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CL400 ChemiLume User Manual

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1. 2 SWITCH f N ronen A CL400 5 CHEMILUME TEST RUNNING WHEN LIT DRAWER LOCKED OXYGEN FLOWING WHEN LIT j NITROGEN FLOWING WHEN LIT M moe CELL DRAWER pepe 2 Exp Suse iex pe AN C Ji c amp 2 Iu Iu POWER CORD SOCKET I EL 02 4 20 FUSE HOLDER 120V INPUT LINE FUSES 220 240Vac 250V T1 5A Oy Np gt OUT Ho90C9 OUT 115 120Vac 250V T2 8A 100Vac 250V T3 0A 7 L 9 PIN MALE SERIAL PORT pur ae uw wm TEST CELL TEMP CALIBRATION PORT GAS OUTLETS OVERHEAD VIEW CELL COVER WITH GLASS LENS SPECIMEN SOLID P SPECIMEN HOLDER STAINLESS STEEL OR ALUMINUM N v NET y C SIDE VIEW Figure 4 CLA00 ChemiLume Component Descriptions 2 5 SYSTEM CONNECTIONS cont 2 5 3 Chiller Leak Check 1 Grasp the lower portion of the filter housing on the water chiller Fig 3 and unscrew it by turning it counter clockwise If the filter is not present place it into the lower housing Make sure the large O ring is present on the housing Firmly screw the housin
2. Enter some post test comments maximum duration was selected you may stop the test with this method when intensity data has declined to a specific minimum 2 When a test completes the Test Screen 5 17 Test Complete Post test Comments Complete dialog box Screen 5 17 will appear If the test ended abnormally this box will provide a status message indicating the cause Type in any relevant information about the test process and then click on the OK button to save the comments NOTE The final test conditions shown in the Setup Monitor and Analyze views will remain until you click on the Setup Test button This clears the views and allows you to configure and run another test in that cell while other cells may still be under test You may wish to print a report or graph of test results as described below before clearing the views You may also print test results at a later date by opening an archived data file as described in Section 5 6 5 4 PERFORMING TEST cont 5 4 7 Printing Results amp Cell Reloading 1 You may print a test report and or Iesisl timeline graph before clearing the Setup and Analyze screens To do so click on the Report or Graph print button at the top of the screen or select Print from the File menu Include these reports Calibration report 2 In the Printing Options menu Screen 5 18 click on the name of the item s you wish to print Test and or
3. Pre test Phase Test Phase Constant Temp is rising to Dwell at setpoint Temperature setpoint temperature Test Ramped Temp is rising to Controlled temp Temperature controlled ramp ramping period Test starting setpoint Figure 9 Constant Temperature Test Profile In a constant temperature test cell temperature rises at maximum ramp rate to a setpoint you choose and then remains there for the duration you specify under Test Phase Duration After the test phase cell temperature declines to ambient conditions at an uncontrolled rate In a ramped temperature test cell temperature rises at maximum ramp rate to the Starting temperature ramps at the specified rate up to the Ending temperature and then cools to ambient conditions at an uncontrolled rate 5 Select the temperature profile desired by clicking in the white dot beside either the Constant or Ramped descriptor until the black dot appears indicating your selection Screen 5 2 If you select Constant you must specify Test Phase Duration as discussed below Test duration cannot be set for a ramped temperature test since it is determined by the selections made for Starting and Ending Temperatures and Ramp Rate Note When values are inserted to define a Ramped test the software shows a Projected Test Phase Duration The test will not stop after that time period The test stops after the Ending temperature is reached or it stops on error if the Ending temperature is
4. Cell conditioning is performed CL400 System Configuration at the beginning of each test Communications Advanced Test Seting Intensity Standard l Temperature Calibration Probe Cell Conditioning before specimens are placed ume m in the holders to clean the Condition cell when testing above V Enabled Condition cell when testing above specimen holders of any ZH Duration at temperature Duration at temperature contaminants that could emit light and alter test results The EN E us date empty holders are heated at afc an elevated temperature at c2 ES least 50 above the peak V Enabled cel when testing above V Enabled Condition cell when testing above test temperature for a 1 Duration at temperature Duration at temperature duration of at least 60 Fo 5 minutes This applies to tests nee MON pei that have a peak temperature ize fo ae of at least 200 C For tests at lower peak temperatures non residual solvent such as specimen holders and cell lens cover is acceptable Note for Initial Software Configuration Skip the steps below if you are performing the software configuration for the first time The following procedures are normally performed during test setup after you are aware of the test conditions required in each test cell The test setup procedure will refer you back to this section 3 5 CELL CO
5. Material Polypropylene 2 001 Intensity Elapsed time 0 33 10 Temperature 199 6 C Line adjustment handles 1079 Intensity mV 0 lt 0 00 00 0 05 00 0 10 00 0 15 00 0 20 00 Elapsed Time h m s High Time h m s 0 32 30 0 25 00 Low Time h m s 0 00 00 Integrated Intensity 5174 zoom in 0 30 00 Timeline OIT Integral Time to Failure Automatic Points Define Custom Points Logging File cell Screen 5 28 Integral Automatic Points Selection 5 Manual Point Selection Click on the Define Custom Points button and the definition lines will appear with adjustment handles 5 5 ANALYZING TEST DATA cont 5 5 3 Integral Analysis cont 6 Adjust each line horizontally by moving the cursor onto a handle and holding the right mouse button down Drag the line as required and then release the mouse button Only the portion of the intensity curve between the definition lines will be integrated Note For a more detailed view of the curve when making manual point selections click on the zoom button move the cursor to a point just outside the area of interest hold the left mouse button down and drag a zoom box around the area Release the mouse button Cell 1 testing Polypropylene XJZ 001 setup M monitor analyze FK calibrate Material Polypropylene XJZ 001 Intensi
6. x setup ff monitor analyze F lt Alibrate Material Polypropylene XJZ OD Intensity 991mV Timeline Elapsed time 0 33 30 Temperature 199 7 C 1 Pt d OIT 8000 7000 Integral 5 5000 4000 e 5 3000 c 2000 1000 0 4 44 lt 0 00 00 0 10 00 0 20 00 0 30 00 04 00 0 50 00 1 00 00 Elapsed Time h m s m m gt gt Analyze lo h m s 0 11 30 Induction Period b Lowe Ipeak h m s 0 22 42 Oxidation Rate Constant a inverse hours Critical Degree of Conversion 0 50 Time to Failure h m s Tame nie Logging File cell1 txt Screen 5 30 Time to Failure Automatic Points Selection 3 To perform the analysis you must define beginning of intensity curve deviation from exotherm baseline peak value of intensity curve and the critical degree of conversion These values may be defined automatically or manually When the Automatic Points option is selected a default value of 0 50 is used for the critical degree of conversion but this default value may be altered to your preference before initiating the analysis 4 Automatic Point Selection Click on the Automatic Points button and two lines will appear Screen 5 30 indicating the automatically determined locations of and lsa on the intensity curve Go to Step 8 if you wish to conduct the analysis using the default critical degree of conversion value sh
7. Atlas Polymer Evaluation Products HE ILUME E R A Y Z USER S GUIDE FOR INSTALLATION AND OPERATION August 14 2000 Software Ver 1 00 Win 95 Doc Part No 14 2696 00 ATLAS Click the Home Em button on any page to return here 1 0 WARNINGS AND PRECAUTIONS 1 2 0 INSTRUMENT INSTALLATION 2 2 1 Uncrating 2 2 2 Selecting a Location 2 2 3 Facilities Requirements 3 2 4 System Requirements User Supplied 4 2 4 1 Computer Specifications 4 2 4 2 Water Chiller Specifications 4 2 5 System Connections 5 2 5 1 Gas Supply Connections 5 2 5 2 Water Chiller Connections 5 2 5 3 Chiller Leak Check 8 2 5 4 Electrical Connections Power 8 2 5 5 Computer Connections 9 2 6 System Startup 10 2 6 1 CL400 ChemiLume 10 2 6 2 Computer and Monitor 10 2 6 3 Chiller Temperature Adjustment Tuning 11 3 0 SOFTWARE SETUP 13 3 1 System Data 13 3 2 PMT Intensity Standard 14 3 3 Temperature Calibration Probe 15 3 4 Advanced Test Settings 16 3 5 Cell Conditioning Settings 17 3 6 Appearance Settings 19 3 7 Communications Settings 20 3 8 Saving the Configuration File 20 3 9 Opening a Configuration File 22 3 10 Autoloading a Configuration File 22 4 0 SOFTWARE OVERVIEW 24 4 1 Menu Commands 24 4 2 Screen Controls 25 4 3 Window Views 26 4 4 Special Menus 29 5 0 SOFTWARE INSTRUCTIONS 30 5 1 Adjusting Gas Supplies and Chiller 30 5 2 PMT Calibration Note 31 5 3 Test Definition 31 5 3 1 Cell Conditioning Phase 31 5 3 2 Procedure 31 5 3 2 1 Test
8. Cells 121 cell Material Polypropylene XJZ 001 Test Status Test complete halted by user 2 cell2 300 0 90007 Material Test Status Test complete test duration reached Polypropylene XJZ 001 9000 4500 2 Mr rp aanjesaduia M mv Miintensity mv 0 0 00 00 Elapsed Time h m s e 4 Cell3 Idle Screen 5 15 All Cells Timeline Graph View 5 4 PERFORMING TEST cont 5 4 5 Exporting Data cont 3 Data files may only be exported in ASCII EmmmETTETTETTEITTIT Tx text txt format Thus the Save as type s case gt e ez selection box may not be altered R2Bul2nt tst celld txt R29u33nt tst Dk1173nt tst 5 Dk1234nt tst 5 Dkf 3nt t t 4 Click in the edit box beside File name and type in the file name desired Click on the Save button to save the file 5 4 6 Test Completion amp Stopping a Test Filename ERE Save as type Chemilume test data 5154 Cancel 1 You may stop the test in a cell at any time by clicking on the Stop Test button in the Screen 5 16 Copy Data Dialog Box Setup or Monitor view of that cell The test data will be logged up to the time this occurs If during test setup you were unsure of the time duration required for your test and the Lew
9. Font Arial 10pt Analysis Report Click on the Page Layout button Screen 5 19 to include Screen 5 18 Printing Options Menu Report headers or footers on the printout Click on the Font button for fonts 3 Customize graph printouts by using the options of the Graph Print menu J Screen 5 20 If you performed one or T Cid wmo Right more analyses on the test data you Batom 050 21 may print it at this time by following it 5 3 D Xl these instructions To print the timeline cENE 17 t t alone disable all 3 analyses results in Fort the Graph Print Analysis menu Refer to Section 5 5 for instructions on Cancel performing analyses on the test data Screen 5 19 Report Printing Options Page Layout 4 In the Graph Printing Analysis screen Screen 5 20 select the analysis results you wish to print Click 9 Ireswelee As Past on the results names until a check mark appears beside it Include these results Format Show results as Key Placement foh sj 5 Graph printouts may include ci Ric analysis results text or graphical E format Selecting Text Only provides graph and results in text form Text and ppm Graphic provides a graph that has coded lines indicating results as they would appear on the Analysis screen eS as well as a text listing of results Selecting Detailed provides additional infor
