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Micromeritics Gemini VII 2390a Operator'S Manual Download Page 9

Gemini VII

Table of Contents 

239-42828-01 - Nov 2013                                   

v 

BET Surface Area Report  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-26
BET Surface Area Plot. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-27
t-Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-28
BJH Adsorption Cumulative Pore Volume . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-29
BJH Adsorption dV/dlog(w) Pore Volume . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  7-30

8.

OPTIONS MENU

Introduction  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  8-1
Option Presentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  8-1
Sample Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  8-2

Restricted Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  8-2

Units . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  8-3
Graph Grid Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  8-3
Service Test Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  8-4

9.

TROUBLESHOOTING AND MAINTENANCE

Introduction  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-1
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-1
Preventive Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-4

Recovering from a Power Failure  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-4
Lubricating Elevator Drive Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-5
Cleaning the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-5
Cleaning the Analysis Dewar. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-5
Replacing Port Filter (Frit) and O-ring  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-6
Replacing the Sample Tube O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-7
Inspecting and Changing Vacuum Pump Oil. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-8

Inspecting the Oil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-8
Changing or Adding Oil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-8

Replacing the Alumina in the Oil Vapor Trap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-11
Changing the Vacuum Pump Exhaust Filter  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-15
Performing a Leak Test  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-16

Connecting Gases. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-18

Guidelines for Connecting Gases to the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-18
Disconnecting the Depleted Bottle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-18
Connecting a Replacement Gas Bottle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-19
Cleaning and Verifying the Gas Line. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-22

Performing a Blank Analysis for Diagnostic Purposes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-26
Performing a Reference Analysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-28

Analyzing Reference Material . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-29

Calibrating the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-30

Zero Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-30
Match Transducers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-31
Sample Servo . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-31
Balance Servo. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  9-32

Summary of Contents for Gemini VII 2390a

Page 1: ...Gemini VII Operator s Manual V3 02 239 42828 01 Jan 2014...

Page 2: ...soft Windows and Windows 7 and Windows Vista are registered trademarks of Microsoft Corporation Gemini is a registered trademark of Micromeritics Instrument Corporation Micromeritics Instrument Corpor...

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

Page 4: ......

Page 5: ...INTERFACE Introduction 2 1 Instrument Components and Connectors 2 1 Front Panel 2 2 Sample Compartment 2 3 Rear Panel 2 4 Turning the Analyzer On and Off 2 5 Turning the Analyzer On 2 5 Turning the An...

Page 6: ...lysis 3 24 Start Analysis 3 25 QuickStart Analysis 3 26 Blank Analysis 3 27 Generating Reports 3 28 Printing Files 3 30 Listing Files 3 31 Exporting Isotherm Data 3 32 Format of Exported Data 3 33 Con...

Page 7: ...t Options 5 24 Freundlich Report Options 5 27 Temkin Isotherm Report Options 5 28 t Plot Report Options 5 30 Alpha S Method 5 33 f Ratio Method 5 34 BJH Adsorption Desorption Report Options 5 36 Tabul...

Page 8: ...re 6 20 Match Transducers 6 20 Reset Pressure Calibration 6 21 Sample Servo 6 21 Balance Servo 6 21 Save to File 6 22 Load from File 6 23 Service Test 6 23 7 REPORTS MENU Introduction 7 1 Common Field...

Page 9: ...Cleaning the Analysis Dewar 9 5 Replacing Port Filter Frit and O ring 9 6 Replacing the Sample Tube O ring 9 7 Inspecting and Changing Vacuum Pump Oil 9 8 Inspecting the Oil 9 8 Changing or Adding Oil...

Page 10: ...olume and Area Distribution C 10 Explanation of Terms C 10 Calculations C 11 Compendium of Variables C 18 Horvath Kawazoe C 19 Slit Pore Geometry original HK C 19 Cylinder Pore Geometry Saito Foley C...

Page 11: ...Based on Statistical Thermodynamics F 1 Theoretical Background F 1 Molecular Simulation Methods F 2 Molecular Dynamics Method F 2 Monte Carlo Method F 2 Density Functional Formulation F 3 Models Inclu...

Page 12: ...Table of Contents Gemini VII viii 239 42828 01 Nov 2013...

Page 13: ...r configurations Organization of the Operator s Manual This operator s manual is organized as follows Chapter Description Chapter 1 GENERAL INFORMATION Provides a general description features and spec...

Page 14: ...ram and analyzer system components Appendix A FORMS Provides a sample information worksheet used to assist in obtaining a sample mass Appendix B ERROR MESSAGES Provides a list of program error message...

Page 15: ...tify notes of importance warnings and cautions Equipment Description Notes contain important information pertinent to the subject matter Warnings contain information to help prevent actions that may c...

Page 16: ...to the following table for a brief summary of some of the model reports and features The basic function of the Gemini analyzers is to determine the surface area of solid materials Analyses are perform...

Page 17: ...VII Series can report discrete point adsorption isotherms consisting of up to 1 000 adsorption points and with the Gemini 2390t up to 1 000 adsorption and desorption isotherm points The Gemini requir...

Page 18: ...analyzer application and is the recommended degassing unit for the analyzer VacPrep 061 The VacPrep degasses up to six samples at up to 400 C with either flowing gas or evacuation FlowPrep 060 The Fl...

Page 19: ...d and or copied and pasted into other documents The report zoom feature provides the viewing of fine graph details and the ability to shift the axes Reports can be customized with a choice of fonts an...

Page 20: ...adsorption only Pressure Resolution 0 1 mmHg Accuracy and Linearity Better than 0 5 full scale Transducer manufacturer s specification Vacuum System External Vacuum source achieving 20 10 3 mmHg or be...

Page 21: ...5 VAC Power 150 VA maximum Frequency 50 to 60 Hz Gases Adsorbate Optimized for nitrogen in a liquid nitrogen sample bath Gemini may be used with non corrosive adsorbate gases having vapor pressures at...

Page 22: ...minimum hard drive formatted in NTFS one partition Video Adapter capable of 1024 768 minimum resolution One RS 232 serial port Two USB ports One 10 BaseT Ethernet port can be 10 100 CD ROM drive Micro...

Page 23: ...oftware components of the Gemini VII Shortcuts File name conventions Menu Structure Instrument Components and Connectors Component Description Power indicator Blinks when power is applied to the analy...

Page 24: ...Front Panel Sample compartment door Power Indicator Component Description Power indicator Blinks when power is applied to the analyzer illuminates when analysis program is initiated and ready for oper...

Page 25: ...e Gemini II 2390p and 2390t Diagram Diagram of port numbers and locations as well as the positions of the balance and sample tubes The empty tube represents the balance tube installed on the left port...

Page 26: ...ve inlet port For attaching the adsorptive analysis gas supply Vacuum pump connector For attaching the vacuum pump hose Keypad connector Not used with the for Gemini VII version Ethernet port For conn...

Page 27: ...Exit from the analyzer program or use the Alt F4 keyboard shortcut If an analysis is in progress the following message is displayed Select Yes and the analysis program closes The analysis continues an...

Page 28: ...ntrol is enabled Refer to Enable Manual Control page 6 8 onscreen graphs and tabular reports Refer to Report Shortcut Menus page 7 17 Shortcut Keys Shortcut keys can be used to activate some menu comm...

Page 29: ...Open a report options file F6 Cascade windows F7 Tile windows F8 Start a report F9 Close all open reports F10 Generate a Heat of Adsorption report Alt F4 Exit the program Shift F2 List sample informat...

Page 30: ...le extensions assigned to files in the Gemini VII program File Status Description All All sample information files in the specified directory Analyzing Sample information files that are currently bein...

Page 31: ...menu contains com mands and in some cases a submenu A submenu is indicated when the command is followed by an arrow Report options RPO Heat of Adsorption Report HOA Thickness curve THK Alpha s curve A...

Page 32: ...ly if a SmartPrep degassing unit is installed on the analyzer The options contained on this menu are explained in the SmartPrep operator s manual Reports Use to run reports and view the results Refer...

Page 33: ...eft of the active window Window Menu Option Description Cascade Stacks open windows in a fanned format so that each window title bar is visible F6 can also be used as a keyboard shortcut Tile Resizes...

Page 34: ...rator s manual Micromeritics on the Web Provides a link to the Micromeritics web page www Micromeritics com Gemini VII on the Web Provides an Internet link to additional Gemini VII information Gemini...

Page 35: ...sing Regulators Guidelines for Connecting Gases Connecting Gases Cleaning and Verifying Gas Lines Inspecting and Changing Vacuum Pump Oil Inspecting and Changing Alumina Changing the Vacuum Pump Exhau...

Page 36: ...Menu Structure Gemini VII 2 14 239 42828 01 Dec 2012...

Page 37: ...ic format Format Description Advanced Displays all parts of sample information and parameter files Navigate to parameter screens by clicking the tabs across the top of the window Basic Displays the en...

Page 38: ...steps to establish defaults for a sample information file in the Advanced format 1 Go to Options Sample Defaults 2 In the Sequence Number alpha numeric text box specify a default file name string The...

Page 39: ...roup box select if data are to be automatically collected or manually entered 7 The optional user defined fields in the User Parameters group box may be used to enter and track information from anothe...

Page 40: ...ns Sample Defaults 3 In the Sequence Number alpha numeric text box specify a default file name string The Sequence Number field must contain a minimum of three 3 numbers This number is incrementally s...

Page 41: ...in Advanced format and saved to the directory specified in Options Parameter Files Directory 7 Click Save then click Close Restricted Format Restricted format presents the sample information file in t...

Page 42: ...tion or use the F2 keyboard shortcut 2 Accept the next sequenced file number or enter a new name in the File name text box Click Open 3 Click OK to create the file 4 Enter a sample description in the...

Page 43: ...file Refer to Spec ifying Sample Defaults page 3 1 If using the Basic format switch to the Advanced format to edit parameter file values If using the Restricted format parameter files cannot be edite...

Page 44: ...analysis Refer to Sample Information Files page 5 8 6 Click the dropdown arrows to select default parameter files for Degas conditions Analysis conditions Adsorptive properties and Report options 7 Cl...

