Hitachi F7000 Instruction Manual
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6.1 6 - 1 6. 3-D TIME SCAN 6.1 Flow of Operation This section explains the parameter setting and operating method for 3- D time scan. Measurement proceeds along the following flow. Fig. 6-1 Operational Flow (3-D time scan) Click button and set your analytical conditions. • Scan range • Data mode • Scan speed, etc. Click button. • Sample name • Auto File • File name, etc. Set a sample. Click button to execute wavelength scan. • Spectrum tracing • Peak detection Click button. Measurement result will be displayed in a report format. Start Method setting (See 6.2.) Sample name/ comment input (See 6.3.) Measurement (See 6.4.) Data processing (See Section 7.) Result output in report (See 6.9.) End
6.2 Creating an Analysis Method 6 - 2 6.2 Creating an Analysis Method Set the analytical conditions (method) prior to measurement. (1) Click the button on the Measurement toolbar. The window in Fig. 6-2 appears. (Or select the Method command from the Edit menu.) Fig. 6-2 Analysis Method (2) On the Analysis Method window, analytical conditions for the 3-D time scan mode can be set. The following tabs are provided on this window. These tabs are detailed on the subsequent pages. • General • Instrument • Monitor • Processing • Report
6.2.1 6 - 3 The parameters shown in Fig. 6-3 are provided at the General tab. For the settable range of each parameter, refer to Appendix G. Fig. 6-3 General Tab 1 Measurement (mode) A measurement mode is selectable. Here, select “3-D Time scan.” For Wavelength scan, Time scan, Photometry and 3-D Scan, refer to Sections 2, 3, 4 and 5, respectively. 2 Operator Enter an operator name. 3 Instrument The name of the connected instrument is indicated. 4 Sampling - Standard Indicates that samples are to be exchanged manually. 5 Comments Enter a description or notes on measuring conditions. 6.2.1 General Tab 1 2 3 4 5 6 7 8
6.2 Creating an Analysis Method 6 - 4 6 Load Click this button to read out saved analytical conditions. Upon clicking, the file opening window appears. So, select an analytical condition file. 7 Save When you click this button after setting the parameters, the analytical conditions can be saved by overwriting. In case of a new analysis method, clicking this button displays the “Save As” window. You must enter a file name for saving in this window. 8 Save As Click this button for renaming the set conditions for saving. The “Save As” window appears, so enter a file name.
6.2.2 6 - 5 The window shown below is based on that 3-D Time scan is specified for Measurement at the General tab. When you click the Instrument tab, the window in Fig. 6-4 appears. For the settable range of each parameter, refer to Appendix G. Fig. 6-4 Instrument Tab 1 Scan mode Select a scan mode here. In case of Synchronous, the abscissa of the graph stands for excitation wavelength. The unit indication of the abscissa becomes ‘EX/EM (nm).’ 2 Data mode Select a data mode. The Phosphorescence mode is for acquiring only phosphorescence after extinction of excitation beam while turning a chopper on the excitation side. 3 Chopping speed Select a chopping speed. Setting is allowed when Phosphorescence is selected for Data mode. The Phosphorescence mode is for acquiring only phosphorescence after extinction of excitation beam while turning a chopper on the excitation side. An increase in chopping speed makes the chopper turns faster. 6.2.2 Instrument Tab 3 4 5 6 7 2 1 8 9 21 10 13 14 15 16 17 12 11 18 19 20
6.2 Creating an Analysis Method 6 - 6 4 EM WL For the Excitation scan mode, enter the fixed wavelength on the emission side . For the Synchronous scan mode, enter the start wavelength on the emission side. 5 EX Start WL This is the start wavelength on the excitation side in wavelength scan. Enter the shorter wavelength side of measuring wavelength range. 6 EX End WL This is the end wavelength on the excitation side in wavelength scan. Enter the longer wavelength side of measuring wavelength range. 7 EX WL For the Emission scan mode, enter the fixed wavelength on the excitation side. 8 EM Start WL This is the start wavelength on the emission side in wavelength scan. Enter the shorter wavelength side of measuring wavelength range. 9 EM End WL This is the end wavelength on the emission side in wavelength scan. Enter the longer wavelength side of measuring wavelength range. 10 Scan speed Set a scan speed. 11 EX Slit Select a slit width on the excitation side. 12 EM Slit Select a slit width on the emission side. 13 PMT Voltage A function for controlling the voltage of the photomultiplier detector (photomultiplier tube). As a reference, changing from 400 V to 700 V increases the data value about two digits and changing from 700 V to 950 V increases it about 1 digit. When a check mark is put for PMT Voltage 0-1000V, the photomultiplier voltage is settable within a range from 0 to 1000 V. 14 PMT Voltage 0-1000V When a check mark is put in this box, the photomultiplier voltage is settable within a range from 0 to 1000 V.
