Jasco FTIR 4000 and 6000 series Operations Manual
Contents
1. Ready Fig 2 12 Spectra Measurement Program This completes the preliminary operations needed for the measurement software The instrument is now accessible to the user 15 2 2 Measurement The polystyrene film included with the instrument is used as a test example for measuring saving and printing spectral data 2 2 1 Setting of Instrument Measurement Parameters In JASCO Spectra Manager CFR measurement parameters are created with an audit trail After starting a measurement program set the measurement parameters or select a preset parameter file For test purposes set the initial measurement parameters to the values listed in the table below Table 2 3 Initial Measurement Parameters Standard Number of scans 16 Sample Data type T Abs R Int Resolution 4 cm Operator Auto save OFF not Checked Range 4000 400 View Range 4000 400 Division Send data ON Checked Vertical axis AT Comment Print out OFF Not Sample Checked Vertical axis Background Single Source Standard Apodization function COS Detector TGS Zero filling ON Checked Sample Standard Phase correction Mertz chamber Gain Auto Phase correction Auto filter Aperture Auto Use timer Off Not Checked Scan speed Auto Filter Auto Note 1 For the FT IR 4000 series a spectral scan range from 7800 to O cm can be selected however valid data can only be collected from 7800 to 350 cm For the FT IR 6000 series a value from 15 000 to O2. 2 25 Enter the password for the currently logged user and click lt Sign gt to complete the electronic signature process for the file save Creation Signature P Usemame Administrator Reason Improvement of S M w Cancel Fig 2 25 Creation Signature dialog 6 This completes the saving of spectral data to a file The title bar of the view changes to View lt Polystyrene jws gt 24 3 Spectra Manager Reference Spectra Manager is the program that manages communication such as selection starting stopping the spectrometer and setting the communication port between the PC and spectrometer and starts the various spectra measurement analysis programs and the File Viewer program Fig 3 1 Instrument sub tree Lists the names and ID numbers of all instruments currently connected to the PC Measurement programs are associated with each individual instrument and can be started by double clicking the desired measurement program EE Spectra Manager Program View Help Ge Instrument beat FT IR 4100typeA Ed Spectra Measurement E Analysis JASCO Canvas 24 Spectra Analysis Tnstrumen Model Name Serial No Conditions Username FTAIR 4100 FT4TR 4100 400961016 Waiting Analysis sub tree Status bar Analysis programs are listed here Newly installed Displays the status of communication application programs are automatically added to this between the PC and spectrometer list
3. eee eR e po AAA data range box Ma E E er this can be set to Single single beam Interferogram Int T R or Abs See Table 4 2 Measurement Data types for details Sample _ Specifies the data type to be used for sample measurements o Background Specifies the data type to be used for background measurements Accessory Shows the accessory information 36 4 2 8 2 Information tab The Information tab shown in Fig 4 13 contains the following settings E Parameters Advanced Mal Standard Information Data Optics FFT Timer Sample Operator Division Comment a Display information dialog before measurement ie Information Tab of the Parameters dialog Sample Enter the sample name up to 127 alphanumeric characters Operator Shows the logon name of the current user Cannot be modified Division Shows the Division or Workgroup for the current user Cannot be modified Comment Enter any comments here up to 127 alphanumeric characters if desired wa a information dialog measurements The dialog then prompts for all the information before measurement displayed on the Information tab 37 4 2 8 3 Data tab The Data tab shown in Fig 4 14 contains the following parameters E Parameters Advanced Bele Standard Information Data Optics FFT Tirner Data type 21 Abs A Int w Auto save Use auto save Folder Format st
4. 29 vil ales Open Parameters lt 2 lesan ae esos cds 29 AA sil Parameter e arean ie ENEE II by bucce lila ss OAE 30 PMA A btes Setaes haa ce aces 30 d2 Measure Menta A 30 A Cal A eo 31 A Sample AAA A A 32 7 ENS ee aaa UL 2 O eae ete URN rea ea ree URI Tr MMT Ve UTE Re CSRS WA nen em Mae nee NUE TeT ne 32 42A MOROS ale Iii 32 2o Monitor Backo round lacra crii 33 420 Sample Measurement P n A A 34 4 2 1 Backeround Measurementt A eiea 35 ELS Parametere a a a aa A 35 kO A A 36 A 202 Moria On WAGE didas 37 eo Oaa CAD E E E 38 Aza Optica tard 39 a FETE mer La Dichscaatedesthatescie cde ajeteaatatdis hat angles E tuned tales hee ec ace 41 43 SEM MICA a a S S 42 Ao TAA maaa a a a a a a 42 BAe a a eaa a i a e eaa a EA 43 PEE Se A a E ft ha a eM O 43 AAD A ete tte Asa cedar aceasta ett ca iat A E shar E sabes Stace Alena OENE 44 AD A A A sae 45 Perea A O II II A Saancmestuacabe 46 IN O A O A A A 46 BAG NS otis des telat atic a A as ota A sed baat 47 ME SAUS OAL A a a 47 Ao e E i O CEEI E O E E da ees 47 ALO Customize Toobar rt id A 47 AS AA O NN 48 ASe A A A O AA 48 Vill 1 Introduction The following section describes how to read this manual and explains the notation screen configuration and special terms used throughout this manual Read this section first 1 1 Measurement System Configuration of Fourier Transform Infrared Spectrometer The JASCO Fourier Transform infrared spectrometer
5. 7 l PS a Addidelete instruments r A O ad o EN ES ES E a x O E o on 762 i 2 ange 7 Table 1 3 Privileges assigned to each Workgroup Access Level Electronically sign data OK OK OK Figure 1 2 shows the typical operating flow of the JASCO Spectra Manager CFR First a user is created registered and the System Access Level is assigned using the Administrative Tools A Workgroup is created registered and individual users and analytical instruments are assigned to the Workgroup Detailed access to instrument control and analysis applications can be set at the User and Workgroup levels Access control levels as required by 21 CFR Part 11 regulations are determined by the Administrative Tools settings Routine analyses can then be conducted by the operator using the measurement analysis applications in JASCO Spectra Manager CFR Since all levels of access are managed by the Security Manager individual users are only able to execute procedures that are allowed by their assigned access level Access control ranges from declaring measurement parameters to conducting measurements and performing data analysis Analytical data obtained using any of the procedures described above can be saved as an electronic record with an electronic signature The JASCO Canvas CFR report creation utility allows printing to paper medium in user defined formats Administrative Tools User registration Workgroup registration Access ng ht
6. AI he ok tk QB ate AE AD AT 4 Spectra Analysis E m wiew 1 Me mory 1 Item Contents User Division Company Jasco Creation Date 2004 04 09 13 12 sample Mare Comment Data Information 000 00D Wavenumber cm 1 Fig 2 23 Spectra Analysis Program and View of Measurement Results This completes sample measurement 2 2 4 Saving the spectrum The spectrum can be saved to file from either the Spectra Analysis or Spectra Measurement programs as follows 1 Select Save As from the File menu The Save As dialog appears Fig 2 24 Save data Saven O Heneko OL E Filename pye 40426 Save as type JASCO Standard File jws y Fig 2 24 Save As dialog 2 First ensure that the file type is set to JASCO Std JWS in the Save as Type drop down menu This usually does not need to be changed 3 Navigate to the directory folder in which to save the spectrum using the Save in drop down list 23 Note In Spectra Manager CFR there may not be a choice of directories available for saving the file In this case save the file in the pre selected directory 4 After selecting the appropriate location enter the filename Polystyrene in the File Name field 5 After entering the filename click the lt OK gt button The extension jws is added to the filename and the file is saved as Polystyrene jws In Spectra Manager CFR the Creation Signature dialog is then displayed Fig
7. Programs are started by double clicking a selection from this list Fig 3 1 Spectra Manager window Note Communication refers to sending control signals from the PC to the spectrometer or transferring measurement data from the spectrometer to the PC 3 1 Analysis Applications All of the analysis programs are located in the Analysis sub tree of the tree view in the left panel of the Spectra Manager main window Applications can be started in one of three ways The first is to double click the name of the application The second is to right click on the application then select Start from the context menu that appears The third way is to select the application of interest then select Application Start from the main menu 3 2 Measurement Applications All measurement applications are associated with individual instruments and these are contained in the Instrument sub tree of the tree view in the left panel of the Spectra Manager main window A spectrometer should be turned on prior to starting the associated measurement program Similar to the analysis applications measurement applications can be started in one of three ways by double clicking the application by selecting Start from the right click context menu or by selecting Application Start from the main menu Multiple measurement programs cannot be run simultaneously for a single spectrometer 25 3 3 Exit To exit Spectra Manager select Program Exit from th