Page 45: ...Entered and click Open or double click the file name The reporting window displays 3 Save the changes in the sample information file by clicking the Save button Opening Files with a Status of Preparin...

Page 46: ...ning Sample Information Files Gemini VII 3 10 239 42828 01 Dec 2012 4 The Sample Information window displays in the specified format Advanced Basic or Restricted The following is shown in Advanced for...

Page 47: ...re enter the values each time an analysis is performed Predefined parameter files are included with the program and can be edited as needed or new parame ter files can be created The Replace button c...

Page 48: ...he file 4 Enter a description in the Description text box 5 Use the Insert button to enter up to five stages of degassing soak temperature ramp rate and soak time 6 Click Save then click Close The fil...

Page 49: ...e the points for the pressure table Use the Insert Delete Clear and Append buttons to assist in entering data 6 Click the following buttons to specify 7 Click Save then click Close The file saves with...

Page 50: ...Enter a name in the File name text box Click Open 3 Click OK to create the file 4 Enter a description in the Adsorptive text box for example the gas and the temperature 5 Enter the mnemonic for the Ad...

Page 51: ...ons files may be defined to include overlay options This system allows the overlay of up to eight plots of different samples onto a ninth plot of the same type or overlay one plot type onto a differ e...

Page 52: ...he Selected Reports list box and click Edit Makes changes as necessary Click OK 8 Click Save then click Close The file saves with a RPO file extension Preparing for Analysis The following table outlin...

Page 53: ...s if used Ensure the detergent is dissolved before placing the sample tubes and filler rods into the water If too much detergent is used it may be difficult to rinse from the sample tubes 4 Fill the s...

Page 54: ...n for two hours at 110 C 9 Remove the sample tubes and filler rods from the oven and allow to cool 10 Wipe a rubber stopper with a lint free cloth 11 Label the sample tube and stopper for identificati...

Page 55: ...support on the balance Tare the balance and allow it to stabilize at zero 0 3 Place the sample tube set on the sample weighing support and place it on the balance 4 Record the stabilized weight on th...

Page 56: ...contaminants which may have adsorbed to the surface or pores Appropriate degassing units are available from Micromeritics Refer to ORDERING INFORMATION page 10 1 for ordering information If using the...

Page 57: ...h the sample tube to the analysis port Ensure it is fully in the port Secure it in place by screwing the connector nut onto the analysis port Hand tighten the connector nut 4 If the balance tube is no...

Page 58: ...e receiving container gradually to minimize thermal shock pour the liquefied gas slowly to prevent splashing vent the receiving container to the atmosphere For glass Dewars Use a plastic stirring rod...

Page 59: ...ce the analysis Dewar onto the elevator 2 Fill the Dewar with the analysis bath liquid liquid nitrogen Large Dewar fill to about 5 cm 2 in from the top Small Dewar fill to about 2 cm 3 4 in from the t...

Page 60: ...partment door Performing an Analysis Begin analysis after the sample has been degassed and transferred to the analysis port The system pro vides these types of analyses Start Analysis standard allows...

Page 61: ...determination 4 Click Report after analysis to automatically generate reports when the analysis is complete On the Report Settings window select the report destination Click OK 5 Click Start to start...

Page 62: ...r dispose of the sample material as applicable QuickStart Analysis When using the QuickStart option it is not necessary to prepare sample files in advance Sample files are assigned automatically and g...

Page 63: ...A window displays data as they are collected A short delay is encountered before the port status changes from the Idle state at the bottom of the screen 6 When the analysis is complete remove the sam...

Page 64: ...ore or dispose of the sample material as applicable Generating Reports Reports Start Report file or use the F8 keyboard shortcut 1 Select the report in the Name column The selected report name appears...

Page 65: ...3 29 3 If only one file was selected in step 1 the Select Reports window displays Verify the reports to generate and click OK If multiple files were selected this window does not display 4 Click a tab...

Page 66: ...down the Ctrl key on the keyboard while selecting the files To sort a column click the column header 3 Click Open 4 In the Report Settings window select one of the following Preview to send the file...

Page 67: ...to create a list of sample file information for example file name date time the file was created or last edited file identification and file status 1 Go to File List file type file 2 From the Name co...

Page 68: ...estination directory and enter a file name in the File name text box Select to save the file as a REP XLS or TXT file format 5 Click OK The following example shows a sample information file printed to...

Page 69: ...o export To select more than one file hold down the Ctrl key on the keyboard while selecting the files To sort a column click the column header 3 Click Open The file is automatically converted to a SM...

Page 70: ...Select to save the file as a REP XLS or TXT file format 5 Click OK to close the window Converting Files Converts StarDriver files MGD extension to a sample information file with a SMP file extension O...

Page 71: ...Overlays overlay two different types of plots from one sample This type of overlay is available only for BJH Adsorption Desorption DFT Pore Size Surface Energy Dollimore Heal Adsorption Desorption Ho...

Page 72: ...ighlight Isotherm and click Edit b On the Isotherm Report Options window select a plot in the Selected Reports group box then click the Options button to the right of the selected plot c On the Plot O...

Page 73: ...other fields Click OK to return to the Report Options tab c Continue with Step 3 BJH Adsorption BJH Desorption Dollimore Heal Adsorption Dollimore Heal Desorption MP Method a In the Selected Reports l...

Page 74: ...s with the name of the edited and saved file in the File name text box To select more than one file hold down the Ctrl key on the keyboard while selecting the files 7 Click Open 8 Select the report de...

Page 75: ...Gemini VII Generating Graph Overlays 239 42828 01 Dec 2012 3 39 10 The report screen displays with tabs across the top of the screen Click each tab to view the reports...

Page 76: ...report 1 Go to File Open Sample Information 2 Select a sample file to overlay graphs of other samples To select more than one file hold down the Ctrl key on the keyboard while selecting the files To...

Page 77: ...report and click and click Edit 5 Click the dropdown arrow on the Overlay field and select a second variable to overlay Click OK to return to the Report Options window 6 Click OK again to return to th...

Page 78: ...lick Open and select the report destination in the Report Settings window and click OK 10 If only one file was selected in step 8 the Selected Reports window displays Verify the reports to generate an...

Page 79: ...ng calibration files importing an analyzer from a previous installation on this PC adding or modifying SmartPrep uninstalling the software The analysis program can also be installed for offline data m...

Page 80: ...atically starts the installation If the installation does not immediately start navigate to the CD Rom drive locate and double click the setup exe file System Installation videos for hardware componen...

Page 81: ...not proceed with installation until these tasks have been completed If the prerequisites have been met click Next 4 On the Choose Users screen select one of the following then click Next Install for a...

Page 82: ...ck Next to accept the default installation directory or click Browse to change the installation location then click Next 6 On the Choose Start Menu Folder screen select a folder for the program shortc...

Page 83: ...system for the each analyzer and serial number to be installed In the Step 1 group box If Then installing the analysis program during initial installation select the number of analyzers to be installe...

Page 84: ...abel is located near the power switch b Click Next 9 On the Ethernet Ports screen select one option from the following table If Then the configured port is listed Select the port then click Next to pr...

Page 85: ...Next A screen displays for each unit installed 11 If installing a SmartPrep at this time on the Configure SmartPrep screen select the number of SmartPrep instruments to be installed and the Com Port...

Page 86: ...gistration screen displays Click the appropriate link to register the product or to log into your portal or click Next to register later 14 The Completing the Gemini VII Setup screen displays Select o...

Page 87: ...gram 1 Ensure that the analysis program is not operating and the analyzer is idle 2 Insert the setup CD into the CD ROM drive The setup program starts automatically If the program does not start autom...

Page 88: ...not overwritten There are three types of subsequent installations a later version than the current installation the same version as the current installation an earlier version than the current install...

Page 89: ...ions only the applicable option displays and click Next Upgrade software to version n from version n Reinstall software version n Downgrade software to version n from version n If the option Downgrade...

Page 90: ...VII Installed screen displays Click Next 5 The Gemini VII Reinstalled screen displays Select one of the following Reboot now I want to manually reboot later Select the Create a desktop icon checkbox t...

Page 91: ...connect an Ethernet cable from the Ethernet labeled port on the rear of the analyzer to a numbered port on the Ethernet switch taking care not to use the uplink port on the switch 3 Use an Ethernet c...

Page 92: ...Installing the Software Gemini VII 4 14 239 42828 01 Dec 2012 Software 1 Start the setup program The Welcome screen displays Click Next 2 On the Select Task screen select Add an analyzer Click Next...

Page 93: ...ling the Software 239 42828 01 Dec 2012 4 15 3 On the Add Analyzer screen enter the serial number of the analyzer being added Click Next 4 The Analyzer S N n Installed screen indicates a successful in...

Page 94: ...omputer Source PC to a another Destination PC This operation does not move sample or parameter files Use a file management program such as Explorer or a backup restore utility to move these types of f...

Page 95: ...ftware 239 42828 01 Dec 2012 4 17 3 On the Select Task screen select Move an analyzer from one PC to another PC Click Next 4 On the Move Analyzer screen use the dropdown list to select the source anal...

Page 96: ...the CD from the CD ROM drive and store in a safe location b Disconnect the Ethernet cable from the Source computer and reconnect it to the configured Ethernet port on the Destination computer If movi...

Page 97: ...reen displays Click Next 8 On the Move Analyzer screen click Next 9 On the Analyzer Installed screen click Finish Sample and parameter files are not copied and moved with the analyzer Use a file manag...

Page 98: ...talling the Software Gemini VII 4 20 239 42828 01 Dec 2012 Removing an Analyzer 1 Start the setup program On the Welcome screen click Next 2 On the Select Task screen select Remove an analyzer Click N...

Page 99: ...unit and serial number of the analyzer to be removed Click Next 4 The Analyzer Removed screen displays Click Finish This operation removes the selected instrument from the list of attached instruments...