6.2.2 6 - 7 15 Response When “Auto” is selected, response will be set automatically depending on scan speed. Select “Auto” usually. 16 Corrected spectra A function for determining the spectrum inherent to a sample by correcting the photometer wavelength characteristic using the saved instrument parameters, following measurement with the instrument parameters for photometer control. If there are no instrument parameters for the wavelength range to be measured, only the wavelength range that allows correction is scanned. And if there is no wavelength area measurable, an error will occur. The Instrument Response command is provided in the Utility menu for operating this function. When this setting is at ON, “Corrected spectra” appears on the monitor window. (See Fig. 1-43 in 1.6.) 17 Shutter control The shutter can automatically be closed in other than measurement for slowing down sample deterioration due to the energy of excitation beam and opened when measurement starts. 18 Replicates Set the number of repeat measurements. 19 Cycle time Set a repetition interval. 20 Range of corrected spectra Spectrum correction range is indicated. 21 Prediction measurement time The predicted measurement time is indicated. After change of a parameter such as scan speed, click the Update button. The predicted value will then be updated.
6.2 Creating an Analysis Method 6 - 8 When selecting the Monitor tab, the window in Fig. 6-5 appears. For the settable range of each parameter, refer to Appendix G. Fig. 6-5 Monitor Tab Assign the following parameters. 1 Y-Axis Max (maximum) Enter a maximum value for Y-axis on the monitor window. 2 Y-Axis Min (minimum) Enter a minimum value for Y-axis on the monitor window. 3 Contour interval Function for setting intervals of drawing contour lines. 4 Open data processing window after data acquisition Select whether or not to conduct data processing after sample measurement. When selected (check mark is applied), an icon (as shown in ) is displayed for the data processing window at the end of measurement. And by opening this icon, data processing such as peak detection is available. 6.2.3 Monitor Tab 2 1 4 5 3
6.2.3 6 - 9 NOTE: When the remaining memory capacity of PC in operation is very small (system resource is less than 20%), the data processing window will not open even if this item is turned ON. Either close the presently opened data processing window or restart the FL Solutions program. 5 Print report after data acquisition Select whether or not to print a report after sample measurement. When selected (check mark is applied), printing will be made automatically after measurement. The items set at the Report tab will be printed. When this item is not selected, data processing is allowed by reading out a file via [File] - [Open].
6.2 Creating an Analysis Method 6 - 10 On selection of the Processing tab, the window in Fig. 6-6 will be displayed. For the settable range of each parameter, refer to Appendix G. Fig. 6-6 Processing Tab 1 Peak Finding: Integration method Select an integration method for the peaks to be displayed in the data processing window. 2 Threshold Set a detection limit for the photometric value axis of peak and valley. Peaks or valleys below the setting will not be detected. 3 Sensitivity Select the number of data points in the horizontal axis direction (abscissa). For detecting sharp peaks, select a sensitivity value of “1.” Or select “8” for detecting broad peaks. 6.2.4 Processing Tab 1 3 2