8. Transmittance T spectrum xx 100 Single beam spectrum of background Therefore when measuring a sample without first measuring the background only a single beam Single or interferogram IF spectrum can be selected in the Parameters dialog Transmittance spectra can be obtained by measuring the sample single beam spectrum after measuring a single beam background spectrum with the appropriate arithmetic calculations being performed for the 2 single beam spectra The single beam spectrum represents the total energy spectrum of the light source sample if present and other optical elements The absorption by water and carbon dioxide in the air also directly influences the spectrum These external influences can be eliminated by obtaining the ratio between the background and sample measurements as described above The concentrations of water vapor and carbon dioxide in air are constantly changing Therefore if absorption by water vapor and carbon dioxide will significantly affect a spectrum the background should be re measured just prior to the sample spectrum However it is not strictly necessary to measure the background each time a sample is measured The table below lists the file types that can be selected Table 4 2 Measurement File Types IF Single T R Abs Int IF Single T R Abs Int IF Single T R Abs Int Note 1 For multiple measurements be sure to measure the background periodically This will minimize t
9. and Setting FT IR properties Turn on the PC and monitor power switches Windows will start up after which the following start up desktop is displayed on the screen FT IR properties need to be set prior to using the FT IR instrument The method for setting the instrument properties is described below Note Only users with Administrator privilege have access to this function 1 After Administrative Tools is selected right click the mouse button on the instrument and click on the Resister Instrument command Fig 2 1 E Administrative Tools Operation View Help m Administrative Tools Ih trumern Model Mame Serial No Conditions 2a cis Register pean TAIR 41 FTIR 4100 400961016 Waiting nalysis l a e System Information Fig 2 1 Properties 2 Select a driver name and click the lt Next gt button Fig 2 2 Select Instrument Driver Select Instrument Driver Driver name Description FTIR Control Driver JASCO FTA1RA 4000 6000 seres control diver Cancel Fig 2 2 Select Instrument drivers 3 After entering the Instrument type Model name and Serial No clicking the lt OK gt button will register the FT IR to the control PC Fig 2 3 In this case please input an optional name for Instrument input the Serial Number found on the plate on the side of the FT IR and select the Model Name from the drop down list Instrument Properties Enter Model Mame a
10. em can be selected the valid data range will vary depending on the available beamsplitters sources and detectors Note 2 This field can be set to any value maximum of 127 alphanumeric characters Note 3 In Spectra Manager CFR these values are automatically set using current user information and cannot be changed To set the instrument parameters in the Spectra Manager CFR the user must have an access level of Manager or Analyst Select the instrument Parameter Setting dialog using the Measurement menu Fig 2 13 or click on the instrument parameters tool button to access the instrument parameters dialog Fig 2 14 16 1 2 3 4 Sample Background Monitor sample Monitor backeround Sample Parameter Fig 2 13 Parameter command in the Measurement menu E Parameters Advanced lx standard Information Data Optics FFT Timer Number of scan FP Auto Estimated scan time 00 00 47 Resolution Range View range A ee Fit view range to data range Vertical axis Sample AT v F Auto baseline correction Settings Pl Auto background scan Settings Pl Evaluation Settings Accessroy Not equipped Fig 2 14 Parameters dialog On the Standard tab set the Number of Scan to 16 Click on the Auto check box to deselect Auto if necessary Set the Resolution to 4 cm This is set by changing the value in th
11. point for the horizontal or vertical axis Set As Default Check to use the selected settings as the default settings on restart 4 4 6 Toolbar The toolbar submenu 1s used to turn toolbars on and off File Display tool buttons related to file functions Measure Display tool buttons related to measurement functions View Display tool buttons related to view menu functions 4 4 7 Status bar Toggles display of the status bar 4 4 8 Information bar Toggles display of the spectrum information 4 4 9 Customize Toolbar Displays the Edit Toolbar dialog shown in Fig 4 26 which can be used to toggle toolbars on and off and to customize the various toolbars Edit Toolbar File Measurement View Display O button text Fig 4 26 Edit Toolbar dialog File Check to display file related toolbar buttons a a Cee a Check to display view menu related toolbar buttons O Cait Click to open the Customize Toolbar dialog 47 Customize Toolbar El Ed Available toolbar buttons Current toolbar buttons wit Analysis Separator cel Open Par ul Save Par o FigW4 27 Customize Toolbar dialog Display button text Displays text descriptions under each button on the toolbar 4 5 Help Menu This section describes the Help menu shown below Fig 4 28 Help About Fig 4 28 Help Menu 4 5 1 About Select this item to display the version in
12. tab Fig 2 15 Enter Air as the Sample Name Change other settings as desired The Operator and Division fields are input automatically for the current user To input a Comment click on the comment field If the Information fields are to be changed before every measurement check the Display information dialog before measurement check box Note The Operator and Division fields cannot be changed in Spectra Manager CFR 7 Select the Data tab Select T Abs R Int from the drop down menu for the Data Type Ensure that Auto save and Print out data are unchecked 1 e OFF but that Send data to spectra analysis is checked 8 Select the Optics tab Each parameter is set as follows Source is Standard Detector is TGS and Sample chamber is Standard In addition all of the IF interferogram parameters Gain Aperture Scan speed and Filter are set to Auto 9 Select the FFT Timer tab Each parameter is set as follows Apodization function 1s Cosine Phase correction is Mertz and Phase correction filter 1s Auto Check the Zero filling check box and uncheck the Use timer check box Note To maintain the audit trail for Parameter Settings in Spectra Manager CFR the instrument parameters must be saved every time they are changed lt In the case of Spectra Manager CF R gt If you try to close the parameter settings file withou
13. the Spectra Manager program 4 Spectra Measurement Reference Spectra Measurement reference Refer to this section when necessary for further information on the Spectra Measurement program 1 3 21 CFR Part 11 21 CFR Part 11 is a set of regulations regarding the digital archive of data and data records for GLP GCP and GMP procedures A number of areas are covered by these regulations including 1 access control and electronic signature requirements for data recorded by any computer controlled analytical system in which the results are digitally archived 2 the provision of security functions that can only be accessed by authorized personnel to ensure the security and integrity of data and 3 a data auditing mechanism with automatic creation of an audit trail to maintain a record of any creation modification or deletion of instrument data 1 4 Features of the 21 CFR Part 11 compatible Spectra Manager JASCO Spectra Manager is an integrated software package that acts as a common platform for the JASCO range of analytical instruments including UV VIS near infrared infrared fluorescence Raman polarimetry and circular dichroism spectrometers The Spectra Manager software provides functionality ranging from analytical instrument control and spectral data processing to sophisticated specialized data analysis programs JASCO Spectra Manager CFR provides security and auditing functionality that ensures the security integrity and confi
14. your JASCO distributor the model name and serial number of your instrument Notices 1 JASCO shall not be held liable either directly or indirectly for any consequential damage incurred as a result of product use 2 Prohibitions on the use of JASCO software Copying software for purposes other than backup Transfer or licensing of the right to use software to a third party Disclosure of confidential information regarding software Modification of software Use of software on multiple workstations network terminals or by other methods not applicable under a network licensing agreement concluded with JASCO 3 The contents of this manual are subject to change without notice for product improvement 4 This manual is considered complete and accurate at publication 5 This manual does not guarantee the validity of any patent rights or other rights 6 In general company names and product names are trademarks or registered trademarks of the respective companies 7 JASCO and the JASCO logo are registered trademarks of JASCO Corporation JASCO Corporation 2002 All rights reserved Printed in JAPAN 1V Limited Warranty Products sold by JASCO unless otherwise specified are warranted for a period of one year from the date of shipment to be free of defects in materials and workmanship If any defects in the product are found during this warranty period JASCO will repair or replace the defective part s or product
