation pressure P0 based on the liquid nitrogen temperature measured near the sample (Pt100). Exactly follow the instructions the instrument prompts while performing calibration.
Display the data during transducer calib. To display in real time the pressure values during calibration.
Load from disk a modification inside prg. to SO1990 The instrument internal program can be modified and this option allows to load from disk the lines of instructions to be sent to the instrument. Changes will be “remembered” by the instrument until it is shut off. When the instrument is switched on again, the transfer of changes must be repeated.
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Acquisition Parameters Menu Select default parameters: •
Mesoporous
•
Microporous
•
Non porous
•
File in memory (parameters in memory
In a page, such as the one shown in Figure 3-10, the analytical conditions of the instrument to perform the analysis can be set or displayed.
Figure 3-10. Example of Mesoporous Page The parameters shown in the boxes are derived from the file chosen in the sub-menu of Acquisition Parameters. The name of the file in memory is reported below the buttons bar, while the name of the file chosen is reported inside the parameters box.
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If the button READ is pressed, the data are read from the instrument and they will replace those present in the boxes
•
If the button SEND is pressed, the data reported in the boxes are sent to the instrument. Button
Description
LOAD FROM DISK
To load the valuesof Acquisition parameters from a dedicated file (extension .Cus) previously saved on disk. The loaded data will appear in the corresponding boxes.
SAVE TO DISK
To save the acquisition parameters displayed in the file of the analysis in memory. The parameters can also be saved in a dedicated file (extension .Cus).
READ
To request via RS232 the analytical conditions set in the instrument and to display the values in the relevant boxes.
SEND
To send to the instrument the data of the analytical conditions displayed in the boxes.
EXIT
To exit the section Acquisition parameters page and to go back to the page as control panel of the instrument.
Other Menu It allows to access the following functions
Leak test To check the pneumatic system for vacuum leaks. With vacuum in the system and the solenoid valves in the appropriate position, the software checks that no increase in pressure higher than the set value occurs in one minute. This value is required at the beginning of the test, and it is either defined by the sofware, as a function of the transducer installed in the instrument, or manually entered by the user.
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The test can go on for more than one minute. In this case, every 5 minutes, the software will keep the user informed whether the leak is increasing (+), decreasing (-) or constant (=). The messages and the development of the leak test are shown in the upper right box of the page. To stop the test, press the button EXIT.
Change gas The Sorptomatic can use two different gases. Exactly follow the instructions prompted by the software to switch from one gas to the other.
Menu Menu This menu allows to access the following functions: Function
Description
Normal
To restore the size of the D.S.D. panel window, after it has been reduced with Short.
Short
The D.S.D. panel window is reduced, the boxes Status, Ads, Des, P.Load, P.Equi, P0 Sat., are reported in the buttons bar. This option allows to position the D.S.D panel in a way to use the Main Menu and simultaneously see the status of the instrument connected.
Command Buttons The Digital Status Display dialog window include the following command buttons.
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EDIT FURNACE 1 / EDIT FURNACE 2 To display a menu to set the temperature or a temperature program for the ovens 1 or 2 (Furnaces).
Set Status Option
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Description
On
The oven is switched on and it will reach the set temperature.
Off
The oven is switched off.
On+Stop Heat
The oven is switched on and it will reach the set temperature. If the gases freed from the sample exceed a preset pressure value (see Section 2, paragraph 2.3.1 of the Sorptomatic 1990 Instruction Manual), the oven is switched off. When pressure goes below that value, the oven is switched on again, and so on.
On+Rate temperature
To activate the temperature program defined in the Rate program section of this window.
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Set Temperature (° C) Move the pointer by dragging it on the temperature bar until the desired temperature value is reached. To run a temperature program, the temperature to be set must be the same as the initial temperature and, before starting the temperature program, the oven must be in the Ready status.
Rate program Parameters
Description
Initial Temperature (°C)
Initial temperature of the temperature program. The box shows the current oven temperature that should have been already set, and the oven must be in Ready status for the program to start.
Temperature rate (°C/min)
Increments of temperature in degrees centigrade per minute used to reach the final temperature. Select one of the values displayed in the pulldown menu.
Final temperature (×C)
Final temperature to be reached. This temperature will be kept for the time set in the following option. Enter in the box the desired value, or use Up/Down keys.
Time before Off (hours)
Time in hours for which the final temperature has to be kept before switching off the oven. Enter in the box the desired value, or use Up/Down keys: a value of -1 indicates infinity (that is manual shut off).
Button
Description
LOAD RATE PROGRAM
The temperature values, Initial/Final/Rate, and the Time can be loaded.
SAVE RATE PROGRAM
The temperature values, Initial/Final/Rate, and the Time can be saved in a file with .Rat extension.
Rate program includes the following active buttons
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Button
80
Description
SEND TO INSTRUMENT
By using this button the oven status and the temperature program can be changed or set and the data sent to the instrument via RS232.
EXIT
To exit this menu. If the instrument settings have to be changed, first press SEND TO INSTRUMENT.