Page 100: ...s section provides instructions and changing an analyzer s Ethernet port in case of an Ethernet port malfunction Ensure that the new Ethernet port has been configured 1 Start the setup program On the...

Page 101: ...one option from the following table If Then the configured port is listed Select the port then click Next to proceed to the next step the configured port is not listed Click Specify On the Specify Eth...

Page 102: ...nalyzer Configuration Updated screen click Finish Reinstalling Calibration Files for an Analyzer Calibration files specific to the analyzer are contained on the original calibration CD only and not on...

Page 103: ...re 239 42828 01 Dec 2012 4 25 2 On the Select Task screen select Reinstall calibration files for an analyzer Click Next 3 On the Reinstall Calibration Files screen select the unit and serial number fr...

Page 104: ...Installing the Software Gemini VII 4 26 239 42828 01 Dec 2012 4 On the Analyzer S N n Installed screen click Next 5 On the Analyzer Calibration Reinstalled screen click Finish...

Page 105: ...ous Installation on this PC This section provides instructions on importing an analyzer from a previous installation on the same PC 1 Start the setup program On the Welcome screen click Next 2 On the...

Page 106: ...click the Browse button to locate the installation directory of the previously installed instrument then select the serial number of the instrument files to be imported Click Next 4 When the previous...

Page 107: ...012 4 29 5 On the Analyzer Added screen click Finish Adding or Modifying SmartPrep This section provides instructions on how to configure the software to connect up to four SmartPrep instruments 1 Sta...

Page 108: ...239 42828 01 Dec 2012 2 On the Select Task screen select Add or Modify SmartPrep Click Next 3 On the Configure SmartPrep screen select the number of SmartPrep units to be installed and the Com Port f...

Page 109: ...ox Click Finish to complete the process Uninstalling the Analysis Program This section provides instructions on uninstalling the analysis program status files analyzer setup files and resulting empty...

Page 110: ...the Analysis Program Gemini VII 4 32 239 42828 01 Dec 2012 3 The Uninstallation Complete screen displays Click Next 4 The Completing the Gemini VII Uninstall screen displays Click Finish to close the...

Page 111: ...d button descriptions are listed in a Common table at the beginning of their respective chapters Field and button descriptions not listed in the Common table are listed in their appropriate heading Re...

Page 112: ...elected File saves the report as a file Click the Browse icon to the right of the text field to select the directory where the new file will be stored Enter the new file name in the File name text box...

Page 113: ...cted report Refer to Report Tool Bar page 7 14 When an analysis has not been run on a sample this button is disabled Print button Sends the report to the selected destination screen printer or file Re...

Page 114: ...e generated by the program The sample information file extension is SMP Parameter files the File name text box contains an asterisk and a default file extension depending on the type of parameter file...

Page 115: ...ve sample file Save As t Curve or Alpha S Curve t Curve saves the relative pressures and corresponding thicknesses as an ASCII text file with a THK file extension These data are derived by dividing th...

Page 116: ...Prints the contents of one or more sample or reports options files to either the screen a printer or to a file List Provides the option to create a list of sample or report options file information fo...

Page 117: ...a prompt displays providing the option to save the file If an analysis is in progress a prompt displays providing the option to exit the program YES saves the changes before exiting the program NO ex...

Page 118: ...en the sample file is created select the Analysis Conditions file for the analysis conditions Once it becomes part of the new sample file edit the new file as needed without affecting the original Ana...

Page 119: ...alysis is running Manually entered select to manually enter data If Manually entered is selected an Entered Data tab displays at the top of the window User Parameters group box These fields are primar...

Page 120: ...er Use this option when the SmartPrep Degasser is installed Close button Preview button Save button Refer to Common Fields and Buttons File Menu Options page 5 1 Field or Button Description Descriptio...

Page 121: ...s and possibly calculation assignments at which data isotherms are to be collected The relative pressures may span the entire range of 0 00000001 to 0 995 p po There must be one adsorption branch foll...

Page 122: ...re dosing checkbox Select to specify pressure targets in mmHg mbar or kPa rather than relative pressure This option is typically selected when using adsorptives at analysis conditions above the critic...

Page 123: ...ect to insert geometrically spaced points from the low pressure range For example to insert 5 points with a 0 01 starting pressure and a 0 16 ending pressure the following points are inserted into the...

Page 124: ...n arrow to select predefined pressure points for surface area t Plot micropore and or BJH adsorption desorption Select Adsorption total pore volume Desorption total pore volume and or Saturation to in...

Page 125: ...sure the free space automatically over the sample prior to data collection Enter select to enter warm and cold free space manually and enter the amount in the text box Calculate select to have the fre...

Page 126: ...quilibration With this method the analyzer increases pressure in steps to the next specified level for data collection It maintains this pressure and monitors volumes or quantities adsorbed When the r...

Page 127: ...lect the adsorptive using the Replace button Mnemonic text box Enter the mnemonic of the adsorptive gas Non ideality factor text box Enter a factor to compensate for the forces of attraction between m...

Page 128: ...reports To include the parameter files in the dropdown list on the Basic and Restricted Sample Information windows save the file to the directory specified in Options Parameter Files Directory Refer t...

Page 129: ...or additional information on thermal transpiration Inside diameter of sample tube text box Enabled when Apply thermal transpiration correction is selected Enter the inside diameter of the sample tube...

Page 130: ...he Collected Data window the isotherm is interpo lated to the value in the P Po fields and the point is used for the total pore volume calculation Otherwise the point selected with calculation assignm...

Page 131: ...selection of pass fail criteria Item n group boxes Upper Lower options and text boxes specify upper and lower limits for the selected parameter A range can be left open by not selecting the limit In...

Page 132: ...erature In the Selected Reports list box highlight Isotherm then click Edit Field or Button Description Select Reports group box Select the checkbox to the left of each applicable report to include th...

Page 133: ...ed during the analysis Time between points time elapsed between points during the analysis Plot Options group box Select the type of isotherm to plot adsorption or desorption Quantity Adsorbed group b...

Page 134: ...muir then click Edit The BET calculation obtains the sample surface area value by determining the monolayer volume of adsorbed gas from the isotherm data The Langmuir calculation determines the surfac...

Page 135: ...ations If Use calculation assignments is selected collected data are used Use pressure range option select and enter the pressure range to be used in the text boxes if not using the Interpolate pressu...

Page 136: ...ir monolayer volume and constant to produce an isotherm Uses the BET Langmuir monolayer volume and constant to produce an isotherm X axis linear X axes begin at zero The X axis field shows the relativ...

Page 137: ...ield or Button Description Specify monolayer capacity checkbox Select and enter the monolayer capacity of the sample Absolute pressure range text boxes Enter a pressure range when calculation assignme...

Page 138: ...axis linear X axes begin at zero The X axis field shows the absolute pressure Y axis Y axes begin at zero The Y axis field shows the quantity of gas adsorbed Cancel button From To text boxes OK button...

Page 139: ...quantity of gas adsorbed Temkin Isotherm plot checkbox Overlays the Temkin isotherm with the analysis data X axis linear X axes begin at zero The X axis field shows the absolute pressure Y axis Y axes...

Page 140: ...In the Selected Reports list box highlight t Plot then click Edit Field or Button Description Thickness Curve group box Select the thickness curve Click Edit to modify the values in the equation for...

Page 141: ...a space or a tab Kruk Jaroniec Sayari Halsey Harkins and Jura Broekhoff de Boer Carbon Black STSA select the thickness curve option and click the Edit button Modify the equation for the selected curve...

Page 142: ...Enter the value to correct for surface areas that are not smooth This brings the values for BET surface area and micropore surface area into accordance For most samples the default value of 1 000 is...

Page 143: ...on To import values from an existing thickness curve ALS ASCII file click Open and select the file containing the values The table to be imported must be saved as ASCII text with a ALS extension It mu...

Page 144: ...t checkbox Select to plot data in graph format X axis the X axis field shows the relative pressure Y axis the Y axis field shows the quantity of gas adsorbed Tabular Report checkbox Overlay Samples ch...

Page 145: ...ears to the left of the Browse button f Plot checkbox Select to generate a normalized isotherm X axis the X axis field is dimensionless in units of alpha s ratio Y axis the Y axis field shows the quan...

Page 146: ...rption then click Edit An incomplete pore distribution may be generated if a thickness curve selection is not a good match for the sample being analyzed Field or Button Description Thickness Curve gro...

Page 147: ...rt Options window Adsorptive button Displays the BJH Adsorptive Options window The recommended adsorptives and their values are shown Up to eight adsorptive adsorbate property factor combinations may...

Page 148: ...or calculating the data for this report If Use calculation assignments is selected collected data points assigned to this report type are used Cancel button Edit button OK button Refer to Common Field...

Page 149: ...s indicate the column order and data contents for the report Table button The fixed pore size table must contain a minimum of two points The points must be strictly decreasing Enabled only when Fixed...

Page 150: ...and click Edit Field or Button Description Plot curve Plot points checkboxes Refer to Isotherm Report Options page 5 22 X Axis Select to have the X axis on a logarithmic or linear scale Y Axis Variab...

Page 151: ...more Heal reports from both adsorption and desorption data In the Selected Reports list box highlight Dollimore Heal Adsorption or Dollimore Heal Desorption then click Edit Dollimore Heal Adsorption D...

Page 152: ...e micropores in the sample material When Sphere is selected options in the Interaction Parameter group box are disabled Interaction Parameter group box Select to determine which interaction parameter...

Page 153: ...er enter the diameter of the sample or adsorbent atom Diameter at zero energy enter the diameter of an atom at zero interaction energy 2 5 1 6 diameter Adsorptive group box Contains the parameters for...

Page 154: ...er unit area of the adsorbent or adsorptive Apply Cheng Yang correction checkbox Select to apply the Cheng Yang correction to the pore size analysis This correction substitutes the Langmuir equation o...

Page 155: ...it To customize the order and data contents of reports click the dropdown arrow for a column and select the data type for that column Plot Options Highlight a plot option in the Selected Reports list...