15. Background measurement 4 2 4 Monitor Sample This function allows measurement parameters to be modified while the spectrum is measured in real time The Monitor Sample dialog shown below is displayed Fig 4 8 32 E Monitor sample Advanced Standard Information Data Optics FFT Timer Number of scan 8 C Auto Estimated scan time 00 00 08 Resolution 4 001 g Range 4000 400 cme View range cm 1 Apply Fit view range to data range Vertical axis Sample 21 Background F Auto baseline correction C Auto background scan 0 Evaluation 10 Accessroy Not equipped 4000 3000 2000 1000 Wavenumber cm 1 C Display amplitude C 16cm 1 Fig 4 8 Monitor Sample dialog The panel on the left of the window shows a real time preview of the spectrum at a resolution of 16 cm with the current energy value in arbitrary units and gain setting displayed on the status bar The current energy value refers to the peak height of the interferogram To display the width of the interferogram check the Display amplitude width check box Measurement parameters can be changed while the spectrum profile is displayed See Section 4 2 8 Parameters and Section 2 2 Measurement for details on the parameters in the Monitor Sample dialog Note In Spectra Manager CFR when instrument parameters are changed the parameter file must be saved before starting
16. JASCO Fourier Transform Infrared Spectrometer FT IR 4000 and 6000 series Operation Manual P N 0302 1899A June 2004 Safety Considerations To ensure operation safety this instrument must be operated correctly and maintained according to a regular schedule Carefully read to fully understand all safety precautions in this manual before operating the instrument Please take a moment to understand what the signal words WARNING CAUTION and Note mean in this manual 1 Safety symbols Instruction manual symbol If the product is marked with this symbol refer to the instrument manuals to protect the instrument against damage WARNING A WARNING indicates a potentially hazardous situation which if not avoided could result in serious injury or even death CAUTION A CAUTION indicates a potentially hazardous situation which if not avoided may result in minor or moderate injury It may also be used to alert against damaging the equipment Do not proceed beyond a WARNING or CAUTION notice until you understand the hazardous conditions and have taken the appropriate steps Note A Note provides additional information to help the operator achieve optimal instrument performance Preface This instruction manual serves as a guide for using this instrument It is intended to instruct first time users on how to properly use the instrument and to serve as a reference for experienced users Before using the instrument read this i
17. arameters E Parameters Advanced al Standard Information Data Optice FFT Timer Source Standard Detector TGs Sample chamber Standard Accesso Not equipped Gain Auto Aperture Auto Scan speed Auto Filter Optical Filter Beam splitter Fig 4 15 Optics Tab Source Specifies the light source to be used If no optional sources have been fitted only Standard can be selected 7 Specifies the detector to use Only TGS can be selected for the standard model i PS IA Standard s_ E Select this when using the standard sample chamber this is the default setting Microscope Select this when using the optional FT IR microscope Secondary sample _ f Select this when using an external sample compartment chamber i Gain Specifies the measurement gain Select Auto for the gain to be automatically set based on the energy reaching the detector Aperture Specifies the instrument aperture for the light source This is normally set to Auto Explanation In Fourier Transform spectrometers the ideal resolution is obtained when the source beams incident on the interferometer beamsplitter are perfectly parallel Since the source aperture of the interferometer is not infinitesimal beams incident on the beamsplitter have 39 some broadening The degree of this broadening affects the resolution of the spectrum obtained Therefore beam broadening must be minimized
18. bar 4 2 8 Parameters This function opens a dialog that can be used to modify all of the instrument measurement parameters The method of changing parameters is identical to the method for the Monitor Background and Monitor Sample dialogs The following describes the Parameters dialog that is used to set the measurement parameters Fig 4 12 Note Parameters can also be accessed by pressing the Parameters button on the toolbar E Parameters Advanced E Elx standard Information Data Optica FFT Timer Number of scan FP Auto Estimated scan time 00 00 41 Resolution Range i cm I View range reo 500 emt Fit view range to data range Vertical axis Sample eT hal Auto baseline correction Settings P Auto background scan Settings Evaluation Settings Accessroy Not equipped Fig 4 12 Standard tab of the Parameters dialog 35 This dialog contains five settings tabs Standard Information Data Optics and FFT Timer The parameters pages can be selected by clicking on the appropriate tab at the top of the window The dialog buttons are described below lt Advance Click this button to change the advance mode E Mode gt if _ lt Basic Mode gt Click this button to change the basic mode 0 000 lt OK gt Click this button to accept newly entered parameters and close the dialog When using the Monitor Sample or Monitor Background window cli
19. btained by spectral measurement JASCO Canvas Prints spectral data in a desired format Administrative Tools Controls administration of user s and or software which refers to the Spectra Measurement Spectra Analysis and JASCO Canvas programs This manual explains how to use the Spectra Measurement program Please also refer to these other manuals Hardware Function Manual Spectrometer operations Spectra Analysis Instruction Manual Analysis of instrument spectra JASCO Canvas Document construction and print templates Administrative tool Administrative tools functions 1 2 Organization This section describes how this manual is organized This manual consists of four chapters and two appendices starting with Chapter 1 Introduction The following describes each chapter 1 Introduction This chapter describes how to read the manual and explains the notation screen configuration and special terms used Read this chapter first 2 Introduction to Spectra Measurement This chapter describes Spectra Measurement If you are not familiar with Windows or spectrometer operation or are a first time user of Spectra Manager please read this chapter for operations ranging from turning on the spectrometer to starting up Windows Spectra Manager and for information about the spectrum measurement and analysis programs 3 Spectra Manager Reference Spectra Manager reference Refer to this section when necessary for further information on
20. cking this button accepts the new parameters and simultaneously starts le measurement lt Caneel gt Click this button to close the dialog without changing any parameters lt Help gt 0 Click this button to display help information lt Open gt Click this button to load an existing pre defined instrument parameters file lt Save gt Click this button to save an instrument parameters file with file extension par Note In Spectra Manager CFR when instrument parameters are changed the parameter file must be saved before closing the Parameter dialog and starting data collection 4 2 8 1 Standard tab The Standard tab shown in Fig 4 12 contains the following settings Number of scans The number of times the sample will be scanned The signal to noise ratio Improves in proportion to the square of the number of scans Auto Check this to automatically set the number of scans based onthe accumulated signal to noise Estimated scan Shows the estimated scan time which is dependent on the number of time scans and the resolution ola The resolution is defined by the maximum width ofa measurable peak Improving the resolution a smaller number increases the measurement time and increases the data point resolution Range Enter values to set the measured data range Increasing the range o increases the number of data points Viewr range eee values to set the view range in the display Fit view
21. contains the following parameters E Parameters Advanced Pilea Standard Information Data Optics FFT Timer Apodization function ero filling Phase correction Filter width Use timer meva 0 min fse Fig 4 16 FFT Timer Tab Apodization function Set the desired apodization function using the drop down menu Explanation Fourier Transform spectrometers theoretically require an infinite optical path difference the interferometer moving mirror traveling to infinity to obtain a spectrum In reality of course a finite interferogram is obtained which undergoes Fourier transformation resulting in regions that contain actual data and regions that do not where the data values are assumed to be O or discontinuous Therefore an ideal spectrum cannot be obtained The apodization function minimizes these differences by eliminating the discontinuous regions Since the resolution of a spectrum obtained this way will change depending on the apodization function most measurements are made using the same apodization function normally set to Cosine Zero filling Sets zero filling ON OFF Explanation Zero filling is the process of extending the range of the measured data in real space by adding zeros to the end of the interferogram This increases the density of data points in frequency space effectively interpolating the spectrum For example doubling the range of measured data by zero filling effectively interp