10. 00 00 0 05 00 0 10 00 0 15 00 0 20 00 0 25 00 0 30 00 Elapsed Time h m s Baseline Slope D 018mVv s Baseline Intercept 82mVv Peak Slope TES Bo hms 01330 Automatic Points Peak Slope Intercept 13435mv Define Custom Points Logging File cell1 bxt Screen 5 27 OIT Analysis Results 8 Print the results by clicking on the Graph or Report print button at the top of the program screen or by selecting Graph or Report print from the File menu Follow the instructions of Section 5 4 7 for configuring the printing options 9 To perform another OIT analysis of the curve repeat the procedure above beginning with Step 3 5 5 ANALYZING TEST DATA cont 5 5 3 Integral Analysis This analysis may be performed constant isothermal and ramped temperature test data 1 Open a data file as described in Section 5 5 1 above or continue with the currently open data file 2 Click on the Integral button 3 To perform the analysis you must first define the limits of the intensity curve to be integrated These two points may be defined automatically or manually 4 Automatic Point Selection Click on the Automatic Points button and two vertical lines will appear on the graph Screen 5 28 indicating that the entire intensity curve will be integrated Go to Step 7 if full curve integration is desired cell 1 testing Polypropylene XJZ 001 Fal setup monitor analyze FK calibrate
11. Description 32 5 3 2 2 Temperature Profile 33 5 3 2 3 Deviation Alarm 34 5 3 2 4 Test Phase Duration 35 5 3 2 5 Gas Types 35 5 3 2 6 Data Logging 35 5 3 2 7 Saving and Loading the Test Setup 47 5 4 Performing a Test 38 5 4 1 Cell Conditioning and PMT Gain Settings 38 5 4 2 Cell Conditioning Phase 38 5 4 3 Specimen Preparation and Loading 39 5 4 4 Test Monitoring 40 5 4 5 Exporting Data 42 5 4 6 Test Completion and Stopping a Test 43 5 4 7 Printing Results and Cell Reloading 44 5 5 Analyzing Test Data 47 5 5 1 Opening a Data File 48 5 5 2 Oxidation Induction Time OIT Analysis 48 5 5 3 Integral Analysis 51 5 5 4 Time to Failure Analysis 53 5 5 5 Activation Energy Analysis 55 5 6 Archived Files 57 5 6 1 Viewing the Test Details 58 5 6 2 Saving an Archived Test Setup 59 6 0 CALIBRATION PROCEDURES 60 6 1 PMT Intensity Calibration 60 6 2 Cell Temperature Calibration 63 6 3 Gas Flow Verification 67 7 0 MAINTENANCE PROCEDURES 68 7 1 Computer Maintenance 68 7 2 CL400 Maintenance 68 7 3 Water Chiller Maintenance 69 APPENDIX A PROGRAM ERROR MESSAGES 72 List of Figures 1 Dimensions and Clearance Requirements 2 2 CL400 Plumbing Ports b 3 Optional Water Chiller and Service Connections 6 4 1400 ChemiLume Component Descriptions 7 5 Chiller Temperature Controller 8 6 Computer Ports 9 7 Program Icon 10 8 Chiller Controller Display 12 9 Constant Temperature Test Profile 33 10 Ramped Temperature Test Profile 33 11 Intensity Standard
12. Screen 6 1 will appear Click on the Calibrate gt PMT button and the calibration screen Ml Ae Screen 6 2 will appear The dark current tests will vom y ll begin immediately an internal shutter prevents the PMT mE from responding to the intensity standard during the dark IR current test Allow a few minutes for completion OVERHEAD VIEW 5 The low gain test will run automatically Figure 11 Intensity Standard Setup 6 1 PMT INTENSITY CALIBRATION cont setup M monitor li analyze calibrate m Calibration Report Next Step Calibrate Temper Intensity Standard Data Standard ID EMIT Std 0000 osition the intensity standard with filter n the cell and close the cell door Cancel Intensity values adjusted for decay ress continue when ready Clear Report Without Filter 5607 mY With Filter 2338 Measurements Taken During this Procedure 3 Continue With Filter Without Filter mv Status PMT calibration in progress m New PMT Calibration Values High gain factor Current intensity mV Low gain factor Screen 6 2 PMT Calibration View 6 The screen prompt will ask you to remove the filter Alter the setup in the cell drawer to meet this request Close the drawer and click on the OK button 7 When the test is complete results are shown in the Calibration Report
13. be edited in this view Functions Test Setup of Data File View or Save Setup to new name View Test Details O Archived File Bintxt archive file SETUP setup V analyze View Test Details Test History Number of Data Points 442 Logged Time h m s 0 39 00 View Test Setup View Test Details Cell Conditioning Disabled Final Status Test complete halted by user Post Test None Save Setup Comments r Temperature Calibration Date 10 9 1996 Low offset 0 0 C at 50 0 C High offset 0 0 at 250 0 C This view shows the historic Test Date ananas information of an archived data file mm E Calibration Settings at the Time of This Test Parameters Gas Flow Verification Data Points Collected Date 10 14 1996 A s Low nitrogen flow Passe Elapsed Time of Logging File High Low oxygen flow Passed Date Test Performed High oxygen flow Passed PMT Calibration Final Test Status UR Original Post test Comments Low gain Archived File B1nt txt FA setup analyze Timeline Material Oil B1 w Additives Contaminated Integral Test Status Test complete halted by user Time to Failure 2000 1800 1600 1400 1200 1000 800 600 gt Intensity mV 0 06 00 0 16 00 0 20 00 0 30 00 Elapsed Time h m s Date 10 9 1996 Standard used Std 0001 Low gain factor 1 00 arc
14. by these instructions may impair the protection provided by the safety devices TOXIC FUME HAZARD While each test cell in the instrument can accommodate only a very small amount of sample material some polymer ink or oil specimens may release toxic gas when heated to elevated temperatures When locating the CL400 in a laboratory this should be taken into consideration with respect to adequate ventilation or the implementation of a fume hood for repetitive testing of potentially toxic materials N WARNING This symbol indicates that there are special instructions or precautions in the user s manual regarding use of the instrument component to which the label is attached BURN HAZARD Hot Surface gt This symbol indicates that burn hazard exists when using the instrument component to which the label is affixed The operator must take proper precautions such as protective clothing and be aware of the proper procedures marked by this symbol in the user s manual for avoiding injury when using this part of the instrument RADIOACTIVITY HAZARD The intensity standard used for calibration of the CL400 photomultiplier tubes light sensors is a radioactive emission source While its output is extremely low 7 9 it must be handled stored and disposed of according to applicable local safety standards and regulatory policies Special instructions in the manual are marked by this symbol EMERGENCY POWER DISCONNECT In the
15. event of an emergency all power to the CL400 be disconnected by unplugging the power cord from the back panel socket The socket has been located near the top of the back panel for this purpose Be sure to situate the CL400 according to the space requirements in Figure 1 to facilitate this procedure This section describes how to and set up your system hardware and what facilities are required for proper operation 2 1 UNCRATING The components of the CL400 ChemiLume are usually shipped in separate crates Prior to accepting the shipment carefully inspect the crates for signs of mishandling Should hidden damage found immediately notify the carrier Notify Atlas regarding the nature and extent of the damage so that the most appropriate corrective action can be determined Save all packing materials until the instrument is installed and operating properly 2 2 SELECTING A LOCATION Place the CL400 on a sturdy lab bench or other suitable table Instrument space requirement is shown in Fig 1 The location must be convenient to electrical 20 cm 8 in and gas supplies Locate the computer beside the CL400 to facilitate operator access Serial cable length should exceed 7 6m 25 feet Locate the chiller unit near the CL400 on or ben
16. menu at the upper left and select System Configuration 2 Click on the System menu tab to bring up the System menu Screen 3 1 3 Click on the Open button and the Open cmo 1 e ex a File dialog box Screen 3 9 will appear 4 Double click on the file you wish to load or click in the edit box beside File name type in the file name and click on Open 5 The default cfg file will be closed and the EM new file will be opened with its settings NOW Fiesctype System Fiese z defining the software configuration 6 Continue with your testing or analysis pF Open File Dialog BOX procedures 3 10 AUTOLOADING A CONFIGURATION FILE The CL400 program icon can be set up to automatically load a specific configuration file rather than default cfg whenever the icon is used to start the program Follow the procedure below if you want to enable this feature 1 Start the system computer 2 Move the mouse cursor onto the CL400 ChemiLume program icon Press the right mouse button and the icon menu Screen 3 10 will appear 3 10 AUTOLOADING CONFIG FILE cont 3 Select Properties from the menu and the Properties menu Screen 3 11 will appear 4 Select the Shortcut menu by clicking on the Shortcut menu tab Click in the edit box beside Target and add the following text shown in bold face to the right of the program path and ral CL400 Pr
17. phase during which a new empty specimen holder in each cell is typically heated to the peak test temperature plus 50 C see Section 3 5 for instructions on setting the cell conditioning temperature This high temperature exposure will eliminate any contaminants that could emit light during the test and alter results After this the specimens are carefully loaded and the test initiated Note For tests with peak temperatures below 200 C cell conditioning may be disabled and the specimen holders solvent cleaned with a non residual solvent such as freon Refer to Section 3 5 5 3 2 Procedure 1 In the software program bring up the window for a cell in which you will conduct a test by clicking on the cell button bar or by clicking on the Window menu and selecting a cell 5 3 TEST DEFINITION cont 5 3 2 1 Test Description 2 Click on the Setup button at the top of the cell window The Setup view Screen 5 1 will appear 3 Fill in the information for this section by clicking in the white edit boxes and typing Each item appears on the test report setup M monitor B analyze FK calibrate Test Description Material description Polypropylene XJZ 001 Operator LDF Company Your Company Pre test comments Sample pellet from lot 2 Data logging 6 Every El Sampling rate sec reading Log during pre test phase Log temperature data Iv L
18. to bring up the Archived File Analyze view Screen 5 25 5 5 2 Oxidation Induction Time OIT Analysis This analysis may be performed only on constant temperature isothermal test data 1 Open a data file as described in Section 5 5 1 above 5 5 ANALYZING TEST DATA cont 5 5 2 Oxidation Induction Time OIT Analysis cont Line adjustment handles 2 Click on the OIT button E cell 1 testing Polypropylene 2 001 monitor FA setup analyze Material Polypropylene XJZ 001 Elapsed time 0 31 58 8000 7000 e000 5000 4000 3000 2000 1000 p mm 4 4 4 0 00 00 0 08 00 01000 0 15 00 0 20 00 Elapsed Time h m s Intensity mV 0 25 00 0 30 00 Baseline Slope 0 018 Baseline Intercept 82mV Peak Slope 16 693mV s Peak Slope Intercept 13435mV Timeline OIT Integral Time to Failure Analyze Define Custom Points Logging File cell1 tet Screen 5 26 OIT Automatic Points Selection 3 To perform the analysis you must first define the baseline and the maximum slope of the intensity cure These selections may be defined automatically manually 4 Automatic Point Selection Click on the Automatic Points button and two lines will appear on the graph Screen 5 26 Go to Step 7 5 Manual Point Selection Click on the Define Custom Points button and the definiti