Page 156: ...ze then click Edit X Axis Y Axis X Axis the X axis field shows pore radius or diameter in angstroms or nanometers Y Axis the Y axis field shows the quantity of gas adsorbed Variable dropdown list clic...

Page 157: ...utton Refer to BJH Adsorption Desorption Report Options page 5 36 Models list box Lists the models that meet the criteria specified and which match the adsorbate and temperature of the sample data If...

Page 158: ...data display Autoscale Options group box select to autoscale the x axis and or y axes Overlay dropdown list select an overlay for the report Axis Range group box From To fields are enabled when Autosc...

Page 159: ...ports list box highlight DFT Surface Energy then click Edit DFT Surface Energy Report Options fields and buttons are identical to the DFT Pore Size Report Options page 5 46 Dubinin Report Options The...

Page 160: ...the entered exponent value Field or Button Description Report Type group box Select the checkbox to specify report types If Astakhov is selected either select the Optimize exponent checkbox or enter...

Page 161: ...d or Button Description Overlay Samples checkbox Refer to BET Langmuir Surface Area Report Options page 5 24 Autoscale x axis Autoscale y axis checkboxes Select an option to have the X and or Y axes s...

Page 162: ...ints checkboxes Overlay Samples checkbox Refer to Isotherm Report Options page 5 22 Autoscale x axis Autoscale y axis checkboxes Select an option to have the X and or Y axes scaled automatically Both...

Page 163: ...highlight MP Method then click the Equation button Pore size can be expressed in angstroms or nanometers Select Options Units to specify the unit Refer to UNIT MENU page 6 1 Field or Button Descripti...

Page 164: ...elect the data type for that column Plot Options Highlight a plot option in the Selected Reports list box and click Edit to customize the plotting method The MP Method reports hydraulic radius only If...

Page 165: ...sure Po and temperature Analysis method Isotherm collection Sample Log Report In the Selected Reports list box select Sample Log This report provides the following information Manual control operation...

Page 166: ...xamined by the software to determine if the results are within typical ranges If the data selected for validation are determined to be out of range a warning displays and suggestions are given for cor...

Page 167: ...2012 5 57 Entered or Collected Data File If Manually Entered is selected on the Advanced view of the Sample information window an Entered Data tab displays If Automatically Collected is selected a Co...

Page 168: ...lly entered data only select if the pressures are Relative or Absolute Use calculation assignments checkbox Select if calculation data are to be used p and T button Refer to Analysis Conditions Files...

Page 169: ...nd buttons The title bar of the main window displays as Unit n S N n for each attached unit Each unit has a status window displayed in different colors The Unit menu does not appear on the menu bar if...

Page 170: ...in an analysis Select an existing analysis file or create a new one Then specify analysis defaults Field or Button Description Browse button Click to search for a file Select from a file in the Name c...

Page 171: ...ent Schematic displays a schematic of the analyzer Refer to Show Instrument Schematic page 6 12 Edit button Click to edit information in the sample information file Clear button Click to clear all fie...

Page 172: ...alysis button Click to select a print destination Report after analysis checkbox select to send the report to the screen printer or file in either ASCII XLS or REP format Export after analysis checkbo...

Page 173: ...formation file for and assigns the default parameters Edit the parameters of a file using the Edit button or select another file using the Browse button Additional analyses can be scheduled by clickin...

Page 174: ...s selected from the Analysis Conditions tab by clicking the Po and T button Analyzer Model Description Model 2390a Measure the Po only in the Sample tube Ensure a sample tube with no filler rod is att...

Page 175: ...k Analysis Use to obtain sample tube parameters when using a calculated free space A blank analysis can also be used for diagnostic purposes Blank Analysis fields are identical to the Start Analysis p...

Page 176: ...f the following instrument schematic is not immediately visible select Unit n Show Instrument Schematic Field or Button Description Open Sample File button Click to open the Open Sample Information Fi...

Page 177: ...ance tube left side and sample tube Volume adsorbed transducer upper and the differential pressure transducer The reading for the Volume Adsorbed transducer is displayed just above its symbol The read...

Page 178: ...instrument schematic Saturation pressure Po tube Not displayed for Gemini VII 2390a Valves Description 1 Vacuum valve 2 Adsorptive valve 3 Helium valve 4 b Balance reservoir valve 4 s Analysis reservo...

Page 179: ...nd 5s The valve symbol changes to green An alternate method is to either double click the valve or select the valve and press the keyboard spacebar to turn it off on Close closes the selected valve Th...

Page 180: ...by evacuating the sample Enter target displays the Servo Valve Settings window The entered target pressure displays to the left of the sample servo valve icon When the cursor changes to this icon rig...

Page 181: ...status window shows the current status for each port Use this option if there is an automatic operation in progress and the sample file needs to be edited there are multiple units attached to the comp...

Page 182: ...le Sample file number Stage Stage of the analysis as in status bar Last Point Last point and number of points requested P Absolute pressure of last point P Po Relative pressure of last point Q Quantit...

Page 183: ...n Analysis Calibration Message checkboxes Select which logs to display Add Log Entry button Click to manually enter information into the instrument log window for example Changed the port filter To en...

Page 184: ...saturation pressure Volume Correction text box Displays the volume correction of the attached analyzer If a different value is entered in this field it is stored with sample data at the start of an an...

Page 185: ...mini VII Service USERDIAG directory The service representative may request an emailed or faxed copy of the file for diagnostic purposes Field or Button Description Test dropdown list Click to select t...

Page 186: ...analysis in progress Select the ports containing the analysis to suspend or resume Report button Click to view a list of reports to be generated during the test Report dropdown list Select a report to...

Page 187: ...e 7 14 for additional information on viewing customizing and printing reports Calibration Unit n Calibration Use to perform system calibrations Disabled calibration options can be accessed only with t...

Page 188: ...acuate the manifold and zero out the selected transducers Refer to Zero Pressure page 9 30 Match Transducers Unit n Calibration Match Transducers Use to zero and match the selected transducers to the...

Page 189: ...ate the servo valve to the sample pressure transducer The sample pressure transducer should be calibrated before starting this calibration procedure The servo valve should always be reca librated afte...

Page 190: ...can later be reloaded using Unit n Calibration Load from File menu option Field or Button Description File name dropdown list The default file naming convention for calibration files can be used or th...

Page 191: ...backup of the current file is created and saved as SN last cal The backup file is overwritten each time a new one is created Service Test Unit n Service Test Use for service tests performed only with...

Page 192: ...Service Test Gemini VII 6 24 239 42828 01 Dec 2012...

Page 193: ...s menu options used to customize and run reports This chapter provides details of Reports menu options commonly used functions and buttons field by field descriptions and sample reports Reports can be...

Page 194: ...will appear in the File name text box Click Open or double click the file name in the Name column to open the file Multiple files can be selected by holding down the Ctrl key on the keyboard while se...

Page 195: ...a saved report SPC Report Options Reports SPC Report Options Use to generate reports with various SPC Statistical Process Control options All selected variables must be computed for each sample file...

Page 196: ...4 239 42828 01 Dec 2012 If additional report options are required click the More button The selected items also appear as options on the Reports Control Chart screen Click the Graph n button then cli...

Page 197: ...elect to show a graphic on the report header Click the Browse button to locate the graphic in either BMP or EMF format Height Width enter the height and width of the selected graphic These values dete...

Page 198: ...report generation Multiple files can be selected by holding down the Ctrl key on the keyboard while selecting the files Available Files contains files located in the directory specified in the Look In...

Page 199: ...plots the changes in a statistic Report button Click to view the report for the items selected Save as Default button Click to save selected report options as default report settings Browse button Can...

Page 200: ...which is the earliest analyzed file Days sorts by the number of days elapsed from the first file placed on the list which is the earliest analyzed file Graph n buttons Click to define the Y axis of e...

Page 201: ...ple of the standard deviation or at specified positions Entered When Entered is selected enter the High limit and Low limit fields with appropriate values Show report title checkbox and text box Show...

Page 202: ...orbent and the adsorption capacity Multiple adsorption isotherms are obtained on the same sample using the same adsorptive but at different temperatures to obtain the heat of adsorption Field or Butto...

Page 203: ...ed and number of points to insert Insert button insert a row above the selected row Delete button deletes the selected row Clear button clears the entire table of all entries except one Append button...

Page 204: ...rsus the temperature Heat of adsorption plot checkbox Select to generate the Heat of Adsorption data in a graphical format Open button Click to select and open a Heat of Adsorption file Browse button...

Page 205: ...ort header can also contain a graphic and a title Tabular and graphical reports contain sample and instrument statistics such as analysis date time analysis conditions etc The headers contain notes of...

Page 206: ...ed reports The same reports display as tabs across the top of the report header unless the report has been hidden using the Hide button Show button Jumps to the selected report in the Reports list box...

Page 207: ...ears all selections OK button prints the selected report to the printer indicated Cancel button closes the Print window Copies group box select the number of copies and collate option Save button Save...

Page 208: ...specify default report parameters for fonts and curve properties Font group box Font Type list box allows font type and attributes to be edited for the selected item Select an item in the list click E...

Page 209: ...list select a histogram fill option from the list Graph border line thickness text box enter a thickness number for the graph border Load button click to load the last saved default settings Save butt...

Page 210: ...u and select Left or Right for the move Align column Right click on the column to be aligned Select Align Column on the shortcut menu and select Left Right or Center Hide column Select a column to hid...

Page 211: ...y table as text Select to copy the report contents to the clipboard as tab delimited text It can then be pasted into another document Option Description Autoscale all axes Returns the report to full v...

Page 212: ...rpolation point style and pen style for the selected curve Color button click to change the curve color Use default thickness checkbox select to use the default curve thickness Deselect the checkbox a...

Page 213: ...e to modify the label of the selected axis Title font button use to modify the font for the selected axis label Deselect the Use default font to enable font options Select the font attributes and clic...

Page 214: ...ns Select the font attributes and click OK Gridlines Major Minor dropdown lists select to change how to display major minor gridlines Edit legend Select to change the legend location and font Click Fo...