22. data can be automatically transferred to Spectra Manager program after each measurement if the Send data to spectra analysis check box of the Data tab is checked in the Parameters dialog 4 1 3 Open Parameters This function opens a stored instrument parameters file Fig 4 4 29 Load measurement parameter kin DH MO a Y er Files of type Measurement parameter file par w Fig 4 4 Load measurement parameter dialog 4 1 4 Save Parameters Saves the current instrument parameters to a parameter file Fig 4 5 Save measurement parameter Save O nmo MO O Be Save as lype Measurement parameter file par e Fig 4 5 Save Parameters dialog 4 1 5 Exit Exits the Spectra Measurement program 4 2 Measure Menu This section describes the Measure menu Fig 4 6 which allows the user to start and stop instrument measurement and change measurement parameters Measure Harcel Sample Backeround Monitor sample Monitor backeronnd Parameter Fig 4 6 Measure Menu 30 Measurement Overview The transmittance T spectrum of a sample cannot be directly obtained by an FT IR measurement that measures samples using a single beam method To obtain transmittance T spectra measurements background measurement is performed without before sample measurement The ratio between these measurements is then calculated as follows Single beam spectrum of sample
23. data collection Click the lt OK gt button in the Monitor Sample dialog to start sample measurement When measurement is complete data is transferred to the Spectra Analysis program and the measured spectrum is displayed in a new View provided the Send data to spectra analysis box is checked in the Data page of the Parameters dialog Note This operation can also be started by pressing the m Monitor Sample button on the toolbar 4 2 5 Monitor Background This function allows measurement parameters to be modified as the background spectrum is measured in real time The Monitor Background dialog shown below is displayed Fig 4 9 33 EN Monitor backeround Advanced Standard Information Data Optics FFT Timer Number of scan 8 Fl Auto Estimated scan time 00 00 08 Resolution 4 0cm 1 a Range 4000 1400 cm 1 i View range i cm 1 Fit view range to data range Vertical axis Sample Background Single C Auto baseline correction C Auto background scan C Evaluation 0 Accessroy Not equipped 4000 3000 2000 1000 Wavenumber cm 1 Fig 4 9 Monitor Background The panel on the left of the window shows a real time preview of the spectrum at a resolution of 16 cm with the current energy value in arbitrary units and gain setting displayed on the status bar Measurement parameters can be changed whi
24. dentiality of electronic records by enforcing the use of electronic signatures and other security measures as described in the regulations outlined within 21 CFR Part 11 JASCO Spectra Manager CFR consists of three core modules Administrative Tools and Security Manager modules intrinsic components of the Spectra Manager CFR software and a database which is an external component to the Spectra Manager CFR software In addition there are two broad classes of add on modules the instrument drivers which are spectrometer specific and spectral analysis modules which provide a range of sophisticated analytical and data processing tools These add on modules integrate seamlessly with the four core components of the Spectra Manager system to provide compliance with 21 CFR Part 11 regulations over the entire range of JASCO products Figure 1 1 illustrates the system organization Security Manager Spectra Manager CFR Administrative Tools Fig 1 1 Integrated structure of Spectra Manager CFR All of the security management functions of JASCO Spectra Manager CFR are accessed through the Administrative Tools interface The Security Manager components of the system are not directly accessible by a user and thus the operation of these modules is not described For secure management of data and data records JASCO Spectra Manager CFR has two levels of security system level security and workgroup level security Wh
25. e drop down list Click the to the right of the field to display a list of options Select 4 cm from the list Set the Range to 4000 to 400 cm the mid infrared measurement range of the instrument and check the Fit view range to data range check box Set Background to Single This can be set using the same procedure that was used to change Resolution 17 E Parameters Advanced Selle E Parameters Advanced Sells Standard Information Data Optics FFT Timer Standard Information Data Optics FFT Timer Sample Data type ZT Abs ZA Int w Operator Auto have FP Use auto save Folder Comment a Display information dialog before measurement Division Format Send data Send data to spectra analysis Print out Pl Print out data Template wath Mi Parameters Advanced Sells E Parameters Advanced Standard Information Data FFT Timer Standard Information Data Optics FFT Tiner Sources standard Apodization function Sample chamber Standard Zero filling Phase correction Accessom Not equipped Mertz e Gain Auto E Filter width Aperture Auto Auto e Scan speed Auto Filter Auto Use timer Optical Filter Interval ja mir jo SBC Beam splitter Gen Seve COR Cama Cue Fig 2 15 Information Data Optics and FFT Timer tabs of Parameters dialog 18 6 Select the Information
26. e main menu If any measurement or analysis applications are still running the error message shown in Fig 3 2 is displayed Be sure to exit all measurement and analysis programs before exiting Spectra Manager Note Spectra Manager can also be exited by clicking the close box Spectra Manager Close application to exit A Measurement application is currently running Fig 3 2 Error Message 26 4 Spectra Measurement Reference The spectra measurement program communicates with the spectrometer and performs the actual spectral measurements Toolbar Measurements can be conducted and parameters can be set using buttons on this toolbar Spectra measurement File Measure Settings View Help D Item Info AFT IR 4100typed busy Real time monitor Shows the spectrum ES Model FT IR 4100typeA being measured Set MI Serial No 400961016 p 1234 E E Parameters 5 the disp lay style E Scan Range 4000 400cm 1 from the View E Accumulation 8 E Resolution 40cm 1 menu E VerticalAxis ST E VerticalAxis Single Gain Auto E Aperture Auto E ScanSpeed Auto E Filter Auto E Apodization Cosine2 Ey ZeroFilline ON E Source Standard E Detector TGS 0 E Chamber Standard 3000 2000 1000 400 iQ Accessory No accessory Wavenumber cm 1 PTT TTT TTT background 2 8 00 00 06 remaining Instrument Status bar Information bar Displays total accumulation and Displays informat
27. en a user is registered in JASCO Spectra Manager CFR the user must be assigned to one of four possible System Access Levels Administrators Power Users Users or Limited Users The level of control that a user has over the management functions of the software system 1s determined by the System Access Level assigned to that user Workgroups correspond to actual groupings of users within the organization and may represent such divisions as projects departments or research groups Each workgroup has a set of users instruments accessories and analysis applications associated with it and only users registered with the specific workgroup may access the instruments and applications of that workgroup Within a workgroup users are granted access as either a Manager Analyst or Operator with the privileges to modify instrument and analysis settings and use resources within the workgroup determined by the Workgroup Access Level granted Tables 1 2 and 1 3 outline the different privileges assigned to the different types of user at the system and workgroup level By using a two level security model global security authorization is independent of instrument accessory and application authorization resulting in a highly flexible security system Table 1 2 Privileges assigned to each System Access Level Administrators Limited Users ar an gt Access Level Add a Workgroup OK E A o I Modify Wo T
28. esesactstac nse AD SOWIE yea IN AS waa tes neta a as l A O TVN EO i E EE E A E A O A E E E E E A E E 2 LS 2I CER Pare nan aai 2 1 4 Features of the 21 CFR Part 11 compatible Spectra Manager ssssecccccccsssssececcccossssceeeooo 3 1 5 Scope of Description in This Manual sssccssssssecceccccssssceccocosssssccecossssssecccoosssssseceossssssseeeoso 5 1 6 Components of the Program Screen ssssececccssssececccccsssscececoososssesececossssssecoccssssseseceocsssssseeesso 5 A A eet eae aaa ee eed naan 5 KOZ ANC pease tastes Biceps II O O Mee 6 2 Introduction to Spectra MeasureMent cccccccccccrsrsssssssssssssscsccccccccccccccccccsssssssssscceseeeeeceees 8 A O 9 A EERS D ea ne gacissaeoccaeenesace aacocenaeaacdematey caeanechuasaneeass 9 2 1 2 PC and Windows start up and Setting FT IR properties ccccccooooonnccnnnnnnnononocnnnnnnnnnnnnnos 9 24 3 Spectra Manas er Sta 14 2 2 NICASIO Md id A AA AA AAA A ds 16 2 2 1 Setting of Instrument Measurement Parameters cocccccooonnncnnnnncnnnnnnonnnnnnnnnnononinnnnnnnnnnnnos 16 da DACKO ound me ae ment occ A 20 225 Sample Me as mrem ilasan ido 21 22d SAVIO Wie PECAR 23 3 Spectra Manager Referente ci 25 Sek ANMALYVSIS A AAA o 25 3 2 Measurement Applications iii iii 25 3 9 O 26 4 Spectra Measurement Reference sssssssscccccccccccccccccccccsssssssssssssssssccceeeccccccccessssssses 27 41 Pile Menu cts A aaae 29 A tA VCC A A A A AN 29 Az ANS Se