19. window Screen 6 2 You are asked to accept the new values if they are within specification or to discard them if they are out of tolerance or any errors occurred Click on the appropriate button Accepting the new values will update only the currently loaded configuration cfg file see Sections 3 1 3 8 and 3 9 regarding configuration file use and loading 8 You may print a copy of the calibration report by selecting the Report print button at the top of the program window or by selecting Print Report the File menu The calibration report will stay open in this window until you select clear report or you start a new test or calibration procedure 9 Click on the OK button 10 Close the cell window by clicking on the Close X button at the upper right of the cell window Repeat steps 3 9 for each cell to be calibrated
20. you may observe the status of each cell in the Monitor view Screen 5 12 Click on the Monitor button Refer to Appendix A for a listing of warnings that may appear during the test l Cell 1 testing Polypropylene XJZ 001 setup M monitor analyze calibrate r Test State Temperature Intensity Gas flow Oxygen flow detected in system Gas type Oxygen high flow rate PMT coolant OK Door Closed locked Cell status Test in progress currently in test phase m Test Progress Pre test start 3 19 1997 1 44 34PM Test start 3 181 897 1 46 58PM Elapsed time from test start DO hours 0 minutes 23 seconds Temperature Holding isothermal setpoint 250 0 C 249 7 C 310 0 C 85mv 10000 auto scale i Stop Test Open Door Copy Logged Data Clear Warnings Bet Screen 5 12 Cell 1 Monitor View 5 4 PERFORMING A TEST cont 5 4 4 Test Monitoring cont 2 The SP arrow beside the Temperature bar graph indicates Setpoint If the Deviation Alarm is active there will be two horizontal lines extending from the SP arrow These indicate the limits of the alarm tolerance 3 During the test phase the Intensity bar graph is active Select auto scale beneath the graph and the range will be reduced from 10 000mV to a range that will provide a taller more responsiv
21. 2 19 1996 Std 0000 7 00 1 00 Gas Flow Verification Date Low nitrogen flow High nitrogen flow Low oxygen flow High oxygen flow 2 19 1996 Not tested Not tested Not tested Not tested r Dark Current Low gain High gain r Temperature Calibration Date Low offset High offset 2 19 1996 0 0 at 50 0 C 0 0 at 250 0 C Calibrate PMT Cancel Clear Report Screen 6 1 Cell Calibration View Main Perform this calibration for each cell that will be used to 845 conduct a test from one to all four as required LIQUID INTENSITY 77 1 Important Verify that the intensity standard STANDARD information has been recorded as described in Sec 3 2 7840 You will be prompted to do so by this procedure HOLDER gt 2 Remove the cell covers and specimen holders from ERST each cell to be calibrated Fig 4 Install the intensity l standard and its filter as shown in Fig 11 in the first cell to be calibrated Close all the cell drawers C 3 Bring up the window for the first cell to be calibrated by clicking on Cell X in the button bar or by clicking on the Window menu and selecting Cell X DRAWER SIDE VIEW 4 Click on the calibrate button and the main Calibration P screen
22. Curve E l m Time to Failure Analysis 0 00 00 0 05 00 0 10 00 0 15 00 0 20 00 0 25 00 0 30 00 Ese Re omn Activation Energy Determination Auto User Selectable Analysis Limits Logging File 1 54 instrument CALIBRATE EA setup monitor analyze calibrate Current Settings This view is used to perform the cell temperature calibration amp Calibration Gas Flow Verification Calibrate PMT the PMT light sensor EMEN Date 29 996 poene 9 Date 213125 Low nitrogen flow Not tested Clear Report calibration as well as to view Standard used 512 0000 doceo ET x Low gain factor 7 00 and print a summary of i igh oxygen flow ot teste calibration related settings Dark Current Temperature Calibration Parameters E Low gain up Calibrations History oem 00 at SOOO High offset 0 0 at 250 0 C Procedural Prompts for Operator Dark Current Values Display Printable Calibration Reports Accept Discard New Values View Print Cal Setting Summary 4 3 WINDOW VIEWS cont O Archived File Bint xt E setup V analyze 3 ates n E fi 5 ETE ERE e EE This view shows the test setup of an 5 archived data file The setup may be mm archive file SETUP View Setup saved under a new name but cannot
23. NDITIONING SETTINGS cont CAUTION Even with new specimen holders the only effective method for removing microscopic contaminants is by heating to elevated temperature DO NOT attempt to disable Cell Conditioning and resort to solvent cleaning methods for tests with peak temperatures above 200 C or test results will be unreliable and unrepeatable Procedures for Test Setup 1 Enable cell conditioning by clicking in the white box beside Enable until a check mark appears Cell conditioning is required for tests that have a peak temperature of 200 C or higher 2 Click the cursor in the white edit box beneath Condition cell when testing above Type in a value or increment it with the indexer arrows This should be set to the test temperature above which you wish cell conditioning to always take place The factory default is 200 C since solvent cleaning of the specimen holders is adequate for peak test temperatures up to this value It may be set lower than 200 C if desired 3 Set a Cell Conditioning Phase Duration for each test cell The normal setting is 60 minutes Click the mouse pointer in the edit box and type in a value or increment the reading by clicking on an indexer arrow button 4 Set a Conditioning Temperature for each cell This is the temperature to which the empty holder will be heated to clean it before the specimen is loaded It is standard practice to set the conditioning temperature for a cell to a value tha
24. NN z Width diagonalup Pattem printout use the Page Layout menu Screen 5 24 Click on the Font button to select fonts Screen 5 22 Graph Printing Options Pen Styles 10 Print the graph by clicking on OK at the bottom of the menu Titles Pen Styles Axes Layout Scales 11 You may also print test results at a ET NIAE LO later date by opening a test archive file eo Section 5 6 and then performing steps 1 creed T pd hrough 10 above as desired Continue below with cell unloading E Include temperature data Font 11pt Sideways axis titles Screen 5 23 Graph Printing Options Axes 5 4 PERFORMING TEST cont 5 4 7 Printing Results amp Cell Reloading cont CAUTION Burn hazard Avoid Titles Pen Styles Axes Analysis Page Layout contact with the drawer surfaces marked by this symbol Do not open the cell drawer or unload used spec imens until the cell has cooled to 50 or lower The cell is above safe handling temperature and the drawer remains locked when the following indicators are present e Monitor View cell status window Screen 5 24 Graph Printing Options Page Layout indicates Waiting for cell to cool e Setpoint S P arrow is still visible in Monitor View Cell status indicator at lower right of program screen is purple The indicator tur
25. TEST DEFINITION cont 5 3 2 6 Data Logging cont Every Point amp Sampling Rate This method will record light intensity data points at the WIN interval specified This is the most appropriate method PEN nf 3 for specimens that begin emitting light early in the test phase If this characteristic of the specimen is unknown Adaptive 20020 use this data logging method Log during pre test phase Log temperature data F Log status flags Sampling rate sec reading Adaptive amp Threshold Projected data file size 28 This method records data only if the intensity level changes by the amount specified in the Threshold mV Screen 5 6 setting box It is useful for specimens that begin emitting Data Logging Selections light later in the test phase and helps minimize file size 11 Select the data logging method by clicking in the white circle beside Every Point or Adaptive until a black dot appears indicating selection Screen 5 6 Set a value for Sampling Rate or Threshold by clicking in the appropriate edit box and typing in a value or increment it by clicking on an indexer arrow Observe the Maximum Data File Size indicated and adjust sampling rate or threshold to alter file size Sampling Rate Range 1 to 32 767 seconds reading Threshold Range 1 to 10 000 mV milliVolts Data logging options provide the following functions Log during pre test phase If selected data will b
26. am If the program gives an error message about the COM port connection make sure you have properly installed the serial cable between the computer serial port and the CL400 serial port 2 6 SYSTEM STARTUP cont 5 If an error message is still present click on the system button at the top of PMT Irtensiy Standard Temperature Caltbraton Probe Cel Condtioning System Appearance Communi ications Advanced Test Settings the screen and select the Communications menu Screen 2 1 6 Click on the appropriate Comm communications port button that matches the port to which you connected the CL400 serial cable at the back of the computer 7 Click on the Control menu at the top of the screen and select Initialize ChemiLume The controller initialization screen will appear momentarily Screen 2 1 Communications Menu indicating that communications have been properly established between the computer and the CL400 2 6 3 Chiller Temperature Adjustment Tuning It is of key importance that the chiller setpoint is adjusted to a value 3 to 5 above the dew point the temperature at which condensation will occur Setting it too low may cause water condensation on the PMT light sensing tubes inside the CL400 This can have an adverse effect upon light sensing accuracy and stability This is of greatest concern in laboratories with high humidity levels especially during the summer months The ch
27. and Filter Setup 61 12 Temperature Calibration Setup 64 List of Screens 2 1 Communications Menu 11 3 1 System Configuration Menu 13 3 2 PMT Intensity Standard Configuration Menu 15 3 3 Temperature Calibration Probe Configuration Menu 15 3 4 Advanced Test Settings Configuration Menu 16 3 5 Cell Conditioning Phase Settings 17 3 6 Appearance Settings Configuration Menu 19 3 7 Communications Configuration Menu 20 3 8 System Save As Dialog Box 21 3 9 System Open File Dialog Box 22 3 10 Program Icon Menu 22 3 11 Shortcut Editing Menu 23 5 1 Cell 1 Setup View 32 5 2 Temperature Profile Selections 33 5 3 Deviation Alarm Selection 34 5 4 Test Phase Duration 35 5 5 Gas Type Selections 35 5 6 Data Logging Selections 36 5 7 Data Logging Options 37 5 8 Setup Save As Dialog Box 37 5 9 Calibration Diagnostic Reminder 38 5 10 Test Data File Save As Dialog Box 39 5 11 Load Specimens Screen Prompt 39 5 12 Cell 1 Monitor View 40 It is the responsibility of the purchaser of this equipment to establish and implement safety and health procedures or regulations which will protect the operator from unnecessary risks or hazards Procedures for safe use of the supply gasses required by this instrument must be established in compliance with local safety codes and applicable regulatory agencies IMPAIRMENT OF SAFETY DEVICES This instrument is equipped with safety devices to protect the operator and the equipment Operation of the unit in any manner not prescribed