Page 215: ...e button The enlarged area fills the graph area To return to normal view right click in the graph area and select Autoscale all axes or Reset all axes to initial setting on the shortcut menu Axis Cros...

Page 216: ...Report Examples Gemini VII 7 24 239 42828 01 Dec 2012 Report Examples This section of the manual contains samples of some of the available reports Most of the reports can be customized...

Page 217: ...Gemini VII Report Examples 239 42828 01 Dec 2012 7 25 Isotherm Linear Plot...

Page 218: ...Report Examples Gemini VII 7 26 239 42828 01 Dec 2012 BET Surface Area Report...

Page 219: ...Gemini VII Report Examples 239 42828 01 Dec 2012 7 27 BET Surface Area Plot...

Page 220: ...Report Examples Gemini VII 7 28 239 42828 01 Dec 2012 t Plot...

Page 221: ...Gemini VII Report Examples 239 42828 01 Dec 2012 7 29 BJH Adsorption Cumulative Pore Volume...

Page 222: ...Report Examples Gemini VII 7 30 239 42828 01 Dec 2012 BJH Adsorption dV dlog w Pore Volume...

Page 223: ...information files and report option files specifying how units appear on application windows and reports specifying how graph grid lines appear on reports specifying the location of the parameter file...

Page 224: ...laboratories where analysis conditions must remain constant for example in the pharmaceutical industry The Advanced format is not available from the Restricted format Refer to Specifying Sample Defaul...

Page 225: ...s Graph Grid Lines Use to select how grid lines appear on reports This menu option is not available if using Restricted format Field or Button Description X Axis Y Axis options Select major and or min...

Page 226: ...mode is a password protected option used to perform certain service tests with the assis tance of a trained Micromeritics service representative This password is supplied by your service representativ...

Page 227: ...s bath fluid in the Dewar at the start of an analysis Entry of incorrect system volume for analysis Impure gas supply When unexpected analysis results occur check the above first Some common operation...

Page 228: ...to hold a vacuum Check the centering ring at the pump intake port Replace if necessary Refer to Replacing the Alumina in the Oil Vapor Trap page 9 11 Check the centering ring at the top of the oil va...

Page 229: ...rician check cord using a test meter Replace the cord if defective Loose internal connection or broken wire Call a Micromeritics Service Representative for repair or replacement information Expected r...

Page 230: ...re The analyzer saves entered and collected data in case of power failure File parameters and any other data entered will still be present when power is restored If an analysis was in progress when th...

Page 231: ...e slightly higher which in turn can cause pore volume measurement errors in those samples exhibit ing high isotherm slope above 0 97 relative pressure Accumulated ice is likely to melt and form a pool...

Page 232: ...reading much lower than normal A contaminated filter should be replaced as follows 1 Select Unit n Show Instrument Schematic then Unit n Enable Manual Control 2 Right click on the valve of the approp...

Page 233: ...er the new O ring is in place insert the sample tube back into the sample port until it is fully seated 5 Slide the sample tube connector nut up the tube the ferrule and O ring will move along with th...

Page 234: ...The oil level should be midway between the indicators on the oil level window when the pump is running Oil in good condition is clean clear or light in color and transparent Change the oil if it has d...

Page 235: ...he clamp open and remove the trap from the hose 3 Grasp the handle on top of the vacuum pump and place it on a work table 4 Drain the used oil a Place a waste container under the drain spout b Remove...

Page 236: ...to tighten 9 Check the alumina in the oil vapor trap If most of the pellets are no longer white replace the alumina before reattaching the vacuum pump 10 Reconnect the vacuum pump hose 11 Reconnect t...

Page 237: ...p from the hose 3 Loosen the wing nut on the clamp at the bottom of the oil vapor trap Swing the clamp open and remove the trap 4 Remove one end fitting from the trap body and dispose of the used alum...

Page 238: ...n c Bake the alumina for two hours at 300 C d Remove the baked alumina from the oven and allow it to cool until luke warm A desiccator may be used to speed the cooling process 7 Use a small spatula to...

Page 239: ...fitting back onto the trap and tighten securely by hand 12 Lightly tap both ends of the trap body on the work surface to remove remaining dust from the pellets 13 Inspect the centering ring before pl...

Page 240: ...nge of the intake port and the flange of the trap Swing the clamp fastening screw toward the intake port until it fits into the slot in the other half of the clamp Tighten the wing nut securely by han...

Page 241: ...f oil vapor and should be replaced when it becomes so saturated with oil that it is ineffective 1 Turn the power to the unit off by either removing the plug from the power source or by turning the pow...

Page 242: ...est that a leak test be performed to determine if there is a system leak The service representative may request a copy of the report generated by this test The following information is displayed durin...

Page 243: ...at all tests have a Passed status by clicking the tabs and looking for the Passed status for each test run 8 Click Save As and accept the default name displayed in the File name field 9 Click Save Mak...

Page 244: ...ed before connecting to the analyzer The following instructions describe a typical installation Some configurations require additional com ponents for example regulator expansion kits when one gas sou...

Page 245: ...tle Move the replacement bottle close to the instrument and tether it into place It is not necessary to dis connect the gas line from the regulator or the instrument 1 Use an appropriate cylinder wren...

Page 246: ...ontrol knob fully counterclockwise b Slowly open the gas bottle shut off valve then close it c Observe the pressure on the high pressure gauge If the pressure is stable proceed with the next step If t...

Page 247: ...essure a Turn the regulator control knob clockwise until the low pressure gauge reads 15 psig 103 kPag b Open the regulator shut off valve c Open the gas bottle shut off valve and flow gas for 10 to 3...

Page 248: ...To start diagnostic testing go to Unit n Diagnostics 2 Click the down arrow to the right of the Test field and select Clean and Verify Analysis Gas Line Rev n This procedure uses the analysis gas as a...

Page 249: ...off Valve 1 report should read Passed A Passed reading indicates the gas line from the instrument to the regulator is clean and leak free If the Leak Rate field indicates Failed a leak is indicated be...

Page 250: ...line from the instrument to the regulator is clean and leak free If the Leak Rate field indicates Failed a leak is indicated between this connection Check the connections from the regulator shut off...

Page 251: ...or more valves is not in the proper position Set the valves as shown below and ensure the appropriate pressure is displayed on the low pressure gauge If running the test again close the gas bottle va...

Page 252: ...ormed before contacting your Micromeritics Service Representative Helium is required for performing a blank analysis since a measured free space is required If helium is unavailable contact a Micromer...

Page 253: ...rate reports to the specified destination when the analysis is complete On the Report Settings window select the report destination Click OK 7 Click Start to start the analysis A window displays data...

Page 254: ...the accessories kit to perform this analysis The results should match those shown on the label of the reference material bottle within the tolerance level 1 Select File Open Sample Information and cre...

Page 255: ...ified destination when the analysis is complete On the Report Settings window select the report destination Click OK 5 Click the Start button Graphs are displayed as the analyses are performed When th...

Page 256: ...calibrations are greyed out on the Calibration menu To review calibration details of the analyzer go to Unit n Unit Configuration The following calibrations can be performed without the assistance of...

Page 257: ...efore clicking Start Sample Servo Use to calibrate the servo valve to the sample pressure transducer 1 Select Unit n Calibration Sample Servo 2 Click Start The window closes when the calibration is co...

Page 258: ...the balance servo valve Ensure that empty tubes are installed on the sample and balance ports 1 Select Unit n Calibration Balance Servo 2 Click Start The window closes when the calibration is complete...

Page 259: ...lowing gas or evacuation by vacuum evacuation requires a vacuum pump and a regulator 065 00000 00 SmartPrep 065 Windows interface allowing programmable ramp and soak rates degasses up to six samples w...

Page 260: ...m2 g 15 g 004 16818 00 Reference Material Glass SA 5 8 m2 g 004 16821 00 Reference Material Silica alumina 215 m2 g 10 g 004 16833 00 Reference Material Carbon black 30 6 m2 g 10 g Sample Tubes and Ac...

Page 261: ...pport Software and Manuals 239 20828 00 Gemini VII current version software 239 42828 01 Gemini VII operator s manual Vacuum Pump and Accessories 004 16003 01 Vacuum Pump Oil 1 liter 004 16830 00 Acti...

Page 262: ...ec 2012 062 33002 00 Oil Vapor Trap includes alumina and instructions Cables 003 63801 01 Cable Ethernet straight thru Miscellaneous 021 00000 00 Liquid Nitrogen Transfer System Model 021 Part Number...

Page 263: ...Gemini VII Appendix A 239 42828 01 Dec 2012 A 1 A FORMS This appendix contains the following form Sample Data Worksheet Copy and use this form as needed...

Page 264: ......

Page 265: ...__________________________________________________ _________________________________________________________________________________ Sample Mass g NOTE Record all values in grams Before Degas After De...

Page 266: ......

Page 267: ...f this does not eliminate the problem attempt operation using a backup copy of the file Cause B Hard disk may be damaged Action B Contact a Micromeritics service representative if this error message c...

Page 268: ...unction other than the analyzer program Action Select Yes to update the directory information with data from each new file This operation may take a minute Select No to locate the file manually This o...

Page 269: ...invalid file name was entered Action See the description of file naming conventions in a Windows manual and re enter the name Cause More than 50 files are open at the same time Action Refer to an oper...

Page 270: ...has failed The application stops Action A Usually this message is preceded by another message giving the reason for the instrument s failure to initialize Refer to the instructions for that message Ac...

Page 271: ...a list of all windows one of which may contain this file Cause An attempt was made to use a sample file containing errors that is currently open Action Go to the window containing the file correct the...

Page 272: ...ation information and system options information used during program startup does not exist Action Run the analyzer setup program select Change analyzer setup and create the control file used by the a...

Page 273: ...s at least three digits Cause No more sample information files can be created using the currently entered file name sequence number Action Select Options Sample defaults and enter another sequence num...

Page 274: ...rary files during the report possibly due to insufficient disk space Action B Check the space available on the hard disk Cause C An internal processing error occurred Action C Contact a Micromeritics...