29. fer to the Windows operation manual for the maximum size of a specific font Effects Select Strikeout or Underline effects by checking these boxes p Sample Shows a sample of the text font being selected Color list box Select a font color here 45 4 4 4 Grid Grid specifies whether to display grid lines on the real time monitor Selecting this menu item displays the following dialog Fig 4 24 Grid Lines Vertical Asis Set As B O Default Ausia Horizontal Axis Vertical Asis Fig 4 24 Grid Lines dialog Main Horizontal Check to display the main grid lines for the X axis Axis i Auxiliary Vertical Check to display the auxiliary grid lines for the Y axis AR Set As Default Check to use the selected settings as the future default settings 4 4 5 Style Style sets the style of spectrum display Selecting this menu item displays the following dialog Fig 4 25 Scale Settines Wavenumber cm Scale Label Cancel Interval 2 Auto Set As O Manual LI Default oo po Number Format Fig 4 25 Scale Setting dialog 46 Axis Select the horizontal or vertical axis setting style using the drop down menu Scale Manual Check to set a user specified scale display style When Manual is checked be sure to also set the scale interval of the main scale or auxiliary scale Number Format Set the number of digits displayed after the decimal
30. fied period of time 1 e when using an instrument purge or following the initiation of a kinetics experiment 4 3 Settings Menu This section describes the Settings menu shown below Fig 4 17 settings auto alle Fig 4 17 Settings Menu 4 3 1 Auto Align The Auto Align function automatically aligns the fixed mirror to the optimum position where maximum energy 1s obtained with the interferometer Fig 4 18 This function should be used when the energy from the interferometer has decreased for any reason such as when the spectrometer is moved has not been used for an extended period of time or when the beam splitter BS of the interferometer has been changed to access another spectral region Refer to the FT IR 6000 hardware manual for details on changing the instrument beam splitter 42 Auto alignment Return to origin 4 50 40 0 20 Position AU Energy CE 1989 Position s 347 1 p 858 MONO BS Ge EBr Origin 3471 p 858 Fig 4 18 Auto Alignment dialog Start Starts auto alignment E Cancel Stops auto alignment esses y Return to origin Moves the fixed mirror to the original coordinates y Scale Setstheview scale of the fixed mirror s position i Close Closes this menu s ses s s sS SSSS 4 4 View Menu This section describes the View menu shown in Fig 4 19 below The View menu is used to set the real time monitor display setting
31. formation for the Spectra Measurement program 48 JASCO Corporation 2967 5 Ishikawa cho Hachioji TOKYO JAPAN Printed in Japan
32. free of charge THIS WARRANTY DOES NOT APPLY TO DEFECTS RESULTING FROM THE FOLLOWING 1 IMPROPER OR INADEQUATE INSTALLATION 2 IMPROPER OR INADEQUATE OPERATION MAINTENANCE ADJUSTMENT OR CALIBRATION 3 UNAUTHORIZED MODIFICATION OR MISUSE 4 USE OF CONSUMABLE PARTS NOT SUPPLIED BY AN AUTHORIZED JASCO DISTRIBUTOR 5 CORROSION DUE TO THE USE OF IMPROPER SOLVENTS SAMPLES OR DUE TO SURROUNDING GASES 6 ACCIDENTS BEYOND JASCO S CONTROL INCLUDING NATURAL DISASTERS This warranty does not cover the consumable parts listed below 1 Tungsten lamp and other light sources 2 Mirrors in the source section and cell windows 3 Fuses batteries glassware chart paper and ink THE WARRANTY FOR ALL PARTS SUPPLIED AND REPAIRS PROVIDED UNDER THIS WARRANTY EXPIRES ON THE WARRANTY EXPIRATION DATE OF THE ORIGINAL PRODUCT FOR INQUIRIES CONCERNING REPAIR SERVICE CONTACT YOUR JASCO DISTRIBUTOR AFTER CONFIRMING THE MODEL NAME AND SERIAL NUMBER OF YOUR INSTRUMENT JASCO Corporation 2967 5 Ishikawa cho Hachioji shi Tokyo 192 8537 JAPAN Notation used in this Manual To make this manual easy to read the following notation is used Notation Measure menu Parameters Command lt OK gt lt Cancel gt Notation for key operations Notation Shift Enter Alt E Shift gt Meaning The names of menus commands parameters text boxes etc are enclosed in brackets This notation applies to menus and comma
33. h item should be set so as to optimize the registered FT IR Except for a multi configuration FT IR you can set only two items the source and detector names Tables 2 1 and 2 2 show the standard settings for the source and the detector Configuration Standard Optics Accessory Category Light source w Curent settings ltem Setting Status Standard Standard Equipped Property Valid range O00 750 warm up time lo ser Auto scan speed Default Fig 2 6 Configuration Optics Light source dialog Table2 1 Setting conditions for FT IR Light source Setting item Value Category Light source Current settings Standard Display Name Standard Valid range 7800 50 cm Warm up time 0 sec Auto scan speed Not available Standard parameters are displayed These parameters can be changed 12 Configuration Standard Uptics Accessory Current settings ltem Setting Status Equipped Detector Mot Equipped Property Display Name TGS Valid range 15000 _ 220 wiam up time ser Auto scan speed 2 Onorr sec Fig 2 7 Configuration Optics Detector dialog Table 2 2 Setting conditions for FT IR Detector Setting items Value Category Detector Current settings Detector 1 Name TGS Valid range 15000 0 cm 7800 0 cm Warm up time 10 sec Auto scan speed 2 0 mm sec The number in parenthesis is for the FT IR 4000 series Configuration Standard Optics Accessory Catego
34. he Logon dialog shown below is displayed Fig 2 10 All users are required to login before using Spectra Manager CFR Following successful login the Spectra Manager main window is displayed Fig 2 11 14 a Spectra Manager Program View Help Instrument Ihs trumer Model Name serial Ho Cond tions Username ao FTAIR 41 00type A FTAR 4100t FTIR 4100 AOQ0961016 Waiting El Spectra Measurement E Gnalysis E JASCO Canvas Spectra Analysis Username Password Fig 2 11 Logon dialog 3 All of the spectrometers that have been setup are shown under the Instrument item in the tree view in the left panel of the Spectra Manager main window Fig 2 10 To begin spectra measurement run the Spectra Measurement program corresponding to the spectrometer you want to use by double clicking the Spectra Measurement icon The spectra measurement program starts and the following screen is displayed Fig 2 12 Cd Spectra measurement File Measure Settings View Help am gad 38 8 x Item Info E idle ES FT IR 4100typeA min Serial No 400961016 5 Parameters E Scan Range 4000 400cm 1 E Accumulation 8 Resolution 40cm 1 VerticalAxis ST VerticalAxis Sinele Gain Auto Aperture Auto ScanSpeed Auto Filter Auto Apodization Cosine2 E ZeroFilline ON Source Standard Detector TGS Chamber Standard iQ Accessory No accessory 3000 2000 1000 400 Wavenumber cm 1
35. he effects of variation in the measurement environment such as CO and H20 vapor concentrations Note 2 When using an accessory be sure to measure the background data with the accessory mounted in the sample chamber 4 2 1 Cancel This function stops the measurement in progress The following dialog appears when valid data has been obtained prior to canceling the spectrum in progress Fig 4 7 31 Measurement stopped Do you want to keep this data lt Cancel gt Click this button to continue spectral measurement Note Measurement can also be stopped by pressing the Fs button on the toolbar Stop Measurement 4 2 2 Sample This function starts sample measurement Be sure to set the necessary parameters as described in 4 2 8 Parameters before measurement When measurement is finished data can be automatically transferred to the Spectra Analysis program and the measured spectrum displayed in a new View window provided the Send data to spectra analysis check box is checked in the Data page of the Parameters dialog instrument parameters Note Sample measurement can also be performed by pressing the EN button on the toolbar Sample measurement 4 2 3 Background This function starts background measurement Be sure to set the necessary parameters as described in 4 2 8 Parameters before measurement Note Background can also be measured by pressing the IB button on the toolbar
