OPT1 Operating Procedure for Spectrum Acquisition Rev3
Contents
1. Adjust the overlay graph Y axis values as desired the X axis will scale automatically 14 When the scan is complete a If using Single scan mode a New Data Set dialog box will appear Enter a filename and select your data directory and then click OK b If using Auto scan mode the New Data Set dialog box will not appear Data from each sample will automatically appear in separate filenames in the data window Note At this point the data is only stored in temporary memory but not to the computer disk 15 To save the data to the computer disk a Select Save As from the File pull down menu b If more than one dataset is present in the data window click on the Select button to choose the desired dataset c Select your personal directory in the User Data folder to save the file and enter a filename d Select the desired file type in the Save As Type list i Spectrum files spc to save as a spectrum file for the UVProbe software ii Data Print Table txt to save the data as a text file e Click Save 16 See the UVProbe Tutorial instruction manual pages 2 8 through 2 17 and on line help files for an explanation of the various data manipulation and analysis functions 17 To open a previously saved file for data analysis choose Open from the File pull down menu and select the spc file of interest Page 3 of 4 Revision 3 10 06 2010 M Walters 18 Shut down the system a Unload your sample and close sample2. OPT1 Operating Procedure for Spectrum Acquisition Shimadzu UV 3600 UV Vis NIR Spectrophotometer See Chapter 3 in UV 3600 User s Manual and Chapter 2 in UVProbe Tutorial Manual 1 Log in usage using the SMIF web site 2 Load the appropriate sample holder in the sample compartment a Film holder for solid samples b Cuvette holder for liquid samples c 8 Microcell holder for multiple small volume liquid samples with option of measurements taken at elevated temperature s Be sure to connect the communication cable to the socket on the inside of the UV 3600 sample chamber and the two external cables to the temperature controller Note For measurements of absorption as a function of temperature follow the OPTI Operating Procedure for Temperature Analysis using the 8 Position Micro Multi Cell oll ad Turn on the green power switch located on the side of the UV 3600 instrument Open the UVProbe software on the computer Make sure that no samples are present in the sample chamber and that the sample chamber cover is closed 6 Click on the Connect button The system will go through several initialization checks that will take about 5 minutes When completed click the OK button 7 Verify that Spectrum mode is selected or click on the Spectrum icon button to choose spectrum mode U Probe Spectrum Spectrum Mode selected File Edit View Operations Graph Instrument Tools Window Help a Huje 8 Create a data co
3. chamber cover b Exit the UVProbe software c Turn off the green power switch on the side of the UV 3600 instrument d If the 8 position multi cell holder was used i Turn off the power switch on the back of the temperature controller if used ii Unload the 8 cell holder sample compartment and install the sample holder assembly ili Remove your samples from the 8 cell holder and clean the 8 cell holder using DI water and or alcohol DI water and alcohols can be found in the sample prep lab When clean return the 8 cell holder to the storage box 19 Log out usage using the SMIF web site Page 4 of 4 Revision 3 10 06 2010 M Walters
4. ge slit width or solvent solution b Make sure that no samples are present in the sample chamber and that the sample chamber cover is closed If using the 8 cell holder select an empty cell position using the cell next button Page 2 of 4 Revision 3 10 06 2010 M Walters c Click Baseline on the photometer button bar verify the wavelength range and that the sample chamber cover is closed and then click OK to start the baseline measurement 11 Load the sample into the sample compartment and if desired load a reference into the reference compartment If using the 8 cell holder i Load your samples in the 8 cell holder If using the Auto scan mode start with the front compartment the compartment closest to the red dot and load the samples sequentially The number of samples should match the number of cells selected previously in the method file ii Move to cell position 1 if using Auto scan mode or to the first sample if using Single scan mode iii If desired turn on the temperature controller power switch located on the back of the controller To manually set the desired measurement temperature see pages 2 6 and 2 7 in the Instruction Manual for TMSPC 8 use the front panel of the temperature controller to 1 Press Mode button to select Normal mode 2 Use the Up Down arrows to select the desired temperature 3 Press Start button 12 Click the Start button on the instrument bar to initiate the measurement 13
5. ired slit width typical value is Inm Note 5nm is the maximum value for our instrument 3 Set source lamp to AUTO will automatically switch between the two lamps at preset wavelengths 4 Press the Details button and select stair correction v Inthe Attachments tab window chose None unless the 8 microcell attachment is being used If using the 8 microcell attachment 1 Select 8 microcell and the number of cells to use 2 Load the empty 8 cell holder with the red dot facing the front Make sure that no samples are present in the cells and close the sample chamber cover 3 Click on the Initialize button make sure the sample chamber cover is closed and then click OK It will take a couple of minutes for the holder to initialize 4 When initialization is complete click OK in the Spectrum Method Window You should see buttons at the bottom of the software window that allow you to manually move the holder to the various sample positions 1 Auto Zero EE Baseline o To WL Start sisconnect got Cell gat Cell gone cel 9 Save the data collection method by selecting Save As under the File pull down method a Choose your personal directory to save the file b Enter a name in the filename box c Inthe Save As Type list choose Method File smd and then click Save 10 Perform a baseline correction a A baseline correction should be performed at start up and anytime you change the wavelength ran
6. llection method or load a previously saved method see pages 3 11 to 3 13 in the UV 3600 User s Manual a To load a previously saved method choose Open from the File pull down menu go to your personal directory in the User Data folder select Method File smd as the file type and choose the desired method file b To create a new data collection method F i Click the Method icon to display the spectrum method dialog box ii In the measurement tab window enter 1 2 3 Page 1 of 4 Desired wavelength range start at longer wavelength and end at shorter wavelength Scan speed typical value is medium Sampling interval typical value is Inm or click Auto to have the instrument select an appropriate sampling interval Scan mode a Choose single scan mode when using the cuvette holder or film holder for a single reading across the selected wavelength range or when using the 8 microcell holder Revision 3 10 06 2010 M Walters and you wish to manually measure each sample individually b Choose Auto scan mode if using multiple samples in the 8 microcell holder and you would like all samples measured automatically Then select your data directory and enter a filename for the results iii In the Sample Preparation tab window enter your sample identification information if desired iv In the Instrument Parameters tab window enter 1 Desired measurement mode typically set to absorbance or transmission 2 Des
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