28. bration levels 6 1 PMT INTENSITY CALIBRATION Calibration involves placing the liquid intensity standard into a cell drawer and then initiating the test with the calibration start button You must subsequently install a filter during the procedure to alter the standard s emission level Text prompts on the calibration page guide you through the procedure outlined below Intensity Calibration Quick Reference 1 Standard in drawer with filter 2 Standard in drawer without filter 3 Accept or discard calibration results Print report The above procedure must be carried out for each of the 4 test cells and takes about 6 to 12 minutes per cell Procedure Important The CL400 cells must be at room temperature prior to beginning the PMT calibration CAUTION The intensity standard is a radioactive emission source and must be LN handled carefully to avoid breakage and contamination Its output is about 8 micro Curies an extremely low emission rate but it must be handled stored and disposed of according to local health and safety standards In the event of breakage avoid direct contact with the liquid Clean up and dispose of the contamination according to applicable hazardous waste regulations 6 1 PMT INTENSITY CALIBRATION cont Cell1 idle sd HB setup M monitor analyze K calibrate Current Settings m PMT Calibration Date Standard used Low gain factor High gain factor
29. e light intensity curve Time to Failure Points Integral Points Grid OIT OIT Baseline OIT Peak Slope vertical line on graph indicating start of test oxygen flow phase user adjustable endpoint lines that define analysis limits user adjustable endpoint lines that define analysis limits graduated grid overlay on graph line indicating Oxidation Induction Time result on graph user adjustable baseline indicator line for OIT analysis user adjustable slope indicator line for OIT analysis 3 6 APPEARANCE SETTINGS cont 3 Click in the white box beside Show grid on graph until a check mark appears if you want a grid overlaying the graphs for easier reading 4 Click in the white box beside Auto arrange cell windows until a check mark appears if you prefer to have only one program window open at a time and auto minimizing of all others that are open 3 7 COMMUNICATIONS SETTINGS This menu allows selection CL400 System Configuration of the serial communications PMT Intensity Standard Tene ea Conditioning port that the software ze ma Communications Advanced Test Satings uses to communicate with the CL400 Comm port selection 1 Click once on the Communications menu tab orm Screen 3 7 to bring up the menu 2 Click in the white circle beside the Com port desig nation to select the computer serial port to which the CL400 is connected A black dot ap
30. e System Configuration menu will close Saving Customized Configuration Files 1 Click on the system button at the top of the screen or click on the File menu at the upper left and select System Configuration 2 Perform the procedures detailed Sections 3 1 through 3 7 applicable to the Su es Ex 1 configuration options you wish to customize 3 Click on the System menu tab to bring up the System menu Screen 3 1 4 Click on the Save As button and the Save 6 The file just saved will become the currently loaded configuration file To create additional new configuration files open the DEFAULT CFG file in the System menu make alterations and then perform a Save As Screen 3 8 System Save As Dialog Box File name Configuration TomL As dialog box Screen 3 8 will appear z Save as type System Files cfg Cancel 5 Type in the desired file name ending with cfg and then click on the Save button 3 9 OPENING A CONFIGURATION FILE When the CL400 software program is started it automatically loads the DEFAULT CFG file and is configured with the settings of that file If you wish to load a different configuration file in which you have saved custom settings for graph colors advanced test settings etc as described in Sections 3 1 through 3 6 you must load it from the System menu Proceed as follows 1 Click on the system button at the top of the screen or click on the File
31. e critical degree of conversion by clicking in the Critical degree of conversion edit box and typing in a value or by incrementing the value by clicking on an indexer arrow Critical degree of conversion is defined as the amount of oxidation that will produce a detrimental effect in the material It is customer defined and based results from experimental data and factors related to the application of the material 5 5 ANALYZING TEST DATA cont 5 5 4 Time to Failure Analysis cont 8 Click on the Analyze button to perform the analysis The results are shown at the lower right of the view Screen 5 31 9 Print the results by clicking on the Graph or Report print button at the top of the program screen or by selecting Graph or Report print from the File menu Follow the instructions of Section 5 4 7 for configuring the printing options 10 To perform another analysis repeat from Step 3 5 5 5 Activation Energy Analysis ell 2 test complete FA setup monitor analyze calibrate Material Polypropylene XJZ 001 Timeline Test Status Test complete test duration reached Integral Wilntensity mv 22 y gt bb zoom out Elapsed Time h m s Analyze Analysis Start Time him s 0 01 04 Activation Energy 1 00 Automatic Eome Analysis End Time h m s 0 08 56 Actual Ramp Rate 5 0 C min Custom Eze zc nm cR Screen 5 32 Acti
32. e drawers 6 In the Setup view of each cell click on the Start Test button A calibration reminder will appear Screen 5 9 Click on O K Cancel Diagnostic Reminder 5 4 PERFORMING TEST cont 5 4 2 Cell Conditioning Phase cont Starting test enter name for logging file 7 dialog box for entering the data logging file name will appear Screen 5 10 Click in the edit box to the right of File and type in a suitable file name for the data logging file Do not add an extension It will be added automatically Click on the Save button and cell conditioning will begin Filename Save as type Chemiume test data tt H Cancel 8 cell conditioning requires about 2 hours to complete since the cells must be Screen 5 10 Test Data File Save As Dialog Box allowed to cool to at least 50 C before the specimens can be loaded At that time a screen prompt Screen 5 11 will advise you to load the specimens Observe cell temperature in the Monitor view Click on PE the Monitor button or select Monitor in the View menu 2 os teca dr 4 Press OK when ready to begin CAUTION Burn hazard Avoid contact with Lom cell drawer surfaces marked by this symbol Don t open the drawer until it has cooled to 50 Load specimens only after the cell has cooled or results may be invalidated Screen 5 11 Load Specimens Screen Prompt 5 4 3 Specimen Preparation and Loading T
33. e et p rov i d ed wi th yo ur System Communications l Advanced Test Settings i ntens i ly stan d ar d PMT Intensity Standard Temperature Calibration Probe Cell Conditioning edit box and type the appropriate value for each parameter specified in the menu You may also click on Liquid Scintillation Intensity Standard Values Intensity Values the arrow buttons to With Fiter increment the value in an edit Standard ID su Important Do not leave any ma T pm parameters blank each is CalbrationDste i zb 98 34 required for proper operation Be sure to fill in the month day and year These are critical for accurate Cancel determination of the intensity Screen 3 2 PMT Intensity Standard Configuration Menu standard s output over time since it declines decays at a very specific rate 3 3 TEMPERATURE CALIBRATION PROBE The optional temperature cal b rat on ki t nc u d es a System l Appearance Communications Advanced Test Settings ro b e an d m et er th at are Intensity Standard Temperature Calibration Probe Conditioning used to calibrate the cell temperature control system Th i S menu S creen 3 3 Temperature Calibration Probe Offsets i n cl u d es Act u al an d j cat e d Nominal Temperature C Actual Temperature C Indicated Temperature Temperatu
34. e indicator bar 4 While the test s is running there are specific options available for examining data as it is collected in the Analyze view Screen 5 13 and for exporting it to another application If you chose to Log Temperature Data in the test setup temperature data may be observed immediately in the timeline graph Click on the Analyze button in the cell window to observe the graph To observe and compare the graphs of all the active cells double click on the All Cells window icon at the bottom of the screen or click on the Window menu and select All Cells see Screen 5 17 next page Material Polypropylene XJZ 001 Intensity Elapsed time 0 31 33 8000 7000 6000 5000 gt L3 C e Intensity mV 2000 1000 0 Elapsed Time h m s Temperature 200 4 C 0 00 00 00500 01000 01500 0 20 00 02500 Logging File cell1 tx 22 eunje1ad Screen 5 13 Cell 1 Analyze View Timeline Graph 1 testing Polypropylene 2 001 M setup M monitor analyze F calibrate Timeline OIT Integral Time to Failure 5 4 4 Test Monitoring cont 5 4 PERFORMING A TEST cont 5 To zoom in on a portion of the graph click on the Zoom In button beneath the graph The cursor will change to indicate a zoom window Screen 5 14 6 Move the cursor onto the near the area to be enlarged Hold the left mouse button down and
35. e recorded during both the pre test and test phases This is useful in some cases for examining pre test temperature performance Selecting this option will increase data file size Log temperature data Normally only intensity data is recorded Selecting this option will cause cell temperature data to be recorded as well This is most useful for providing a full record of test conditions and for revealing the relationship of temperature to intensity in the timeline graph Temperature data is always logged for Ramped tests since it is required for the analysis of ramped test data 5 3 TEST DEFINITION cont 5 3 2 6 Data Logging cont Log status flags Status flags messages are recorded in the data file to mark the occurrence of events such as gas status and temperature out of tolerance warnings These are useful Screen 5 7 for analyzing the test data and observing the exact time Data Logging Options position of test events Log temperature data Log status flags Log during pre test phase If this option is selected an event will always be logged as it happens independently of sampling rate or intensity threshold logging options This increases data file size 12 Select the desired logging options described above by clicking in the white box beside the appropriate ones until a check mark appears Screen 5 7 5 3 2 7 Saving amp Loading the Test Setup At this point test definition for Cell 1 is comp
36. eath the bench Do not locate the CL400 in an area where stray electrical signals RFI EMI and vibrations might adversely affect computer operation If vibration is unavoidable install damping material of equal thickness beneath each foot of the table CAUTION CL400 weighs 39 kgs 85 Ibs The optional chiller weighs 74 kgs 163 Ibs Each should always be lifted by two individuals or one person using a hydraulic lift cart M M a 15 cm 6 in i S E d 53 om 24 in eH Figure 1 Dimensions and Clearance Requirements 2 3 FACILITIES REQUIREMENTS Environmental Requirements CL400 Only Operating Temperature 13 C 56 F to 30 C 86 F Humidity 25 75 Storage Temperature 10 C 50 F to 60 C 110 F Humidity 20 80 Altitude 2000 m 6560 ft Installation Category Pollution Degree II Refer to computer manual and chiller manual for their environmental specifications Electrical Requirements CL400 100Vac 50Hz 2 6 Amps max Refer to instrument label 115 120 60Hz 2 2 Amps max Refer to instrument label 200V 50Hz 1 3A Amps max Refer to instrument label 220 240 50Hz 1 1 Amps max Refer to instrument label 10 mains supply fluctuations Fusing Requirements 100Vac 250V T3 0A Slow Blow 115 120Vac 250V T2 8A Slow Blow 200 240Vac 250V T1 6A Slow Blow Chiller 100Vac 50Hz Fuse 250Vac 10A IEC 127 Type T Optio