Page 275: ...ocess of performing a calibration operation was started Action Calibration operations should only be done by or under the direction of qualified service personnel Cause A calibration operation was per...

Page 276: ...brary files used by an application does not exist on disk Action Add the library into the Libraries folder Cause The selected file does not have a supported file extension Action Open the adsorptive p...

Page 277: ...a valid file Action Select only files that have been created by the proper program Cause An attempt was made to start an analysis using a file that contains errors and is open for editing Action Finis...

Page 278: ...points selected for the Dubinin report fall within the selected relative pressure range Action Edit the calculation assignments or the fitted relative pressure range Cause There are fewer than two val...

Page 279: ...tion of data for reporting could not be successfully completed No Horvath Kawazoe reports will be produced This message will always be preceded with another one containing additional information Actio...

Page 280: ...ssure remove them and reproduce the Horvath Kawazoe reports Cause The Cheng Yang correction to the Horvath Kawazoe equation requires the value of the monolayer volume as calculated from the Langmuir e...

Page 281: ...ng range Action Change the 1 0 entered value Cause Calculation assignments are not being used and more than one of the report pressure table points is above the range of the collected data and more th...

Page 282: ...could not be restored Default settings will be used Action No action Cause A sample file has been included in the Heat of Adsorption report that does not have enough data Action Remove the file from t...

Page 283: ...ents for the t Plot report Action B Edit the fitted thickness range in the t Plot report editor Cause Fewer than two points were assigned to the requested surface area calculation in the collected dat...

Page 284: ...range in the sample file Cause At least two points are required for the MP Method calculations Action Edit the calculation assignments for the MP Method report Cause An attempt was made to save a samp...

Page 285: ...ted data window and select points for the f Ratio report Cause For some reason the list of available models was corrupted therefore the model selected could not be loaded for the deconvolution Action...

Page 286: ...moved Action Reinstall the software Cause The Isotherm report for the named overlay file has Per gram selected for the Volume Adsorbed and the Isotherm report for the primary file has a surface area o...

Page 287: ...The sample file in the Heat of Adsorption report is corrupt Action Go to Report Heat of Adsorption Select the correct sample file then click Remove Sample Rerun the Heat of Adsorption report Cause The...

Page 288: ...etup program Stop and re start the application Contact a Micromeritics service representative if this error message continues Cause An error occurred accessing the control information disk file requir...

Page 289: ...ction Edit the Po options in the analysis conditions and select Entered or Most recent measured as the saturation pressure method Cause The Dewar does not contain enough cryogen to take an accurate re...

Page 290: ...the calibration file Action Select Unit Calibration Load from File and select a file containing calibration data Contact a Micromeritics service representative if this error message continues Cause Th...

Page 291: ...or setting does not exceed 15 to 18 psi 103 4 to 124 1 kPa Contact a Micromeritics service representative if this error message continues Cause B An error occurred in the pressure measurement electron...

Page 292: ...et valve on the gas bottle is open and that the gas pressure regulator setting is between 15 and 18 psig 103 4 and 124 1 kPa Check the adsorbate gas bottle to see if it is empty replace if necessary C...

Page 293: ...red Action Contact a Micromeritics service representative if this error message continues Cause A power failure occurred during an automatic operation The operation was cancelled Action Restart the op...

Page 294: ...Appendix B Gemini VII B 28 239 42828 01 Nov 2013...

Page 295: ...intervals in the Po tube and several data points were collected in the interval For points taken before the previous Po measurement For points taken after the previous Po use the previous Po PoI Po1 I...

Page 296: ...ing helium onto sample mmHg P2 system manifold pressure after dosing helium onto sample mmHg P3 sample pressure after raising Dewar and equilibrating with helium mmHg TSTD standard temperature 273 15...

Page 297: ...gas capacity of the volume occupied by the sample from the measured free space of the empty tube where VFW calculated warm free space VFC calculated cold free space VWB warm free space of the empty t...

Page 298: ...s below are those used to compute weighted average and first derivative respectively for the 6th point of an 11 point window where the numerical constants are from the Savitzky Golay convolution array...

Page 299: ...PC P is greater than or equal to 0 99 where P equilibrated collected pressure measured by gauge at temp TRM mmHg SD inside diameter of sample tube mm from the Report Options dialog MD thermal transpir...

Page 300: ...esignated pairs where PrelI is the independent vari able and BI is the dependent variable The following are calculated a Slope S g cm3 STP b Y intercept YINT g cm3 STP c Error of the slope SERR g cm3...

Page 301: ...pendent vari able and LI is the dependent variable The following are calculated a Slope S g cm3 STP b Y intercept YINT g cm3 STP c Error of the slope SERR g cm3 STP d Error of the y intercept YIERR g...

Page 302: ...r 2 HJP3 Harkins and Jura parameter 3 STSA1 statistical thickness surface area parameter 1 STSA2 statistical thickness surface area parameter 2 STSA3 statistical thickness surface area parameter 3 Pre...

Page 303: ...rface area correction factor user entered on the t Plot Report Options dialog D density conversion factor user entered on the Adsorptive Properties dialog Micropore Surface Area m2 g where SATOT is th...

Page 304: ...the core of the pore at a particular relative pressure related to the core radius by the Kelvin7 equation After the core has evaporated a layer of adsorbate remains on the wall of the pore The thickne...

Page 305: ...lative pressure Pr1 is assumed to be close to unity so that substantially all the pores in the sam ple are filled The corresponding Kelvin core radius is calculated Only pores smaller than this size w...

Page 306: ...n the increment of volume desorbed during that interval The variable I refers to the interval number that is I 1 for the first interval from Pr1 to Pr2 and so on J refers to each previous interval dur...

Page 307: ...nterval is calculated Since no cores are evaporated in this pressure interval no new pores are revealed Thus no ending Kelvin radius and average pore diameter are calculated for this inter val Note th...

Page 308: ...ure corresponding to DavgK is calculated as follows The thickness of the adsorbed layer at this pressure is calculated as follows The decrease in thickness of the wall layer by desorption from the wal...

Page 309: ...calculations have been performed the diameters corresponding to the ends of the intervals are calculated as follows for all RcJ including RcK 1 The remaining calculations are based on DP I Davg I and...

Page 310: ...s if selected the following calculations are performed 1 Average Fixed Pore Size DFavgJ A calculated for all intervals in the fixed pore size table For the intervals with between the Minimum BJH diame...

Page 311: ...DpFI cm3 g A where INTERP x is the value interpolated from the function X DavgJ and Y dV dDJ 7 dV dlog D pore volume dV dlog DpF I cm3 g where INTERP x is the value interpolated from the function X Da...

Page 312: ...layer desorbed during interval A Tw thickness of remaining adsorbed wall A HP1 HP2 and HP3 are Halsey Parameters from the Halsey Thickness Equation dialog HJ1 HJ2 and HJ3 are Harkins and Jura Paramet...

Page 313: ...cm 4 4 L 2 d0 4 3 L d0 3 10 9 L d0 9 4 3 d0 3 10 9 d0 9 When you use the original Horvath Kawazoe9 method the following equation is solved for each value of P The value of L is determined when the sol...

Page 314: ...ion is solved for each value of P The value of L is determined when the solved for relative pressure is within 0 1 of the collected absolute pressure where K Avogadro s number 6 023 x 1023 R gas const...

Page 315: ...8 31441 x 107 ergs mole K T analysis bath temperature K from an entered or calculated value on the Po and Temperature Options dialog d0 where DA molecular diameter from the Horvath Kawazoe Physical P...

Page 316: ...e different geometrics where G L one of the Horvath Kawazoe equations given above degree of void filling is estimated by first computing the monolayer capacity Vm with the Langmuir equation over the r...

Page 317: ...ectron 0 8183 x 10 6 erg S polarizability of sample atoms cm3 A polarizability of gas molecule cm3 S diamagnetic susceptibility of sample atom cm3 A diamagnetic susceptibility of gas molecule cm3 wher...

Page 318: ...P on the Adsorptive Properties dialog dV dD Pore Volume cm3 g Median Pore Width VHALF VCUMN 2 DMED 10 DL log VHALF VL log log DG DL log log VG VL log log where VCUMN total cumulative pore volume VCUMI...

Page 319: ...arbon Ross Olivier value Carbon Horvath Kawazoe value Zeolite 4 20 9 20 5 08 273 15 Carbon Ross Olivier value Carbon Horvath Kawazoe value Zeolite 4 34 9 35 5 22 194 65 Carbon Ross Olivier value Carbo...

Page 320: ...phite Zeolite DS 3 40 DS 3 04 NS 3 845 x 1015 NS 3 75 x 1015 S 1 05 x 10 29 Ross Olivier S 1 94 x 10 29 13 5 x 10 29 Horvath Kawazoe implicit S 0 85 x 10 24 S 1 02 x 10 24 Nitrogen Argon DA 3 00 DA 2...

Page 321: ...dialog For each point designated for Dubinin Radushkevich calculations the following calculations are done LV log V LP Po P 2 log The intercept log Vo can be found by performing a least squares fit o...

Page 322: ...28 01 Dec 2012 Error of Monolayer Capacity cm3 g STP VoERR Vo x 10YIERR 1 0 SDP Vo 6 023 10 23 22414 cm 3 10 18 nm 2 m 2 Micropore surface area m2 g where molecular cross sectional area of gas nm2 fro...

Page 323: ...point designated for Dubinin Astakhov calculations the following calculations are done LV log V LP Po P log N A least squares fit is performed on the LP LV designated pairs where LP is the independent...

Page 324: ...ptive proper ties dialog Limiting Micropore Volume cm3 g W0 V0 x D where D density conversion factor cm3 liquid cm3 STP from the Adsorptive Proper ties dialog Error of Limiting Micropore Volume cm3 g...

Page 325: ...Equivalent Pore Width Micropore surface area m2 g is calculated by a polynomial approximation over the domain 0 x 1 as follows x 1 1 b1x b2x2 b3x3 b4x4 b5x5 b6x6 b7x7 b8x8 x x 3 x 10 7 x 1 3N 1 3N wh...