36. ifies the line style for the item selected in the Element list i Line Width Specifies the line width for the item selected in the Element list i Sample Displays a sample of the pattern being selected E Set As Default Check to use the changes as the future default settings 44 4 4 3 Font Font specifies the text fonts to use in the real time monitor Selecting this menu item displays the following dialog Fig 4 22 Scale Label Cancel Set As ad Default Vertical Label Orientation Horizontal C Vertical Fig 4 22 Font Setting dialog Item list box Select the item Axis Label Scale Label or Peak Mark to which the font setting is to be applied Select an item and click lt Setting gt to display the following dialog which allows font font style size effects color and script to be adjusted Fig 4 23 Set As default Font style 2 Bold EF Tahoma Bold Italic Terminal O Times New Roman O Trebuchet MS Tunga O Verdana Effects Sample C Strikeout C Underline ISS Color Script Fig 4 23 Font dialog Font list box Select the font to be used using the drop down menu A TT icon designates a TrueType font a printer icon indicates a printer font Size list box Select the text font size With outline fonts such as TrueType all integer numbers up to the maximum size can be designated in addition to the sizes listed in the drop down menu Re
37. ings Send data Send data to spectra analysis Print out Print out data Template Browse wip Data Tab of the Parameters Data type Specifies the data type for the vertical axis Can be one of T Abs R and Int Single sample Single Background or Interferogram The other settings on this tab Auto save Send data and Print out are specified independently of the selected data Le e Y pe Use auto save Check to turn the auto save function ON o o Folder Specifies a a folder for auto Saving of data files E Format Specifies the format for auto save filenames and can be selected from Date amp Number Date No Sample amp Number Sample No Comment amp Number Comment No Sample Comment amp Number Sample Comment No or String amp Number String No String The user specified string of text used when String No J is selected as the filename format E Send data Check to have measured data automatically transferred to the Spectra Analysis program after each measurement i Print out Check the Print out data box to automatically print the measured data after each measurement using a specified Template Use the lt Browse gt button to select a Canvas print template See the JASCO Canvas Program Manual for more details 38 4 2 8 4 Optics tab The Optics tab shown in Fig 4 15 contains the following p
38. ion such as the progress during measurement measurement parameter s and logon name Fig 4 1 Spectra Measurement Program Table 4 1 Tool Bar Buttons File menu MIN Save Data 4 1 1 Save Data Analysis Send 4 1 2 Analysis Send Open Parameters 4 1 3 Open Parameter cal Save Parameters 4 1 4 Save Parameter Measure menu Stop Measurement 4 2 1 Cancel MET Sample Measurement 4 2 2 Sample MT B Background Measurement 4 2 3 Background ME Monitor Sample 4 2 4 Monitor Sample 27 Monitor Background 4 2 5 Monitor Background St Additional Sample Measurement 4 2 6 Sample Measurement Br Additional Background 4 2 6 Background Measurement Measurement Setting menu Scale 4 4 1 Scale E IMEI o Grid 4 4 3 Grid Style 4 4 4 Style 28 4 1 File Menu This section describes the File menu The File menu is used to save spectral data open and save instrument parameter settings and to exit the program Fig 4 2 Eile nave Data Analysis send Open Parameter nave Parameter Exit Fig 4 2 File Menu 4 1 1 Save data Saves measured spectral data to a selected directory on the disk Fig 4 3 Save data Filename pve 040426 Save as type JASCO Standard File jw y Fig 4 3 Save Data Dialog 4 1 2 Analysis send Transfers measured data to the Spectra Analysis program Note The measured
39. le the background spectrum profile is displayed See 4 2 8 Parameters or Section 2 2 Measurement for details on the parameters in the Monitor Background dialog Note In Spectra Manager CFR when instrument parameters are changed the parameter file must be saved before starting data collection Click the lt OK gt button in the Monitor Background dialog to start the background measurement Note This operation can also be started by pressing the E Monitor Background button on the toolbar 4 2 6 Sample Measurement This function is available to perform additional scans after initial sample measurement 1f desired In this case the data type Y axis is the same as the measured data Running additional sample scans improves the S N ratio Additional measurement Additional scans Estimated scan time 00 00 01 Current scans 16 Fig 4 10 Additional Measurement Note This operation can also be executes by pressing the Si button on the toolbar 34 4 2 7 Background Measurement This function is available to perform additional scans after background measurement The data type Y axis is the same as the measured data Running additional sample scans improves the S N ratio Additional measurement Additional scans Estimated scan time 00 00 07 Current scans 16 Fig 4 11 Background Measurement Note This operation can also be executes by pressing the Bt button on the tool
40. measurement system is configured as follows Hardware e Spectrometer e Power supply unit PS 4000 e Personal computer Software e Spectra Manager Ver 2 or Spectra Manager CFR Measurement programs for spectra measurement Analysis programs for spectra analysis Administrative Tools program for administrative functions Refer to Table1 1 Table1 1 Administrative function Administrative function Spectra Manager Ver 2 Registration of spectrophotometers installation of program Spectra Manager CFR Registration of spectrophotometers installation of program Declaring workgroup s users user access level etc 1 1 1 Hardware In this manual the spectrometer refers to the Herschel series FT IR 4000 or 6000 type The personal computer PC is used with the Microsoft Windows operating system 1 1 2 Software Spectra Manager for Windows Spectra Manager means the entire group of measurement and analysis programs for various types of JASCO spectrometers In a narrow sense it means the application programs for communicating with the spectrometer and the spectrum measurement and analysis programs Spectra Manager enables the following 1 Measurement of spectra by spectrometers 2 Startup of analysis programs The standard system of FT IR 4000 and 6000 series includes the following Spectra Measurement Controls the spectrometer and collects spectral data Spectra Analysis Displays processes and prints data o
41. nd for easy identification Shortcut keys used to select menus or commands are underlined The names of command buttons are enclosed in lt gt References made to an item in text are enclosed in double quote marks references made to commands are enclosed in parentheses Meaning Keys are enclosed in square brackets and labeled in bold characters Keys separated by a comma are to be pressed in sequence Keys separated by a plus sign indicate that the second key is to be pressed with the first key held down In this example you need to keep the Shift key held down while you press the gt key Notation for mouse operations Notation Point Click Double click Drag Meaning Place the mouse pointer the arrow cursor on the screen on the item to be selected Press and immediately release the left mouse button Quickly click the left mouse button twice Hold down the left mouse button drag to the desired location then release the button yi Contents Sey CONSIGCTAIIONS iinei or neri EEEE EONS toeoeewaueeeineceeeis i PIS OEE EET E EOT T EO tae ae ii Installati n Reguirem enis A A A iii SIVIC eE cacse eataeuossseerdeces saawias secnesaneaeaueatssutseecacnauia eevee esasaeeatees anes LV DOC ad LV Limited Warranty AAA OI A V Notation used in this MAULE a A AAA EA vi CONTA os vil IM AAA o BN PO O 1 1 1 Measurement System Configuration of Fourier Transform Infrared Spectrometer 1 Mele OWI n ENA E ass
42. nd Serial No of Instrument Model Name FTAR 44 00 e Fig 2 3 Instrument properties dialog The registered instrument name will appear on the right side of the Administrative Tools window Fig 2 4 10 al Administrative Tools Operation View Help m Administrative Tools E gt Instrument E Analysis Application A System Information Instrument Name Model Mame Serial Ho Conditions EF TIR Ooty FT IR 4100 400961016 waiting Registered instrument Fig 2 4 Administrative Tools window Note After performing instrument registration Exit Administrative Tools log off the program and log in again to reset the instrument before performing the following operations 4 After logging into Spectra Manager open the Administrative Tools program and click the Instrument tab to view a dialog similar to Fig 2 4 Select the instrument recently registered and select Properties from the Operation menu or click the right mouse button to obtain the context menu and click on the Properties command Select the Standard tab and verify the Model Display Name and Serial No Configuration standard Optics Accessory Model FT IR 47 Ob ype we Display Name FT AIR 47 Ob yped Serial No 400361016 Version 1 00 00 Build 34 ROM Version 0 00 20 FTAIA 4100 Figure 2 5 Configuration Standard dialog 11 5 Next select the Optics tab Figs 2 6 and 2 7 Eac