Operating Manual
4 Running Analyses This chapter contains the operating sequence to running the blank and sample analysis by using the software for Sorptiomatic 1990.
Operating Sequences Running the Blank and Sample Analysis ............................................................. 82
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OPERATING SEQUENCE Running the Blank and Sample Analysis After the installation of instruments and software, operate as follows: 1. Connect the cable RS232 coming from SO 1990 to COM1 of the computer. 2. From the computer press Start-Programs and the icon SO1990: the program will automatically start. 3. Press Inst.Ser.Port, select instrument1 and assign COM1 to this instrument. 4. For a better management of the analytical files, it is advisable to create new folders, one to save the files of the blanks referring to the burette in use and one for the analyses of samples. 5. Now a blank analysis must be performed. From the Main Menu follow this sequence: •
File >> Open >> Yes,
•
Select the hard disk (C:)
Then select the path: •
Thermo >> Sorptomatic >> Data.
•
Now load the file BlankN2.
6. From the Main Menu press File and then New. Tick all the small boxes of sections and points to delete all parameters in memory and press OK. A window for saving the new file appears. Select the folder where the blank files have to be saved and enter a new file name, then press Save. 7. Select the page Sample information and enter the data of Company name, Operator and Sample name. Leave 0 set in the other boxes.
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8. Select the page Analytical conditions and enter the value 0 in the boxes: Blank Slope and Blank Intercept. Enter 1 in Instrument Hysteresis. 9. Select the page Instruments Parameters and enter the values of volume of piston and dead volume regarding the instrument, reported on the label placed on the piston inside the instrument. 10. From the Main Menu press File >> Save and the page of the previously set file will be automatically displayed. Press Save to memorize the changes done 11. Now select the button Sorptomatic Control to enter the Digital Status Display (D.S.D. Panel). It displays in real time the status of the instrument and allows to communicate with the machine itself. If no message of correct communication is displayed, check that the setting Instrument N.1 is selected. 12. In the D.S.D. panel select File >> Open and load the previously developed blank file. 13. Select Acquisition Parameters, then File in Memory, and the page to set the data to be sent to the Sorptomatic is displayed. Press Send to Instrument and, at the end of the operation, press Exit. 14. Perform the blank analysis just as it is carried out in the program for DOS (refer to the instrument Instruction Manual). 15. At the end of the analysis, the data collected must be transferred from the instrument to the computer in the desired file. Go back to the Main Menu, press the button ACQUIRE POINTS, select the previously prepared blank file and press Save and then Yes. The page containing the parameters of the analysis set will be displayed. If it is correct, press Continue to save. All the data will be transferred and saved on file. 16. Select the page Analytical conditions and press Blank Slope Blank Int. Instrument calculations: the correct values will be automatically displayed. Press Yes if you want to enter them in the page Analytical conditions. 17. Follow the path File >> Save >> Yes to save the new parameters in the file.
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18. Now the analytical procedure must be started. For the sample preparation refer to section 5 of the SO 1990 instruction manual. 19. If an analysis has to be run, proceed as follows: •
from the Main Menu select File >> Open >> Yes
•
select the hard disk (C:)
then the path •
Thermo >> Sorptomatic >> Data.
•
Now according to the type of sample to be analyzed, load the file Highpor, Lowpor or Mesopor.
20. From the Main Menu press File and then New. Tick the boxes of sections and points to delete all parameters in memory, then press OK. A window appears where the options for saving the new file are displayed. Select the folder where the analytical files have to be saved and then enter a new file name. Click Save. 21. Select the page Sample Information and enter Company name, Operator, Sample name, Date, Preparation, Sample mass and Sample density. 22. Select the page Analytical Conditions and by the button LOAD select the blank file referring to the burette in use. The values of Blank Slope, Blank Intercept, Instrument Hysteresis and burette in use will be automatically loaded. 23. Select the page Instrument Parameters and enter the values of Piston volume and Dead volume reported on the label placed on the piston inside the instrument. 24. From the Main Menu press File and Save to go automatically back to the previously set file. Press Save to memorize the changes done. 25. Now select the button Sorptomatic Control to enter the Digital Status Display (D.S.D. Panel) that displays in real time the status of the instrument and allows to communicate with the machine itself.
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If no message of correct communication is displayed, check that the setting Instrument N.1 is selected. 26. In the D.S.D. panel select File >> Open and load the previously developed blank file. 27. Select Acquisition Parameters, then File in Memory, and the page to set the data to be sent to the Sorptomatic is displayed. Press Send to Instrument and, at the end of the operation, press Exit. 28. Perform the analysis just as it is carried out in the program for DOS. 29. At the end of the analysis, the data collected must be transferred from the instrument to the computer in the desired file. Go back to the Main Menu, press the button ACQUIRE POINTS. Select the previously prepared analytical file and press Save and then Yes. The page containing the parameters of the analysis set will be displayed. If it is correct, press Continue to save. All the data of the analysis will be transferred and saved on file. 30. To print reports and graphs, refer to the preceding manual, Software Sorptomatic 1990 for Windows.
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