37. en normal test running Yellow warning latching Red fatal error test stop Blue calibration in progress Purple cooling down White cell conditioning in 4 3 WINDOW VIEWS FA setup ff monitor la analyze r Test Description Material description Polypropylene XJZ 001 Operator LDF Company Your Company Pre test comments Sample pellet from lot 2 Data logging m Temperature profile Constant 200 0 E Set point C Ramped d Start Deviation F calibrate 4 alarm Start Test Save Setup Load Setup Ramn rate Cin Copy Logged Data Ending temperature 20 Tolerance C Every point 2 4 Sampling rate sec reading Gas Types Pre test phase Test Phase C Adaptive A Log during pre test phase Log temperature data Log status flags Projected data file size 31K Test Phase Duration 15 hrs 0 1 min 0 E sec Nitrogen high flow zl Oxygen high flow z MONITOR view This view displays test progress in text and graphical formats Parameters Instrument Status Event Progress elapsed time Temperature Bar Graph Temperature Setpoint Intensity Bar Graph Stop Test Copy Logged Data Clear Warnings Start New Test Cell 1 testing Polypropylene XJZ 001 test SETUP view This view is used to define test conditions and init
38. energy and actual temperature ramp rate based on formulae published in Luminescence Techniques Solid state Polymer Research L Zlatkevich Ed Marcel Dekker NY 1989 Some of the analyses may be performed from partial data before a test is complete such as OIT Time to Failure and Activation Energy Please follow the procedures below for performing analyses on complete saved data files While it is recommended that you perform these procedures after a test is complete they may be performed in the Analyze view while a test is running when adequate data has been recorded 5 5 ANALYZING TEST DATA cont 5 5 1 Opening a Data File To perform an analysis an archived data file must be opened first This is the initial step for each analysis 1 Click on the Open button at the top of the screen or click on the File menu and select Open and the Open File dialog box will appear 2 Double click on the name of the test data file you wish to open or type its name in the edit box beside File and then click on the Open button The Archived File Setup view will appear Archived File B1nt txt E setup analyze Timeline OIT Material Oil B1 w Additives Contaminated Integral Test Status Test complete halted by user Time to Failure Intensity mV zoom in Elapsed Time h m s Screen 5 25 Archived File Analyze View 3 Click on the Analyze view button
39. es in alarm the data logging file when the test temperature exceeds Screen 5 3 the tolerance setting of the alarm If the alarm is Deviation Alarm Selection triggered by a temperature deviation the Temperature heading in the Monitor view turns yellow and the associated Cell Status Indicator Section 4 2 turns yellow at the lower right in the program window In a constant temperature test the deviation alarm becomes active after the setpoint temperature is reached In a ramped temperature test the alarm is active only during the temperature ramping period i e after the start temperature is reached 8 If you desire alarm operation during the test click on the white box beside Deviation alarm until a check mark appears Set the tolerance by clicking in the white edit box and typing in a value or increment the value by clicking on an indexer arrow Range 0 1 to 10 5 3 TEST DEFINITION cont 5 3 2 4 Test Phase Duration This setting for constant temperature tests defines how long the test cell remains at the setpoint temperature 9 Set the Test Phase Duration by clicking in the white edit boxes for Minutes Hours and Seconds and typing in the desired values or increment the values by clicking on the indexer arrows Screen 5 4 Maximum 32 767 Hours 59 Minutes 59 Seconds Note If you are unsure of the duration required for the test leave the setting at the default maximum and then stop the test when yo
40. g back into place 2 Fill the chiller with tap water Fig 3 3 Plug the power cord into the chiller and into an appropriate AC power outlet 4 Start the chiller by setting its power switch to On 1 The water pump runs continuously 5 Check the water level in the reservoir and add more water until the chiller runs continuously 6 With the chiller operating examine connections for leaks Tighten or adjust those that are leaking 7 Adjust the chiller temperature setpoint as follows Press and hold the Set key at far left marked and press the up or down v arrow key until the setpoint is 18 C 65 F Release the Set key Shut off the chiller Additional instructions for fine tuning this setting are included in Section 2 6 System Startup 2 5 4 Electrical Connections Power Electrical power is supplied to the CL400 and the water chiller by standard plug in power cords Figs 3 and 4 Plug the respective cords into the equipment and an appropriately configured AC power outlet The components of this system include devices for extra protection from electrical shock The protective devices may not function properly unless the power cords are connected to properly grounded outlets e It is the user s responsibility to ensure that a proper ground connection is provided rs SET LOW WATER el POWER O JO Ns Figure 5 Chiller Temp Contro
41. he Target edit box Screen 3 10 for typing errors 4 1 MENU COMMANDS File PX Atlas ChemiLume CL400 Cell 2 idle IM Control View Window Help System Contiguration Open Pant Graph Print Report Software setup menus Open a test archive file Graph print menu amp options Test Analysis Exit terminate 2 print menu options program Control P Atlas ChemiLume CL400 Cell 2 idle Eile View Window maize GHemiltnie Test Gas Flow z ChemiLume controller initialization manual l O and N flow verification perform each time a supply tank is replaced or every 3 months m Atlas ChemiLume CL400 Cell 2 idle File Control View Window pen Sette Help On line View PL Atlas ChemiLume CL400 Cell 1 idle File Control view Window Help i cell 1 v Setup View alt S Analyze view Window view Calibrate View select Monitor view alt M Toolbar v Status Bar hal Program screen options Window PL Atlas ChemiLume CL400 Cell 1 idle File Control View window Help cell 1 Tile Window Arrange Icons arrangement v Auto Arrange options 1 Cell 4 idle 2 Cell 2 idle Test cell status amp 3 Cell 3 idle current window 4 Cell 4 idle selection 5 All Cells Lists open archived files CL400 I D and software version instructions select Ce
42. he amount of specimen material used for a test must be adequate to provide reliable emission levels yet small enough to prevent overloading of the PMT light sensor In most cases this must be determined by trial and error It is recommended that initial specimen weight should be in the 0 05 to 0 5 gram range and increased or decreased for subsequent tests based on initial results Attempts should be made to achieve intensity readings in the range of 5000 to 8000 mV at High PMT gain 9 Weigh and prepare your specimen materials Maintain the cleanest conditions possible during preparation to avoid the introduction of contaminants such as dust or skin oils that will alter test results Handle specimens only with clean instruments 5 4 PERFORMING A TEST cont 5 4 3 Specimen Preparation and Loading cont 10 Open a cell drawer Remove the cell cover Use clean tweezers to transfer specimen material from its container into the specimen holder Clean the cell lens cover with a non residual solvent and install it on the cell hand tight only Close the drawer Important Limit the cell open time to 2 minutes to minimize air exposure 11 Repeat step 10 for each active cell 12 Click the OK button of the screen prompt and the test will continue 13 During the pre test and test phases check the gas input pressure and adjust it to 6 9 kPa 1 PSI or 16 oz in if it is out of range 5 4 4 Test Monitoring 1 During the test
43. hive file ANALYZE Timeline View This view allows archived test data files to be analyzed Four different analyses may be performed Functions Timeline View of Test Data Oxidation Induction Time Analysis Intensity Curve Integration Analysis Time to Failure Analysis Activation Energy Analysis 4 4 SPECIAL MENUS ChemiLume Gas Flow Verification x Cell 1 Cell 2 Low Nitrogen Flow High Nitrogen Flow Testing 32 done Low Oxygen Flow High Oxygen Flow Cell 3 Low Nitrogen Flow High Nitrogen Flow Low Oxygen Flow High Oxygen Flow Progress Low Nitrogen Flow High Nitrogen Flow Low Oxygen Flow High Oxygen Flow r Cell 4 Low Nitragen Flow High Nitrogen Flow Low Oxygen Flow High Oxygen Flow Current action Testing high nitrogen flow cell 1 E Last Gas Flow Verification 10 22 1996 2 21 56PM Print Options Report Choices for report types to be printed are made in this screen Font face and size may be specified in Page Layout Reports Test test results Analysis 4 types Calibration PMT or temp Gas Flow Verification This screen is used to confirm gas flow and gas sensor operation see Section 6 3 It checks the four gas flow rates for each cell Functions O and N Supply Check Low and High Flow Rate Check Progress Indicator Pass Fail Notification Report Printing Options x Select Reports Layout Include these re
44. iate a test Parameters Test and Specimen Description Data Logging Options Temperature Profile Gas Selection and Flow Rate Test Duration Test Setup Save and Load Test Start Stop amp Setup EA setup M monitor analyze Test State Temperature Gas flow Gas type coolant Door Cell status Holding isothermal setpoint 250 0 C Oxygen flow detected in system Oxygen high flow rate OK Closed locked Test in progress currently in test phase ln calibrate Intensity 85 Temperature 249 7 C Open Door Copy Logged Data 310 0 C 10000mv pp Test Progress Pre test start 3 19 1997 1 44 34PM Test start 3 19 1997 1 46 58PM Elapsed time from test start 00 hours 00 minutes 23 seconds F auto scale 4 3 WINDOW VIEWS cont 1 testing Polypropylene XJZ 001 BEE ANALYZE setup monitor analyze FF calibrate test data This view provides real time graphing of test data and tools for performing Material Polypropylene XJZ D01 Intensity 1544mV Integral Elapsed time 0 31 33 Temperature 200 4 C analyses El 250 0 ime to Failure 7000 S 218 8 _ 5 2 2 1875 4 Functions 4 Ee M pu Graph Zoom amp Pan Ee Oxidation Induction Time Analysis 1000 31 3 3 Integration of Intensity
45. il an X appears if you would like the software program to provide an on screen reminder about performing required calibrations These include the PMT XE PMT and temperature calibrations It is recommended that the PMT calibration be performed daily to ensure accurate PMT intensity readings The temperature calibration is normally performed every 6 months The on screen reminder ensures that the operator is aware of these requirements at appropriate times Note for Initial Software Configuration Skip the steps below if you are performing the software configuration for the first time The following procedures are normally performed during test setup after you are aware of the test conditions required in each test cell The test setup procedure will refer you back to this section 3 4 ADVANCED TEST SETTINGS cont Procedures for Test Setup 1 Select a PMT Gain Setting for each test cell by clicking in the white dot to the left of the desired setting The normal gain selection is High Use Low gain only for materials known to exhibit high light emissions while oxidizing This setting prevents saturation of the PMT which results is test stoppage Note For specimens with unknown light emission levels you must perform an initial test with the PMT Gain set to Low If Intensity readings are too low or unstable perform a second test using the High gain setting 3 5 CELL CONDITIONING SETTINGS
