4.9 Periodic Inspection of UV Absorbance
4.9.2 Wavelength Accuracy Test
Inspection Procedure
1 Press the [CE] key.
The initial screen is displayed.
2 Press the [
→] (right arrow) key and position the cursor at [VP]. Then press the [
→] (right arrow) key.
The VP function group is displayed.
3 Press the [
↑] or [
↓] (up/down arrow) key to position the cursor at [VALIDATION]
and then press the [
→] (right arrow) key.
Functions in the [VALIDATION] group are displayed.
4 Press the [
↑] or [
↓] (up/down arrow) key to display [CAFFEINE CHECK].
The screens shown on the right are alternately displayed.
5 Use a syringe to fill the flow cell with caffeine and then press [Enter].
The window on the right is displayed for about 30 seconds.
Then the caffeine is measured.
When the caffeine measurement is finished, the screens shown on above are alternately displayed.
Next, the background is measured.
4.9 Periodic Inspection of UV Absorbance Detectors
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6 Use a syringe to fill the flow cell with purified water and then press [Enter].
The window on the right is displayed for about 30 seconds.
Then the background is measured.
7 If the wavelength check result was good and wavelength accuracy are confirmed, the screen shown to the right is displayed.
If wavelength check result was not good, the screen on the right is displayed. If [CHECK NO GOOD] is displayed, follow the instructions in " Corrective Measures if Wavelength Accuracy Does Not Satisfy Control Criteria".
8 Then the wavelength deviation for 205 nm, 245 nm, and 273 nm are displayed.
Control
Criteria ±2 nm of all three wavelengths
Inspection Procedure (2) Inspecting with Manual Wavelength Change.
Using this method, wavelength can also be checked based on theophylline. For more details, contact your Shimadzu representative.
Scope of Inspection
Aqueous caffeine solution is used to manually check wavelength accuracy at 205 nm, 245 nm, and 273 nm.
Preparation for Inspection
• Switch the instrument power ON and fill the flow cell with water.
• If the simultaneous dual wavelength measurement mode is specified, change it to the single wavelength measurement mode.
• Set absorbance to zero at the 350 nm wavelength setting.
• Change the setting of [Z WAVE] in the [CALIBRATION] group to "1".
SPD-40 CL Instruction Manual 3.7.6 Calibration Support Group
After inspection, be sure to reset the [Z WAVE] setting to "0".
Inspection Procedure
1 Confirm that absorbance has stabilized and then, with the flow cell filled with water, set the wavelength to 200 nm and record the absorbance at that point.
2 Similarly, record the absorbance at each wavelength as the wavelength is changed in 1-nm steps from 200 nm to 210 nm.
3 Fill the cell with aqueous caffeine solution (10 mg/L).
4 Record the absorbance at each wavelength as the wavelength is changed in 1-nm steps from 200 nm to 210 nm.
5 Determine the wavelength where maximum absorbance occurs, by calculating the difference between the absorbance of aqueous caffeine solution and the absorbance of water at each wavelength.
6 Record how much the values deviate from the specified value.
7 Repeat the same procedure to manually check and record the absorbance at wavelengths between 240 nm and 250 nm and between 268 nm and 278 nm.
For measurements from 240 nm to 250 nm, find the wavelength at which the absorbance is minimum and record the deviation from the set value.
• If the deviation is more than ±2 nm, then follow the instructions in " Corrective Measures if Wavelength Accuracy Does Not Satisfy Control Criteria".
• After inspection, be sure to reset the [Z WAVE] setting to "0".
4.9 Periodic Inspection of UV Absorbance Detectors
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Inspection Procedure (3) Inspecting with Wavelength Scan Function (Using the LabSolutions)
Using this method, wavelength can also be checked based on theophylline. For more details, contact your Shimadzu representative.
Scope of Inspection
Aqueous caffeine solution is used to check wavelength accuracy at 205 nm, 245 nm, and 273 nm with wavelength scan function .
Confirm that the absorbance peaks for caffeine are within the 205.0 nm ± 2 nm, 245.0 nm ± 2 nm, and 273.0 nm ± 2 nm ranges, respectively.
Preparation for Inspection
• Switch the instrument power ON and fill the flow cell with water.
• Launch the workstation (LabSolutions).
• If the simultaneous dual wavelength measurement mode is specified, change it to the single wavelength measurement mode.
• Turn off the pump.
Inspection Procedure
1 Click the spectral scan on the LabSolutions [Instrument Control] toolbar.
2 Set the starting wavelength to 200 nm and the ending wavelength to 280 nm.
Use the scanning step with the default setting of 1 nm.
3 Confirm that absorbance has stabilized and then, with the flow cell filled with water, perform a scan. Register the results as the base level.
4 Fill the cell with aqueous caffeine solution (10 mg/L).
5 Confirm that the absorbance level has stabilized and then perform a scan.
6 In the results, identify the minimum and maximum absorbance values near 205 nm, 245 nm, and 273 nm. Record how far wavelengths deviate from the setting values.
If the deviation is more than ±2 nm, then follow the instructions in " Corrective Measures if Wavelength Accuracy Does Not Satisfy Control Criteria".
n
Corrective Measures if Wavelength Accuracy Does Not Satisfy Control Criteria
Cause Corrective Actions
The flow cell contains bubbles.
Implement measures to eliminate the bubbles.
4.3 Flow Cell Inspection/Cleaning in the SPD-40 CL Instruction Manual
The flow cell contains a liquid that absorbs light.
Purge the flow cell with either purified water, methanol, or acetonitrile.
The flow cell is contaminated.
Rinse the cell.
4.3 Flow Cell Inspection/Cleaning in the SPD-40 CL Instruction Manual
Wavelength calibration was not performed properly.
Calibrate wavelengths.
4.8 Performing Wavelength Calibration in the SPD-40 CL Instruction Manual
Optical system problem (degradation of mirrors, window, etc.).
Perform optical system maintenance. (Contact a Shimadzu representative. )
4.9 Periodic Inspection of UV Absorbance Detectors