Page 326: ...nm 3 A 3 E 0 N W i W0 ln ln 1 3N Appendix C Gemini VII C 32 239 42828 01 Dec 2012 Equivalent Pore Diameter dV dD Pore Volume cm3 g dV dDi 0 5 W0 3N 10 3 nm 3 A 3 E 0 N Di 2 3N 1 10 3 nm 3 A 3 E 0 N Di...

Page 327: ...With the tI VI data pairs the Akima semi spline interpolation method is used to interpolate quantity adsorbed values based on thickness values that are evenly spaced 0 2 Angstrom apart starting at th...

Page 328: ...urface area occluded for the Ith point m2 g SINCI SI 1 SI Cumulative pore surface area occluded for the Ith point m2 g SCUMI SINCI SINCI 1 SINC1 dA dR pore surface area for the Ith point m2 g dA dRI S...

Page 329: ...m 1 In terms of quantity adsorbed Taking the log of both sides yields Temkin Isotherm Q Qm RT q0 A0P ln Q RTQS q0 A0 P Po ln ln The Temkin isotherm has the form where Q quantity of gas adsorbed Qm qu...

Page 330: ...ore the convolution of an adsorption process with the distribution of one or more properties which affect that process This was first stated mathematically by Ross and Olivier12 for the case of surfac...

Page 331: ...at the same pressure p on an ideal free surface of energy e and the total area of surface of energy e in the sample The exact form of the energy dependent term depends on the form of the model isothe...

Page 332: ...ort Options window as a selection of tables or graphs Regularization DFT allows a selectable regularization also referred to as smoothing constraint to be applied during the deconvolution process to a...

Page 333: ...ted by the usual Least Squares method Refer to BASIC Scientific Subroutines Vol II by F R Ruckdeschel Copyright 1981 BYTE Publications McGraw Hill p 16 If there is only a single point or all N points...

Page 334: ...eport a Single point Surface Area m2 g S1PT Va 1 Pr CSA 6 023 10 23 22414 cm 3 STP 10 18 nm 2 m 2 where Pr pressure closest to 0 3 of the relative pressure points designated for surface area calculati...

Page 335: ...ace Area See Dubinin Astakhov calculations n Dubinin Astakhov Micropore Volume See Dubinin Astakhov calculations o MP Method Cumulative Surface Area of Pores MPSTOT SCUMI see MP method Calculations fo...

Page 336: ...Barrett E P Joyner L S and Halenda P P J Am Chem Soc 73 373 380 1951 9 Horvath G and Kawazoe K J Chem Eng Japan 16 6 470 1983 10 Saito A and Foley H C AlChE Journal 37 3 429 1991 11 Cheng Linda S and...

Page 337: ...s appendix contains instructions for ensuring that the Ethernet connection operates properly Windows 7 1 Select the Windows icon from the Status bar at the bottom of the screen then select Control Pan...

Page 338: ...Appendix D Gemini VII D 2 239 42828 01 Dec 2012 3 Click Network and Sharing Center 4 Click the Local Area Connection for your analyzer...

Page 339: ...Gemini VII Appendix D 239 42828 01 Dec 2012 D 3 5 Click Properties 6 Highlight Internet Protocol Version 4 then click Properties...

Page 340: ...ollowing IP address then enter the following in the IP address field 192 168 77 100 8 The following numbers should display in the Subnet mask field 255 255 255 0 If not enter them Leave all other fiel...

Page 341: ...t the bottom of the screen then select Control Panel 2 Double click Network and Sharing Center 3 Click Manage network connection from the Tasks list on the left side of the window then click Local Are...

Page 342: ...4 then click Properties 6 Click Use the following IP address and enter the following in the IP address field 192 168 77 100 7 The following numbers should display in the Subnet mask field 255 255 255...

Page 343: ...ube has been developed It can reduce the size of the initial imbalance to low levels and allow precise measure ment of adsorbed gas This technique can be performed by the following methods Using glass...

Page 344: ...ute value and the following relationship determine the mass of glass beads to remove from or add to the balance tube to reduce the free space imbalance where 2 515 g cm3 density of glass beads 3 53 th...

Page 345: ...and balance tubes 2 Hold the balance tube horizontally and carefully slide the longer filler rod into the tube 3 Prepare your sample and place it into the sample tube insert the shorter filler rod int...

Page 346: ...and loading the amount of glass beads to use insert a filler rod into the balance tube 2 Insert a filler rod into the sample tube Ensure that the filler rods are equidistant from the top of each tube...

Page 347: ...nteraction of adsorbed molecules with each other Other theo ries such as the Dubinin Astakhov approach also include parameters for the effect of adsorbent porosity Instead of this classical kinetic or...

Page 348: ...his method takes into account both the forces acting between the gas particles themselves and those acting between the gas particles and the atoms of the simulated surface As the simulated particles c...

Page 349: ...fluid is a homogenous system of constant den sity its chemical potential1 is determined by the pressure of the system using well known equations The fluid near the walls is not of constant density it...

Page 350: ...ion iso therm for the model If the value of H is very large the isotherm obtained corresponds to that of an external or free surface If H is smaller a range of pressures is reached where two minima ex...

Page 351: ...ical pore filling pressure In inset c the profile shows the density decreasing to near zero actually the bulk gas density at 4 or 5 molecular diameters from the surface Inset d shows the profile conve...

Page 352: ...otherms for Some Larger Pore Widths Argon on Carbon at 87 3 K Figure D 4 shows model isotherms for pores in the micropore size range Note the logarithmic scale for pressure Figure D 4 Model Isotherms...

Page 353: ...00 relative pressure These models are identical to those supplied with the original DOS version of DFT software Some slight difference from the DOS results may be noted when they are applied to the sa...

Page 354: ...ed Clay Surface Montmorillionite Model isotherms were calculated using a combination of statistical thermodynamic Non Local Density Functional Theory NLDFT calculations and experimental isotherms for...

Page 355: ...ed Interlayered Clay PILC from a Hybrid Density Functional Theory DFT Method The Journal of Physical Chemistry B 2001 105 3 623 629 M L Occelli J P Olivier J A Perdigon Melon and A Auroux Surface Area...

Page 356: ...ions and a slit like pore geometry These models are slightly different from N2 DFT and Ar DFT models that were calculated using NLDFT with density independent weighting functions The reported pore siz...

Page 357: ...copy HRTEM and or X ray diffraction XRD to obtain comprehensive information about the structure of studied carbon material N2 Carbon Cylinder single wall nanotube by NLDFT Ar Argon Cylinder single wal...

Page 358: ...wall nanotubes The reported pore size range is from 3 5 to 1000 Ar Zeolites H Form by NLDFT Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting function...

Page 359: ...Hill de Boer equation and the Fowler Guggenheim equation All of these suffer from the fact that they only describe monolayer adsorption whereas the data may include contributions from multilayer forma...

Page 360: ...onal algorithm Kernel functions corresponding to various classical Kelvin based methods have been calculated for differing geometries and included in the list of models Models Included t 3 54 5 00 P P...

Page 361: ...rties used in the Kelvin equation are N2 Harkins and Jura Thickness Curve The calculation is the same as above except that cylindrical geometry is assumed Geometry Slit Substrate Average Category Poro...

Page 362: ...lindrical geometry is assumed and the film thick ness depends on pore size see reference Geometry Slit Substrate Average Category Porosity Method Nitrogen at 77 K Surface tension 8 88 dynes cm 1 Molar...

Page 363: ...ts on Solids Kazimierz Dolny Poland July 1992 2 Classification of Adsorption Behavior Simple Fluids in Pores of Slit shaped Geometry Perla B Balbuena and Keith E Gubbins Fluid Phase Equilibria 76 21 3...

Page 364: ...Appendix F Gemini VII F 18 239 42828 01 Dec 2012...

Page 365: ...emoving 4 20 turning on off 2 5 Analyzing file status 2 8 Ar Carbon Finite Pores As 12 2D NLDFT model F 11 Ar Carbon Finite Pores As 6 2D NLDFT model F 10 Ar Carbon Slit Pores by NLDFT model F 10 AR C...

Page 366: ...alling 3 22 precautions 3 22 DFT models F 1 See Models DFT report Pore Size options 5 46 Surface Energy F 13 Surface Energy options 5 49 Diagnostics gas line test 9 22 leak test 9 16 Differential free...

Page 367: ...requirements 1 7 1 9 toxic 9 19 Gemini Series 1 4 Glass beads using E 1 Graph copying as metafile 7 22 editing onscreen 7 19 grid lines 8 3 Graph overlay for multiple graphs 3 40 for multiple samples...

Page 368: ...9 Zeolites H Form by NLDFT F 12 Molecular dynamics F 2 Molecular simulation methods F 2 Monolayer capacity 5 27 Monte Carlo F 2 Montmorillionite F 8 Moving an analyzer to another computer 4 16 MP Met...

Page 369: ...5 30 Validation 5 56 zoom feature 7 23 Report options command 5 18 file 5 18 file creating 3 15 list file statistics 5 6 Report relative pressure table 5 25 Reports menu close reports command 7 3 con...

Page 370: ...ting the setup program 4 9 uninstalling the analysis program 4 31 using 2 6 Specifications 1 8 StarDriver files convert 3 34 Start Analysis command 6 2 Start Po measurement command 6 6 Start report co...

Page 371: ...the Vacuum Pump Exhaust Filter 2 13 Cleaning and Verifying Gas Lines 2 13 Cleaning Sample Tubes 2 12 Connecting Gases 2 13 Degassing the Sample 2 12 Determining Sample Mass 2 12 Evaluating data 2 12 G...

Page 372: ...Gemini VII Smart VacPrep Operator Manual Dec 2013 G 1 G Smart VacPrep Operator Manual...

Page 373: ...OPERATOR MANUAL Smart VacPrep Operator Manual Nov 2013 SMART VACPREP INTELLIGENT VACUUM SAMPLE PREPARATION SYSTEM...