46. iller setpoint should be adjusted to a value within the range of 16 C 60 F to 21 C 70 F Adjust it to an upper value of this range if condensation is noticed on the water lines or metal connection hardware Adjustment of the chiller temperature is a two step process As described previously the temperature setpoint is adjusted by holding the Set key and then pressing the up or down arrow key until the desired setpoint is indicated For the most precise temperature regulation the controller may additionally be tuned by conducting the procedure below Factory testing has proven that tuning of the chiller controller at 18 C 65 F with no load CL400 heaters off provides adequate temperature control at elevated test temperatures This section describes initial settings that must be performed in the CL400 ChemiLume software before tests may be conducted These include inputting of System Description 1 0 amp configuration file name PMT Intensity Standard specifications Temperature Calibration Probe specifications Advanced Test Settings PMT gain amp filter values Cell Conditioning Settings Threshold amp duration Appearance Settings color amp graphing preferences These settings are used by the program for test report header construction calibration procedures operating tolerances and scaling of readings Refer to instructions provided with disks to install or upgrade the software program Menu Tab click curso
47. l water It will interact unfavorably with chiller and internal components and connections a 0 0 00 H20 OUT Figure 2 CL400 Ports WATER TEMPERATURE RESERVOIR FILTER FUSE BEER TO iH 7 WITH 5 MICRON HOLDER UB SECTION 2 6 3 TAP WATER POWER CORD SOCKET WATER INLET RETURN 3 8 FNPT WATER OUTLET SUPPLY 3 8 FNPT AIR FILTER FRONT INSTALL PRECISION LOW PRESSURE REGULATORS REQUIRED TO PROVIDE 7 O p 6 9 kPa 1 PSI OUTPUT PRESSURE TH FO o OO i N CL400 ChemiLume A ON NITROGEN 9 BA cur our pop TT Z gt GAS OUTLET NO PLUMBING REQUIRED m UNLESS TOXIC SPECIMENS WILL BE TESTED IF SO E REFER TO LOCAL SAFETY REGULATIONS PORT MAY VENTED OUTDOORS OR RIDENS SYSTEM VIA TUBING RECOMMENDATIONS FOR WATER LINES USE 3 16 I D x 1 4 CAUTION DO NOT O D TEFLON TUBING CONNECT TO EXHAUST SYSTEM THAT MAY ALTER FOR GAS LINES USE 1 8 1 0 x 1 4 O D FLOW RATE RIGID WALL TEFLON TUBING Figure 3 Optional Water Chiller and Service Connections
48. lete and you may save the settings for future use The test settings can then be loaded at a future date by clicking on the Load Setup button in any cell Setup view 13 If desired save the test setup by clicking on the Save Setup button and the Save As swen coe I si dialog box Screen 5 8 will appear Type in 05 the desired file name and do not include an extension set is added automatically Click on OK to save the file 14 If you are setting up more than one test repeat the procedure above Steps 1 through Fiemme 13 for each cell in which you will conduct Saveasiype ChemiLume test seno se H Cancel test Otherwise continue with the next section Screen 5 8 Setup Save As Dialog Box 5 4 5 Before starting a test in the Setup view new empty specimen holders must be loaded into the cells These must then undergo cell conditioning preheat cleaning before the actual specimens are loaded The specimen holder cleaning is an integral initial part of the test procedure and is initiated with the Start Test button in the Setup view Screen 5 1 The holder cleaning at high temperature is mandatory for eliminating contaminants that can emit light during the test phase and alter results Solvent cleaning of the holders is adequate only 7 when conducting tests with temperatures below 200 C Follow the procedure below to initiate a test Tem
49. ll window select buttons Close window double Click View select buttons 4 4 2 SCREEN CONTROLS Graph Report System print print configuration menu amp menu amp menus options options PU Atlas ChemiLume CL400 Cell 1 testing Polypropylene XJZ 00 File Control View Window Help Restore rogram On line pr window Open test instructions mE archive Minimize Exit e program program r Test State Temperature Intensity Temperature Pre test stabilization in progress Gas flow Nitrogen flow detected in system Gas type coolant Nitrogen high flow rate OK Door Closed locked pe Cell status Test in progress Currently in pre test phase Waiting for temperature to stabilize Test Progress Pre test start 5 7 1997 2 55 55PM Elapsed time from pre test start 00 hours 00 minutes 32 seconds 44 6 C 300 0 C 200 0 C Stop Test Open Door Copy Logged Wata OmV Save Setup 10000mv Load Setup apy Logged Wata Om auto scale a 4 VI Yo E cens aie aft ei tec ix re c x Current One or more Minimized cell window additional open window double windows click to maximize Instrument Indicator Comm 1 0K CELL 2 CELL 3 CELL 4 2 57 PM Communications Cell status indicators COM port status Gray cell idle Gre
50. ller 2 5 SYSTEM CONNECTIONS cont 2 5 5 Computer Connections Locate the computer next to the CL400 on the bench Plug the monitor signal cable connector into the monitor port at the rear of the computer Fig 6 Plug the keyboard cable connector into the keyboard port on the back of the computer Plug the mouse connector into the mouse port at the rear of the computer CAUTION Before installing the computer power cord set the voltage selector beneath the power cord socket to match your supply voltage Use a ball point pen or pointed tool to slide the selector to the proper position 230V position shown Connect the power cords to the monitor and the computer and into an appropriately configured AC power outlet Connect the 9 pin serial communications cable to the port on the back of the CL400 Fig 3 and to the serial port on the back of the computer If you are connecting more than one CL400 to the computer please refer to the note under Computer Requirements in Section 2 4 System Requirements Continue with the procedures in Section 2 6 System Startup to verify operation of the CL400 and computer 230V 115V i 2 o 1 2D O O B Figure 6 Computer Ports 2 6 SYSTEM STARTUP Initially you must verify that the com
51. mation including analysis limits etc Screen 5 20 Graph Printing Options Analysis 5 4 PERFORMING TEST cont 5 4 7 Printing Results amp Cell Reloading cont 6 Use the Titles menu Screen 5 21 to add titles to your graph printout Multiple lines of text may be included Click on the pull down menu arrow buttons to select from a list of default titles or you may type ee in your own title Click on the Font button to select fonts Font Arial Bold 14pt 7 Use the Pen Styles menu Screen 5 22 to define the line styles colors and line width of the curves and indicator lines o7 on the graph Screen 5 21 Graph Printing Options Titles 8 The Axes menu allows you to define the range of time intensity esee lars temperature This permits printing m oe ee e cre expanded or compressed graphs You Temperatur EN amp Deed Paten may also zoom in on a detail of a graph Test Stat Indicator com Hwa m2 T Patter choose Current Viewport in this menu zj co Hwan mrs to print only that zoomed view OIT Baseline Color With m sold DIT Peak Slope Indicator Color zjwas ms Pattem Time Failure Analysis Points width je Pattern 9 To add headers or footers to the graph Integral Limits E
52. nal 115 120Vac 60Hz Fuse 250Vac 10A IEC 127 Type T 220 240Vac 50Hz Fuse 250Vac 5A IEC 127 Type Computer 100 220Vac 50 60Hz Universal switchable Gas Requirements Nitrogen Oxygen Input Pressure 6 9 2 0 kPa 1 0 3 0 PSI 6 9 2 0 kPa 1 0 3 0 PSI Flow Rate Low 25 5 0 ml min cell 25 5 0 ml min cell 1 53 0 3 0 in min cell 1 53 0 3 0 in min cell Flow Rate High 50 5 0 ml min cell 50 5 0 ml min cell 3 1 0 3 0 3 1 0 3 0 in min cell Important Standard bottle gas regulators are not adequate for regulating input pressure to 6 9 kPa 1 PSI You must install secondary regulators for each gas type Contact Atlas for recommendations The CL400 is not certified for use with gases other than nitrogen and oxygen Water Chiller Minimum Requirements if customer supplied Thermal Capacity 480 watts 20 ambient Temperature Stability 0 5 2 45 5 REQUIREMENTS User Supplied This section describes the equipment requirements of the system computer and water chilling unit 2 4 1 Computer Specifications Type IBM Compatible Pentium 75 MHz Operating System Windows 95 RAM 16 Mb Monitor 15 Color 1024 x 768 capable Video Controller 1024 x 768 mode or better Hard Disk Drive 540 Mb Floppy Disk Drive 3 5 1 44 Mb Parallel Port 1 Serial Port 1 see note Input Devices Keyboard and mouse Printer Hewlett Packard laser recom Note Addi
53. not reached within 1 hour of the projected duration Pre test Test Phase Phase N Starting o Temp Figure 10 Ramped Temperature Test Profile Temperature profile Constant 200 0 i Set point C Ramped Starting temperature 22 Ramp rate Ending temperaturene Deviation 20 gt Tolerance alarm Screen 5 2 Temperature Profile Selections 5 3 TEST DEFINITION cont 5 3 2 2 Temperature Profile cont 6 For a constant temperature test specify a value for the Setpoint by clicking in that edit box and typing the value desired or increment the value by clicking on the indexer arrows Maximum temperature is 250 C 7 For a ramped temperature test you must specify Starting temperature the cell temperature to be reached before controlled ramping begins Ramp rate the rate at which cell temperature is to increase during the test phase Range 1 to 10 C minute in 0 1 C increments Ending temperature cell temperature to be reached at the end of the test phase Maximum 250 C Set these values by clicking in the appropriate edit box and typing in a value or increment a value by clicking on an indexer arrow 5 3 2 3 Deviation Alarm The Deviation alarm provides visual warnings in the V Deviation 30 Tolerance amp C program and Monitor windows and flags messag
54. ns gray when the cell is cooled 12 After a cell has cooled down the drawer will unlock Open the drawer remove the cell cover and remove the specimen holder Discard the holder and specimen Note The cell cover may have seized due to high temperature exposure You may use large pliers to open it but take great care to avoid scratching the cover lens 13 Conduct another test in a vacant cell by following the procedures of Sections 5 2 through 5 4 14 Continue with Section 5 5 Analyzing Test Data for instructions on performing analyses of the test data 5 5 ANALYZING TEST DATA This section describes how to use the Analyze view to perform four different analyses on the test data 1 Oxidation Induction Time OIT time at which light emission intensity curve begins to increase from baseline which is the time interval to onset of exothermic oxidation of the material Applies to constant temperature isothermal tests 2 Integral integration of area beneath intensity curve between two limits Applies to constant temperature isothermal and ramped temperature tests Yields total integrated intensity in milliVolts 3 Time to Failure duration at test temperature to 50 oxidation Applies to constant temperature isotherm tests Yields induction period oxidation rate constant and material lifetime measurement 4 Activation Energy activation energy of hydroperoxide decomposition Yields activation
55. og status flags C Adaptive Projected data file size 31K Temperature profile Start Test Constant 200 0 2 Set point C Save Setup Ramped Pa REA erat Load Setup Deviation 2 0 alarm Tolerance C Gas Types Pre test phase Test Phase Nitrogen high flow high flow Test Phase Duration 15 4 hrs 0 0 Screen 5 1 Cell 1 Setup View Material Description Type in a description of the specimen to be tested in the cell Company Name Type in the company name associated with the test Note If this is first time a test will be run in the cell the company name previously entered in the System automatically be inserted menu will Operator Type in the name of the person who will conduct the test Pretest Comments Type in information particular to this specimen or the test to be conducted in the cell 5 3 TEST DEFINITION cont 5 3 2 2 Temperature Profile Select your test Temperature Profile and Test Phase Duration according to the instructions below These must be specified first to allow the data logging feature to provide file size estimates 4 The CL400 can perform two types of tests Constant temperature isothermal Fig 9 Ramped temperature Fig 10 Each profile type has two phases Test Phase Phase Temperature Pre test p N Setpoint Time