43. nstruction manual carefully and make sure you fully understand its contents This manual should be easily accessible to the operator at all times during instrument operation When not using the instrument keep this manual stored in a safe place Should this instruction manual be lost order a replacement from your local JASCO distributor 11 Installation Requirements To ensure operational safety observe the following conditions 1 Do not operate the instrument with voltage fluctuations exceeding 10 of the recommended line voltage Otherwise the instrument may not function properly 2 Frequency or spike noise in the power supply should be nonexistent wherever possible 3 Use a three pronged electrical outlet with a proper grounding circuit 4 The operating temperature range is 17 C 27 C Temperature fluctuations during sample measurement should preferably be within 1 C 5 The operating atmospheric pressure range is 950 1060 hPa 6 The operating humidity should be less than 70 RH If ambient humidity is exceptionally high water vapor may deteriorate optical components No condensation should be visible on the purge case window or other components The instrument should preferably be installed in a place where the ambient humidity is less than 60 RH 7 Avoid strong magnetic fields and sources of high frequency noise The instrument may not function properly when near a strong magnetic field or a high frequenc
44. olates every data point in a spectrum Because interpolated points obtained in this way are based on the measured data the interpolated points are generally closer to the true spectrum than achieved by simple arithmetic interpolation 4 Phase correction Sets the desired phase correction here Explanation Theoretically FTIR interferograms are symmetric about the zero point of the optical path difference However an interferogram measured by an actual FT IR is asymmetric due to minor errors in optical alignments and or electrical circuit characteristics Phase correction 1s performed in which asymmetric results are transformed to a symmetric interferogram using phase information at the zero point of the optical path difference Corrected interferograms are converted to IR spectra using cosign conversion FFT Normally this should be set to the Mertz method of phase correction In the case of Far Infrared measurement lt 100cm in which phase correction is unable to be performed use the Power method Filter width Specified the calculation range of the phase correction Normally this should be set to Auto Use timer Specifies whether the timer is used ON OFF When the Use timer box is checked wait time can be set as follows Interval Wait time is the time from when the lt OK gt button 1s clicked to when the actual measurement begins This can be used as required to obtain spectra of samples that change over a speci
45. rogram functions This chapter describes how to 1 Start up Turn on the spectrometer and start Spectra Manager 2 Measure Measure a polystyrene film 3 Save Save the collected spectrum 4 Exit Exit the Spectra Manager program and turn off communication with the spectrometer The Spectra Manager CFR program complies with the FDA 21 CFR part 11 regulations Therefore three different levels of authority manager analyst and operator can be assigned to users by the Administrative Tools program In Spectra Measurement programs managers and analysts have access to all functionalities In contrast operators cannot modify parameter settings In this manual all functions are explained in the context of a manager or analyst using the program 2 1 Start up This section describes how to turn on the spectrometer and start up the Spectra Manager software 2 1 1 FT IR start up Always turn on the RESUME switch before turning on the POWER switch 1 To start initialization when the RESUME switch is not already on turn on the RESUME switch back of the instrument wait five to ten minutes and then turn on the POWER switch top of the instrument 2 Turn on power to the PC only after the End of initialization beep sounds 3 beeps Note It is strongly recommended that the RESUME switch is left on at all times and the POWER switch used to initialize the spectrometer for spectra collection 2 1 2 PC and Windows start up
46. ry BS Current settings Setting Status Equipped Property Display Mame Ge KBr Valid range 7o00 1350 warm up time sec Auto scan speed Default Fig 2 8 Configuration Optics BS dialog 13 Table 2 3 Setting conditions for FT IR Beam spliter Setting items Value Category BS Current settings BS1 Name Ge KBr Valid range 7800 350 cm Warm up time Not available Auto scan speed Not available Standard parameters are displayed These parameters can be changed Finally register any instrument accessories When the Accessory tag is selected the Accessories dialog appears Fig 2 9 Place the accessory in the sample chamber and click the lt Add gt button to input the accessory name Configuration Standard Optics Accessory Registered accessory Mame Type J Variable ATA 040000103 Variable ATA Property Queces Fig 2 9 Accessory setting dialog Detect the magnet configuration of the accessory and click the lt OK gt button to register the accessory Fig 2 9 Comment can be set to any value maximum of 127 alphanumeric characters 2 1 3 Spectra Manager start up After Windows has initialized and the operating system is ready 1 Double click Spectra Manager on the desktop Note Spectra Manager may also be started by selecting Programs Jasco Spectra Manager from the Start menu instead of using the desktop icon 2 Upon starting Spectra Manager t
47. s Note that these settings also affect the previews shown in the Monitor Sample and Monitor Background windows Wie Scale Pattern Font Grid otele Toolbar Status bar v Infomation bar Customize Toolbar Fig 4 19 View Menu 4 4 1 Scale Scale is used to change the scale of the spectrum display using the following dialog Fig 4 20 43 151407 51407 Pl Auto 0 11562 11562 a E Auto Fig 4 20 Scale dialog X axis scale Enter the horizontal axis scale here When Auto is checked the entered values are ignored and the entire measured region is displayed Y axis scale Enter the vertical axis scale here When Auto is checked the entered values are ignored and the specified horizontal axis range is displayed corresponding to the minimum and maximum spectral range of the collected data 4 4 2 Pattern Pattern is used to set the color and line style of spectra After selecting from the menu the following dialog appears Fig 4 21 Pattern Settines Element Ma Color EERE DD roe as i Til uae Default Line Style sample Gil aa Line Width E EEE Fig 4 21 Pattern Settings dialog Element Select the element for which color and line style are to be changed these include spectrum to spectrum 8 the scale line and auxiliary scale lines Color Specifies the color for the item selected in the Element list i Line Style Spec
48. s setting Spectra Manager CF R IiMeasurement is Anal yeis save with electroni signature Review and Approval signature JASCO Carwas CFR Creation of report Fig 1 2 Operation flow 1 5 Scope of Description in This Manual Spectra Manager is an application program that runs on the Windows operating system requiring a basic knowledge of Windows operations This manual does not explain how to open menus select commands and copy files If you are a first time user of Windows familiarize yourself with the Windows operating system by referring to the operation manuals for the Windows operating system 1 6 Components of the Program Screen In later sections figures showing program screens are used to describe the software operation In this section the names of the components of the program screen are outlined 1 6 1 View window In Spectra Analysis you can open multiple spectrum Views within the main program window Fig 1 3 These views have no explicit menu bar toolbar or status bar but the toolbar buttons and other Spectra Manager components can be utilized for the View windows in the same way as in the program window Eile Edit View Processing Window Other Help Sih SR XY nae 194 NG aA sh ME ie FET Wy BE A RE A A Be oS aS eet polystyr jws pyc jws pyembe jws Contents User jasco Division 0 1 156 Company jasco DO 3000 2000 1000 400 Creation Date 2004 04 09 11 14 wavenumber cm 1 Sample Name Comment Da
49. t first saving the parameter file an error message Fig 2 17 will be displayed Click on Save at the bottom of the Parameter dialog and save the Parameter settings file Fig 2 18 Parameters ES The parameter is modified Please save at a file before ending a setup Fig 2 17 Error message for unsaved parameter settings Save measurement parameter T O f D m Save as type Measurement parameter file par ka Fig 2 18 Save Parameter dialog 19 After saving the instrument parameters the Creation Signature dialog appears Fig 2 19 Creation Signature P Username Administrator Heaton Improvement of S N bl Fig 2 19 Creation Signature dialog After entering a password and selecting a Reason for the Parameter modification click the lt sign gt button In this case select Parameter File Creation for the reason There are several Reasons listed in the drop down menu 2 2 2 Background measurement Because the JASCO Herschel series spectrometer 1s a single beam instrument system a background measurement must be made prior to each sample measurement 1 Confirm that the sample chamber is empty then choose Monitor Background from the Measure menu of the Spectra Measurement program The Monitor Background window is displayed Fig 2 20 Note Clicking the E Monitor Background toolbar icon also starts this function Ba Monitor backeround Advanced Standard Informa