Page 374: ...egistered trademark of Micromeritics Instrument Corporation _____________________________________________________________________________________ Micromeritics Instrument Corporation 2013 All rights r...

Page 375: ...e made subject to factory inspection of returned parts MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications are made by persons other than its...

Page 376: ...actures a special product to the purchaser s specifications MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its products other than the liabi...

Page 377: ...lyzer or components WARNING Warnings contain information to help prevent actions that may cause personal injury For Chemisorption Indicates the marked item is applicable to chemisorption analyzers onl...

Page 378: ...sis Conditions etc Keyboard Commands Keyboard commands are represented as bold font weight and black letters Some examples are F2 Alt F4 etc Menu Instructions Menu instructions are represented as bold...

Page 379: ...e 770 662 3636 Fax 770 662 3696 www Micromeritics com U S Inquiries U S Sales 770 662 3633 ussales micromeritics com Quotes Orders and Customer Satisfaction Customer Service 770 662 3636 orders microm...

Page 380: ...Contact Us vi Smart VacPrep Operator Manual...

Page 381: ...Smart VacPrep 3 1 Backfill the Smart VacPrep Ports 3 1 Evacuate the Smart VacPrep Ports 3 1 QuickStart Degas Conditions 3 2 Load QuickStart Degas Conditions into a Sample File 3 4 Start Smart VacPrep...

Page 382: ...6 1 Replace the Smart VacPrep Fuse 6 2 Sample Tube Installation on the Smart VacPrep 6 2 Oil Based Vacuum Pump 6 3 Inspect and Change Vacuum Pump Oil 6 3 Replace the Alumina in the Oil Vapor Trap 6 7...

Page 383: ...eters is available A record of the sample preparation time and temperature can be recorded as part of the sample data file The degas program may be started or terminated by using the analyzer software...

Page 384: ...hen be started either by pressing the Select and Start buttons on the Smart VacPrep unit or by going to Smart VacPrep Unit n Degas Start Degas A Check Seal or TransSeal can be used to transfer air sen...

Page 385: ...Width 53 cm 20 75 in Depth 44 cm 17 in Weight 32 kg 70 lbs Evacuation Period Determined by selected elapsed time or achievement of selected low pres sure target Evacuation Rate Selectable evacuation r...

Page 386: ...driver to gently pry open the cover of the compartment 2 Firmly press down on the voltage indicator and roll the indicator to display the appropriate voltage for your environment Selections are 100 Va...

Page 387: ...n IP address will be assigned to the unit allowing the unit to connect automatically during startup Up to three additional degasser units can be installed Menu options for the Smart VacPrep are provid...

Page 388: ...n prompted enter the serial number of the unit being added Duplicate serial numbers are not allowed 2 Click Add Initialization begins REMOVE A SMART VACPREP UNIT Smart VacPrep Remove 1 Select the seri...

Page 389: ...o display the Unit IP Setup window The IP address and Subnet mask assigned during installation display Do not edit these fields unless instructed by a Micromeritics service representative OK Saves and...

Page 390: ...2 About the Software 2 4 Smart VacPrep Operator Manual...

Page 391: ...ckfill pressure in the Backfill pressure field 2 Select the ports to be backfilled 3 Click Start to start the process or Cancel to stop the process EVACUATE THE SMART VACPREP PORTS Unit n Smart VacPre...

Page 392: ...lity to enter commonly used degas conditions for each Smart VacPrep port without the need for a sample information file Degassing can then be easily started using the front panel buttons on the Smart...

Page 393: ...ator Manual 4 Click Save Repeat these steps for each port to be configured If multiple ports will have the same degas conditions parameters click Edit on the port and use the Copy QuickStart Degas Con...

Page 394: ...tions from the Smart VacPrep Unit Use to copy the degas conditions settings from the selected Smart VacPrep unit and port Degas Conditions Use to browse for a DEG file that contains degas condition pa...

Page 395: ...will stop and hold the sample temperature approximately constant until the pressure falls below the Hold pressure This prevents damage to the sample struc ture due to steaming and or elutriation due...

Page 396: ...ort 5 Attach the heating mantle using the metal clip If a straight wall tube is used heating mantles with elastic cords are available Refer to the Parts and Accessories section of the analyzer oper at...

Page 397: ...dashboard numbers right click on the dashboard setting then click Reset Field or Button Description Days until roughing pump service is due Annual maintenance is recommended The number of days until...

Page 398: ...escriptions Table continued SHOW SMART VACPREP LOG Smart VacPrep Unit n Show Log Use to display a log of recent analyses calibrations or messages Field Description Add Log Entry Use to enter informati...

Page 399: ...eadsheet XLS a portable document format PDF or an ASCII text TXT file format Analyzer Log Fields and Buttons Table continued SHOW SMART VACPREP SCHEMATIC Unit n Show Instrument Schematic Use to displa...

Page 400: ...access the shortcut menu hover the mouse pointer over the component and right click Schematic Shortcut Icon Available Options Valve options l Close Closes the selected valve l Open Opens the selected...

Page 401: ...e vacuum valves are closed and the vacuum level on the selected ports is monitored l The Status window indicates that the degassing operation is being checked and displays the outgassing rate as it be...

Page 402: ...r Button Description Sample The name of the sample file Skip Skips the current degas operation Status Indicates the current status of the degas Smart VacPrep Status Fields and Buttons Table continued...

Page 403: ...lated Topics See Smart VacPrep Pressure Offset below See Smart VacPrep Servo Valve Calibration on the next page SMART VACPREP PRESSURE OFFSET Smart VacPrep Unit n Calibration Pressure Offset Use to pe...

Page 404: ...ed before starting this calibration procedure 1 Go to Smart VacPrep Unit n Calibration Servo Valve 2 Click Start The window closes when the calibration is complete Click Cancel to stop the cal ibratio...

Page 405: ...ime or periodic running of a sequence of diagnostic tests A separate list of tests is saved for each of the possible test frequencies Tests are categorized and flagged as requiring intervention or not...

Page 406: ...if the instrument is idle at any time during the entered time frame Test Frequency Select how often the test is to run unattended Test Sequence Provides the test file identification and estimated run...

Page 407: ...s not immediately visible go to Unit n Show Instrument Schematic Schematic Components Description 1 6 Sample port valves 7 8 9 Vacuum and backfill valves Heating mantle con trols Sets the ramp rate an...

Page 408: ...flat head screwdriver to gently pry the fuses out of the holder 3 Insert a new fuse into each holder then push the holders back into the slot until snug 4 Press the compartment cover shut Ensure it cl...

Page 409: ...t the heating mantle thermocouple plug into the thermocouple connector 7 Insert the heating mantle power plug into the power connector and twist the power plug to lock securely 8 After installing the...

Page 410: ...on the oil level window when the pump is running Oil in good condition is clean clear or light in color and transparent Change the oil if it has darkened Change or Add Oil Drain the oil while the pump...

Page 411: ...ain plug and drain the oil into the waste container 6 Replace the drain plug 7 Remove the drain plug from the oil fill port on top of the pump 8 Slowly add oil to the port until the level is midway be...

Page 412: ...no longer white replace the alumina before reattaching the vacuum pump See Replace the Alu mina in the Oil Vapor Trap on the facing page 10 Reconnect the vacuum pump hose 11 Reconnect the power cord t...

Page 413: ...lumina pellets are no longer white Do not perform the following procedure on used alumina The resultant oil vapors may cause a fire 1 Disconnect the vacuum pump from the analyzer and place it on a wor...

Page 414: ...y Under normal circumstances these cracks will not cause problems or leaks Prepare fresh alumina 1 Preheat the oven to 300 C 2 Pour approximately 180 grams of fresh alumina into a glass or metal conta...

Page 415: ...of the trap body 9 Screw the other end fitting back onto the trap and tighten securely by hand 10 Lightly tap both ends of the trap body on the work surface to remove remaining dust from the pel lets...

Page 416: ...amp and place it around the flange of the intake port and the flange of the trap Swing the clamp fastening screw toward the intake port until it fits into the slot in the other half of the clamp Tight...

Page 417: ...usted by the oil filled vacuum pump The filter minimizes the release of oil vapor and should be replaced when it becomes so saturated with oil that it is ineffective Exhaust filters are used to minimi...

Page 418: ...it around the exhaust port flange and the exhaust filter flange Swing the clamp fastening screw toward the exhaust port until it fits into the slot in the other half of the clamp Tighten the wing nut...

Page 419: ...URO BUNA N for use with sample port dust frit 004 27041 00 Sample port dust frit 20 microns 067 33601 00 Operating supplies sample tube o rings 1 2 in and 12 mm sample port dust frit o rings for sampl...

Page 420: ...d alumina 500 grams for oil vapor trap 004 25491 02 Centering ring NW 40 BUNA N AL for use with hybrid turbo vacuum pump 004 25509 00 Clamp NW 10 16 004 25626 08 Flex tube 3 4 in OD x 48 in long NW 16...

Page 421: ...ng it to the preferred unit 4409 A free IP address on the same subnet as s could not be found Cause All IP addresses on the network for the Ethernet card specified during installation are in use by ot...

Page 422: ...ouple is unplugged or has malfunctioned Action Ensure the thermocouple is plugged in If the problem persists contact your Micro meritics service representative 4420 Communications error Cause The appl...

Page 423: ...pen by this or another application Cause The selected sample file is damaged Action Select another sample file 4425 The sample s on port d has an invalid status and cannot be used for degassing Cause...

Page 424: ...8 Error Messages 8 4 Smart VacPrep Operator Manual...

Page 425: ...B Backfill port Smart VacPrep 3 1 C Calibration Smart VacPrep 4 1 Smart VacPrep pressure offset 4 1 Smart VacPrep servo valve 4 2 Configuration Smart VacPrep 2 3 Contact Us v D Dashboard Smart VacPrep...

Page 426: ...unit 2 1 schedule diagnostic tests 5 1 schematic 3 9 show dashboard 3 7 show status 3 11 software about 2 1 specifications 1 3 start degas 3 5 troubleshooting and maintenance 6 1 use 3 1 Soak time de...

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