56. on lines will appear with adjustment handles 6 Adjust each line by moving the cursor onto a handle and holding the left mouse button down Drag the line end as required and then release the mouse button The horizontal line baseline should be adjusted to match the slope of the curve as shown with the line passing through the center of the curve data points 5 5 ANALYZING TEST DATA cont 5 5 2 Oxidation Induction Time OIT Analysis cont The peak slope line should be adjusted to pass through the steepest point of the ascending curve Both ends are adjustable to allow angling of the line Note For a more detailed view of the curve when making manual point selections click on the zoom button move the cursor to a point just outside the area of interest hold the left mouse button down and drag a zoom box around the area Release the mouse button 7 Click on the Analyze button to perform the analysis Results are shown on the graph by the OIT line and beneath the graph in the edit boxes Screen 5 27 Cell 1 testing Polypropylene XJz 001 1 17 Ex setup monitor analyze F calibrate Material Polypropylene XJZ D01 Intensity 1327mV Timeline Elapsed time 0 32 22 Temperature 199 8 OIT 8000 250 0 7000 218 8 Integral E 6000 82 Time to Failure 5000 15833 4000 42508 E E 5 3000 93 8 E 2000 25 9 1000 31 3 ww o0 4 44 lt zoom in 0
57. operties General Shortcut file name Target type Application C CL400 CL400 exe cfg c CL400 your cfg Target location cl400 wh ere Target C ci400 c1400 exe cfg C CL400 your ctg cfig indicates that a unique NUR 21400 configuration file is to be loaded Shortcut key None Bun Normal window hal CACL400 indicates the path to the subdirectory in which the cfg file is located Eind Target Change Icon your cfg is the name of the configuration CK Concet file to load at program startup Screen 3 11 Shortcut Editing Menu Note If your configuration file is located in a subdirectory other than CACL400 change the path in the command line to reflect the actual subdirectory location 5 Click on the OK button when finished 6 Repeat the procedure above for each CL400 icon on the desktop applicable only to multiple instrument Open installations eS 7 Confirm that you have performed the above steps cut properly by double clicking on the CL400 program icon EL AEN to start the program Create Shortcut Delete 8 In the program click on the System button near the Rename top of the screen and then click on the System menu Properties tab The System menu should indicate the file you designated for autoloading beside Configuration File Screen 3 10 If the file name shown is default cfg repeat the steps Program Icon Menu above and check the command line in t
58. ough 3 6 Be aware that this file will contain the specifications for your calibration standards and PMT gain settings etc Thus you must be careful that these are properly configured for each new configuration file created At program startup you may load a uniquely named configuration file by accessing this screen and clicking on the Open button These procedures are discussed in detail in Section 3 7 8 Do not click the OK button in these procedures until you are advised to do so Important When you finally exit from the system configuration menus by clicking on the OK button all settings will be automatically saved in the file designated in Step 7 above Or you may save the configuration under a new file name see Section 3 7 3 2 PMT INTENSITY STANDARD An optional kit is available for use with the CL400 that contains a liquid intensity standard The standard is a radioactive low emission source It is used to calibrate the PMT photomultiplier tube or light sensor monitoring each test cell The intensity standard comes with a specification sheet that characterizes its emission output and the date these measurements were performed This is critical information that must be recorded in the software configuration to allow accurate PMT calibration 1 Click on the PMT Intensity Standard menu tab to bring up the Standard Values listing Screen 3 2 3 2 PMT INTENSITY STANDARD cont 2 Refer to the specification S h
59. our secondary gas regulators to the CL400 back panel inlets with rigid 1 8 inch I D x 1 4 inch O D teflon tubing see Figs 2 amp 3 If you purchased the regulators and chiller from Atlas all tubing is supplied 6mm adapters are available from Atlas for gas connections Limit gas line lengths to 3m 10 ft maximum between the CL400 and supplies After making connections adjust the gas pressure to 9 7 kPa 1 4 PSI or 22 oz in on some regulators This setting is above the 6 9 kPa 1 PSI maximum input pressure since the CL400 gas flow is off During operation the pressure will drop slightly due to flow Readjust the gas regulators to 6 9 kPa 1 PSI during operation to achieve the most accurate setting Readjustment may also be required if you choose to run a test in only a single cell rather than all four 2 5 2 Water Chiller Connections The chiller supplied by Atlas has 3 8 FNPT threaded inlet and outlet ports Fig 3 Install tubing compression connectors similar to those on the back of the CL400 Use the supplied 3 16 inch I D x 1 4 inch O D teflon tubing to connect the chiller ports to the CL400 water ports in Europe or Japan use 6mm adapters If an alternate tubing is used it must be capable of withstanding 120 PSI at 86 F 828 kPa at 30 As much as possible avoid unnecessary bends and minimize tubing lengths to promote cooling efficiency Fill the chiller with clean tap water Fig 3 DO NOT use deionized D
60. own otherwise go to Step 7 5 5 ANALYZING TEST DATA cont 5 5 4 Time to Failure Analysis cont 5 Manual Point Selection Click on the Define Custom Points button and the and la definition lines will appear with adjustment handles eak 1 testing Polypropylene XJZ 001 setup M monitor analyze FK calibrate Material Polypropylene XJZ 001 Intensity 915 Timeline Elapsed time 0 33 49 Temperature 200 2 C TEE OIT 8000 7000 Integral 5 Time to Failure 5000 4000 e 3000 r 2000 1000 0 4 4 zoom ou zoom in 0 00 00 0 10 00 02009 03000 04000 05000 1 00 00 Elapsed Time h m s 00 h m s 0 11 30 Induction Period b 14 0 him s 0 22 42 Oxidation Rate Constant a inverse hours 49 7 Automatic Points Critical Degree of Conversion 1 50 Time to Failure h m s 0 15 53 Points Logging File cell1 44 Screen 5 31 Time to Failure Analysis Results 6 Adjust each line horizontally by moving the cursor onto a handle and holding the left mouse button down Drag the line and then release the mouse button Note For a more detailed view of the curve when making manual point selections click on the zoom button move the cursor to a point just outside the area of interest hold the left mouse button down and drag a zoom box around the area Release the mouse button 7 Select a value for th
61. pears in the white circle to mark the selection Screen 3 7 Communications Configuration Menu 3 8 SAVING THE CONFIGURATION FILE The new software configuration can be saved in two ways 1 by clicking on the OK button at the lower right of the menu all settings are saved in the current config uration cfg file or 2 by returning to the System menu and clicking on the Save As button the configuration file may be given a new name ending in cfg The main purpose of the Save As button is to allow the user to create new configuration files without altering the startup settings initially saved in the DEFAULT CFG file normally loaded at startup 3 8 SAVING THE CONFIGURATION FILE cont Preserving the DEFAULT CFG file and performing a Save As to create new configuration files will allow the user to always be aware of the startup settings when creating a new file Atlas advises saving the initial con figuration to the DEFAULT CFG file and then creating user configuration files from it with the Save As function Saving the DEFAULT CFG File Save the initial software configuration just completed as default cfg Create customized configuration files for multiple CL400 units by following the steps under Saving Customized Configuration Files below 1 Click on the System menu tab to bring up the System menu Screen 3 1 2 Click on the OK button at the lower right of the window and the file will be saved to the hard disk Th
62. perature 5 4 1 Cell Conditioning and PMT Gain Settings 1 Click on the system button at the top of the screen to Conditioning Period 2 2 2 N 5077 Load Specimens Screen Prompt Appears bring up the system configuration menus Time 2 Bring up the Advanced Test Settings menu Adjust Cell Conditioning the PMT Gain settings according to the instructions Temperature Profile under Procedures for Test Setup in Section 3 4 3 Bring up the Cell Conditioning menu and Wis adjust the settings according to the calibration should be performed instructions under Procedures for Test rcu que Setup in Section 3 5 Temperature calibration should be performed once every year Last PMT calibration 2 19 1996 Last Ternperature Calibration 2 19 1996 4 Save the new settings in the current configuration cfg file by clicking on OK to exit the system configu ration menus or Press OK to continue with your test or CANCEL to go back and perform a calibration save to a new file by clicking on the Save As button in the System menu and naming Dont show this reminder any more a new file see Section 3 8 for instructions Screen 5 9 Calibration 5 4 2 Cell Conditioning Phase 5 Open each cell drawer in which a test is to be conducted Remove the cell cover Fig 4 Place a new clean specimen holder into each cell and reinstall the covers Close th
63. ports Calibration report Print Options Graph User preferences for printing graphs of analysis results are specified in these screens Parameters Titles amp Axes Pen line Colors Page Layout amp Fonts Analysis E Aii Graph Printing Options x Titles Styles Axes Analysis Page Layout Line 1 z Line 2 Font Arial Bold 14pt Cancel 5 2 PMT CALIBRATION Perform the PMT calibration Section 6 1 at the beginning of each testing day Print the summary of results each day and compare them to determine calibration stability If conditions in your laboratory are very stable the PMT calibration interval may be lengthened to twice or even once per week 5 3 TEST DEFINITION To run a test in the CL400 you must first specify the temperature profile data logging interval gas type and I D information for the test report The Setup view of each cell window is used for this purpose The independent Setup views allow you to perform up to four different tests at the same time or the same test on four different specimens As well you may conduct identical tests with identical specimens in each cell for rapid determination of a material s average performance You may setup and initiate a test in one or more cells while tests are still running in other cells 5 3 1 Cell Conditioning Phase Tests having a peak temperature of 200 C or above include a cell conditioning