50. ta Information lt 400 278 0 304727 Fig 1 3 Spectra Analysis view window 1 6 2 Dialog Commands and items in menus with an ellipsis at the end open a dialog when clicked Usually the dialog has parameters that must be set The components of dialogs are described below Fig 1 4 In Spectra Analysis 1f you click the View menu a drop down menu appears If you then click Style in the drop down menu the Scale Settings dialog shown as Fig 1 4 appears Drop down list Scale Settmgs Warvenumber cm 1 Scale Label Option buttons Interval The black dot e shows Check box ASE Command button that an option has been 3 selected M Default Group Text box Fig 1 4 Scale Settings dialog Drop down formats Example Number Format Number of digits displayed after the decimal point Meaning Box with an arrow button Here the currently selected parameter is displayed Clicking the arrow displays a parameter list Operation 1 Click the arrow A parameter list is displayed 2 Click an item in the parameter list The desired value is set Group Example Scale Label interval Meaning Group of related selection items enclosed by a frame It includes option buttons and check boxes from which multiple items can be selected simultaneously Option Radio button Example Interval Auto Manual Meaning One of the elements that constitute a group Only one item can be selected at a time The item
51. ticalAxis Single Gain Auto Aperture Auto Scanspeed Auto Filter Auto Apodization Gos ine2 E ZeroF illine Ch Source Standard Detector TGS Chamber Standard iQ Accessory Mo accessory 3000 2000 1000 400 Wavenumber cm 1 OLEO EA backeround 28 00 00 06 remaining Fig 2 21 Spectra Measurement view during background collection A progress bar is displayed in the toolbar while data measurement is in progress When the background measurement is finished sample measurement may begin 2 2 3 Sample measurement To measure the supplied polystyrene film open the sample chamber lid and insert the film into the holder As already mentioned the Herschel series provides a T R or Abs spectrum by measuring a Single spectrum with the sample in the sample compartment and obtains the ratio to the background already measured stored in instrument memory Solvents can also be measured as the background and used as a reference spectrum 1 Select Monitor Sample from the Measure menu of the Spectra Measurement program The Monitor Sample window opens Fig 2 22 21 Note Clicking the ml Monitor Sample tool button also starts this function H Monitor sample Advanced Standard Information Data Optics FFT Timer Number of scan PF Auto Estimated scan time 00 00 08 Resolution Range sono a00 ema Wiew range Fit view range to data range Vertical axis Sample T Background C Au
52. tion Data Optics FFT Timer Number of scan Fl Auto Estimated scan tine 00 00 08 Resolution Range View range Fit view range to data range Vertical axis Sample Puto baseline correction Settings Puto background scan Settings Evaluation Settings Accessroy Not equipped 0 4000 3000 2000 1000 Wavenumber cm 1 Fig 2 20 Monitor Background dialog 20 The spectrum is displayed in the Monitor Background window in real time so measurement parameters may be changed while observing the spectrum change Note that the spectrum preview is always displayed using an instrument resolution of 16 cm and that changing the wavenumber range may not immediately alter the preview After all parameters have been set appropriately proceed with background measurement after saving the instrument Parameter settings Observe the spectrum preview shown in the Monitor Background window and if there are no problems click the lt OK gt button to start actual measurement The following screen is displayed Fig 2 21 Note If you change the parameters in this dialog in Spectra Manager CFR the instrument parameters will need to be saved again with the electronic signature 5pectra measurement File Measure Settings View Help Item E ad FTTR 4100type 4 busy r Model FTAIR 4100type A I Serial No 400961016 Parameters scan Range 4000 400cm 1 Accumulatior 5 Resolution 40cm 1 Vertical fiel wT Ver
53. to baseline correction Settings C Auto background scan Settings Evaluation Settings Accessroy Mot equipped 1000 Wavenumber cm 1 Fig 2 22 Monitor Sample window 2 Select the Information tab in the Monitor Sample dialog and enter Polystyrene as the Sample name The comment can also be changed if desired 3 Verify the preview of the spectrum profile and click the lt OK gt button to start measurement A progress bar appears during measurement as for background measurement 4 When measurement finishes the Spectra Analysis program is started automatically and a window displaying the last spectrum measured opens Fig 2 23 This window is called a View window View Memory 1 is displayed on the title bar because the measured spectrum is not yet saved to disk If the measured spectrum did not automatically appear in the Spectra Analysis window the Send Data check box in the Data parameters tab may not have been checked Select File Send Data from the main menu to transfer the spectrum to the Spectra Analysis program Note If the Spectra Analysis program was already running the window will not be activate once the new spectrum is measured and sent to Spectra Analysis Click Spectra Analysis in the Windows task bar to display the program on the screen and view the collected spectrum 22 m File Edit View Processing Window Other Help eh 28 XY Heed 4d na ae LA Z aA why Rt ie FFT My BE of
54. when high resolution is required in the spectral region by reducing the size of the source aperture Table 4 3 lists the resolution corresponding to each aperture diameter and the standard aperture diameters used for different spectral regions Table 4 3 Standard Aperture Diameters Aperture diameter mm 1 80 2 50 3 50 5 00 7 10 7 10 Scan speed Speed of the interferometer moving mirror This is directly related to the frequency characteristics of the detector Normally this should be set to Auto When the interferometer speed is Auto the actual speed used is determined based on the type of detector as shown in Table 4 4 Table 4 4 Detectors and Scan Interferometer Speeds i al ltd Mel Ll a IRT 30 Scan speed mm sec Note 1 The IRT 3000 and IRT 30 are sold as optional measurement accessories and not as detectors Since these include an MCT detector however they are treated as a type of detector Filter Sets the filter to be applied to signals from the detector The filter frequency is related to interferometer speed When Auto is selected a filter is applied according to the interferometer speed as shown in Table 4 5 Table 4 5 Scan Interferometer Speed and Optimum Filter Frequency FT IR 4000 Series Interferometer speed 2 0 4 0 mm sec Filter Hz FT IR 6000 Series Interferometer speed 0 25 mm sec Ea taje 40 4 2 8 5 FFT Timer tab The FFT Timer tab shown in Fig 4 16
55. which contains a black dot is the one selected Operation To change the item click the desired radio or option button The black dot shows which item is selected Text box Example Main scale auxiliary scale Meaning Box for entering a number or character string When the box is gray this item cannot be changed Operation 1 Click in the box 2 Enter numbers and characters by using the keyboard Check box Example Used as the default Meaning Box for setting an item ON OFF Operation Clicking the box toggles between ON and OFF An x mark or check mark means ON the item is selected Command button Example Meaning Operation lt OK gt lt Cancel gt Button with the name of the operation to be executed A button enclosed with a thick line for example the lt OK gt button will automatically be selected if you press the Enter key Clicking a command button with such as lt Open gt or lt Save gt opens a dialog Click a command button Clicking the lt OK gt button executes the command with the current setting s Clicking the lt Cancel gt button closes the dialog and cancels any settings that have been changed 2 Introduction to Spectra Measurement This chapter describes how to use the Spectra Measurement and Spectra Analysis programs using typical examples Some functions are not described here See the reference chapters later in the manual for full descriptions of all p
56. y source 8 Avoid vibration from vacuum pumps electric motors processing equipment and machine tools 9 Avoid dust and corrosive gas Do not install the instrument in a location where it may be exposed to dust especially in locations exposed to outside air or ventilation outlets that discharge dust particles 10 Ensure that the environmental conditions meet the specifications of the instrument Reliable measurements cannot be made when the operating environment contains gases which have absorption bands in the spectral range of the instrument 11 Do not install the instrument in a location where it may be exposed to direct sunlight 12 Install the instrument in a horizontal and stable position This includes the table or desk upon which the instrument is installed 13 Ensure that no air conditioning or heating unit blows air directly onto the instrument The temperature changes associated with air vents may inhibit stable measurements 14 Install the instrument in a location that ensures adequate space around the instrument for maintenance Note The above conditions do not ensure optimal performance of this instrument 111 Servicing Contact your local JASCO distributor for instrument servicing In addition contact your JASCO distributor before moving the instrument to another location Consumable parts should be ordered according to part number from your local JASCO distributor If a part number is unknown give
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