64. puter is functioning properly that the CL400 powers up and that the chiller temperature is properly set Full functionality of the CL400 cannot be verified until the software program is operating and initial calibrations are performed 2 6 1 CL400 ChemiLume 1 Turn on the CL400 power switch Fig 4 The power switch should light up to indicate power is present If it doesn t check the power cord connection to ensure it is fully engaged in the socket on the back of the unit and plugged into an AC power outlet of the correct voltage 2 If the power switch is still not lit unplug the CL400 from the power source and check the input fuses on the back of the unit Fig 4 Contact Atlas Service if the CL400 fails to operate when power is applied 3 Turn on the chiller 2 6 2 Computer and Monitor Important To conduct the following steps the CL400 software program must be installed Refer to software installation instructions with disks if the program is not present on your computer 1 Turn on the video monitor 2 Make sure that the computer disk drive is empty Remove any disk or shipping protector from the drive 3 Turn on the computer power switch The Windows 95 ALL operating system will initiate Figure 7 4 The Windows 95 initial screen desktop screen Program includes a 1400 ChemiLume icon Fig 7 Move the Icon mouse cursor onto the icon and double click the left mouse button to start the CL400 progr
65. r here to select 3 1 SYSTEM DATA 1 Start the system computer as described Section 2 6 2 the CL400 ChemiLume program by double clicking on the System Description program icon System Name System SerialNumber 2 Click on the system Company Name fYourCompary button at the top of the Configuaton Fie 7 screen or click on the File menu at the upper left and select System Configuration 3 Click on the System menu tab to bring up the System Description parameters as shown in Screen 3 1 Screen 3 1 System Configuration Menu 4 System Name Click in the white edit box and type in the name you prefer for the CL400 If you have more than one CL400 attached to the computer it is advisable to include an identifying number in the name 5 System Serial Number Type in the serial number found on the label at the back of the CL400 3 1 SYSTEM DATA cont 6 Company Name Type in the name of your company This name appears on the test report 7 Configuration File Indicates the currently loaded configuration cfg file that defines the software setup Note If the configuration file name default cfg is used this file will be loaded automatically at program startup If you wish to create different configuration files to be used with different CL400 units return to this screen System after you have performed the setup in Sections 3 2 thr
66. re values that CN allow the software program to determine the offset me system and meter probe Ponsa readings These values included on the certificate supplied with the temperature probe and must be entered in this menu Cancel 1 Click on the Temperature Calibration Probe menu tab to bring up the menu Screen 3 3 Temperature Calibration Probe Configuration Menu 3 3 TEMP CALIBRATION PROBE cont 2 Click in the white edit boxes and type in the required parameters for the Actual and Indicated Temperatures as listed on the calibration probe certificate 3 4 ADVANCED TEST SETTINGS These settings allow the user CL400 System Configuration to select the sensitivity level PMT Intensity Standard Temperature Calibration Probe Cell Conditioning of the PMT photomultiplier ae S Coi tube or light sensor for differing specimen emission rates An automatic carg calibration reminder that will Clow vo appear on the screen before each test is initiated may E Cell 2 Cell 4 also be enabled in this menu C Low C Low High High 1 Click on the Advanced Test Settings menu tab Screen 3 4 to bring up the menu Show calibration reminder 2 Click in the white box beside Show calibration Screen 3 4 Advanced Test Settings Configuration Menu reminder unt
67. stretch the view box to enclose the area desired Release the mouse button Click on the panning arrow buttons to move the zoomed view to the desired position Click on the Zoom Out button to return to a full graph view 7 The Analyze view includes features for performing test data analyses and printing a report covered Section 5 5 Analyzing Test Data 5 4 5 Exporting Data As test data is gathered it may be examined visually in the Analyze view or it can be copied to a file for export to another analysis program The copy procedure saves the currently logged test data and will not affect or interrupt test data logging to the file originally named at test initiation 1 To export the test data during the test click on the Setup or Monitor button to return to a screen that includes the Copy Logged Data button 2 Click on the Copy Logged Data button and the Copy Data dialog box Screen 5 16 will appear Zoom view box 7 Cell 1 test hatted setup F M monitor analyze Timeline OIT Integral Time to Failure Material Polypropylene XJZ 00 Test Status Test complete haj d by user 0 00 00 0 10 00 0 30 00 04000 05000 Elapsed Time h m s 0 20 00 Cursor time 0 29 20 Screen 5 14 Zoom View Selection Box Logging File cell1 tt Cursor Intensity 4502 Cursor Temperature 140 7 C
68. t is 50 above the peak test temperature to be reached in that cell Set each by clicking in the white edit box and typing in a value or by incrementing the value by clicking on an indexer arrow The maximum allowable setting is 300 C 3 6 APPEARANCE SETTINGS This menu allows selection of screen colors for graphs and analysis data as well as selections for the use of a graph grid overlay and cell window arrangement Graphs appear in the All Cells window and in the Analyze window for each cell if a test is running or if an archived file is open 1 Click on the Appearance menu tab Screen 3 6 to bring up the menu 2 Choose screen colors for the various graph elements by clicking on the pull down CL400 System Configuration PMT Intensity Standard Temperature Calibration Probe Cell Conditioning System ance Communications Advanced Test Settings Colors Graph background Integra points E Temperate Intensity on Test phase start indicator DIT baseline Failure time analysis points NI DIT peak slope Show grid on graph Auto arrange cell windows Screen 3 6 Appearance Settings Configuration Menu menu button down arrow and then the desired color Graph Background fill color of graph normally black or white for best contrast Temperature Intensity Test Phase Start Indicator cell temperature curv
69. tional Serial Ports If more than one CL400 ChemiLume is to be connected to the system computer an additional serial interface card must be installed in the computer Such serial cards are available with single or multiple ports Atlas recommends using a serial board having two ports such as the Black Box Corporation Dual Port RS 232 422 485 Serial Interface or equivalent 2 4 2 Water Chiller Specifications The water chiller provides constant temperature cooling for the four PMTs photomultiplier tubes in the CL400 The PMTs are very sensitive and must not only be properly cooled but maintained at a stable operating temperature The load on the chiller increases with CL400 test temperature therefore the chiller must be capable of rapid response and tight temperature control Operating Environment 5 C 41 F 40 C 104 F Thermal Capacity 480 watts 20 C 68 F Temperature Stability 0 5 Flow Rate 8 7 liters min 2 3 gal min Filtration 5 microns or better 2 5 SYSTEM CONNECTIONS Connect gas and water supplies first to eliminate leaks 2 5 1 Gas Supply Connections The CL400 requires nitrogen and oxygen for proper operation These gases may be supplied from a central facility source or via bottled supply In either case secondary regulators are required for limiting input pressure to the CL400 to a maximum of 6 9 kPa 1 PSI It is recommended that these be purchased from Atlas Make connections from y
70. ty 1196mV Timeline Elapsed time 0 32 46 Temperature 199 9 C OIT 8000 250 0 70005 218 8 Integral 6000 187 5 5 s Time to Failure 5000 15534 4000 125 0 3 5 3000 938 2000 625 1000 31 3 05 4 44 lt zoom 0 00 00 0 05 00 0 10 00 0 15 00 0 20 00 0 25 00 0 30 00 Elapsed Time h m s Analyze Low Time h m s 0 00 00 Integrated Intensity High Time h m s 0 32 30 Define Custom Points Logging File tt Screen 5 29 Integral Analysis Results 7 Click on the Analyze button to perform the integration The results are shown in the Integrated Intensity box at the bottom of the view Screen 5 29 8 Print the results by clicking on the Graph or Report print button at the top of the program screen or by selecting Graph or Report print from the File menu See Section 5 4 7 to configure the printing options 9 To perform another integration repeat from Step 3 5 5 ANALYZING TEST DATA cont 5 5 4 Time to Failure Analysis This analysis may be performed only on constant temperature isothermal test data 1 Open a data file as described in Section 5 5 1 above or continue with the currently open data file Line adjustment handle 2 Click on the Time to Failure button Cell 1 testing Polypropylene XJZ 001
71. u are satisfied with the results as observed in the Intensity graph of the Analyze view 5 3 2 5 Gas Types These settings allow you to select the gas type and flow rate during the pre test and test phases of your test You may also choose None to prevent gas flow During a constant temperature test the specimen is typically exposed to nitrogen during the pre test phase to prevent oxidation while temperature is rising and then is exposed to oxygen during the test phase at setpoint temperature to optimize oxidation Your needs may differ and you also have a choice of two flow rates Low Flow 25 ml minute cell High Flow 50 ml minute cell 10 Select Gas Type by clicking on the pull down menu button Screen 5 5 and then clicking on the desired selection Do this for both Pre test and Test Phase 5 3 2 6 Data Logging Two methods for logging test data are available to accommodate specimens with differing light emission characteristics Every Point and Adaptive Secondary options allow you to set data collection preferences You may experiment with different sampling rates and observe the Projected Data File Size 100 0 0 I sec Screen 5 4 Test Phase Duration Phase Duration Gas Types Pre test phase Test Phase Nitrogen low flow low flow Nitrogen low flow Nitrogen high flow Oxygen low flow Oxygen high flow Screen 5 5 Gas Type Selection 5 3
72. vation Energy Analysis Results This analysis may be performed only on ramped temperature test data 1 Open a data file as described in Section 5 5 1 above or continue with the currently open data file 2 Click on the Activation Energy button There are no user adjustable setup options for this analysis 5 5 ANALYZING TEST DATA cont 5 5 5 Activation Energy Analysis cont Calculations are performed upon the data beginning at the oxygen start time beginning of test phase and ending at the last data point recorded end of controlled temperature ramp 3 Click on the Analyze button Results are shown at the lower right of the view Screen 5 32 4 Print the results by clicking on the Graph or Report print button at the top of the program screen or by selecting Graph or Report print from the File menu Follow the instructions of Section 5 4 7 for configuring the printing options 5 To perform another analysis repeat from Step 3 Calibration of the PMT photomultiplier tube light sensors in the CL400 ensures that each is operating properly and is accurately calibrated This must be conducted initially on a daily basis After you acquire a short history of calibration results you may determine that PMT calibration is only necessary at 3 day intervals or weekly Examine the calibration results collected and make your own determination PMT stability can be affected by ambient temperature fluctuations and vi

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