I OBJECTIVE
To
provide a written procedure regarding the Operation and Calibration of UV/
II SCOPE
This procedure applies to the UV/VIS Spectrometer used in the Quality Control Department.
III RESPONSIBILITY
It is the responsibility of Quality control personnel to follow the procedure as given in this SOP.
IV DOCUMENT REFERENCE(s)
SOPs: a) Policy
on calibration (Current version of QA 00X)
b) Operation
and calibration of
Analytical Balance (Current version of
QC00X)
|
S.No |
Details |
Format No. (Current
version) |
|
1 |
Performance check of UV/VIS spectrophotometer |
QC00X/F01 |
V SCHEDULE:
5.1 The performance of the equipment is once every 3 months.
5.2 If the performance check is failed, inform the service engineer.
5.3 In case of any performance check failure, raise a deviation report, and
investigate the Correctness of
previous results and the releases.
VI PROCEDURE
1.0
Switch “ON” the
instrument, computer, and printer.
1.1 Select the UV/Win lab icon, and double-click on the UV/Win lab icon. A display with methods, data region, Result
window, graph, start, Auto zero and setup options will appear on the screen.
1.2 Double-click on the methods
icon. It consists of different types of
methods, (Scan, TD, WP, Conc. And others) based on their relevant applications.
1.3 Scan: It consists of methods
used for wavelength scans between upper and lower ranges. Select the method double click on it and set the start and stop wavelengths along with data interval
and number of cycles.
1.4 Wavelength program (WP):
It consists of methods used for determining the absorbance. At many
wavelengths. Select the method double-click on it and set the no. of wavelengths along with the no. of cycles.
1.5 Select the method
as per requirement and set the method parameters as mentioned above. Open the method and enter the sample name,
factor, and sample information.
1.6 Click the “START” button. Then “Please insert sample Blank” is
displayed.
1.7 Then fill the cells with a blank solution and insert them in the sample holder.
After completion of blank correction “Please insert next sample” is
displayed. Then fill the sample cell
with the sample solution to be analyzed insert the sample cell into the
sample holder and gently close the compartment door.
1.8 At the end of the analysis, a report will be printed automatically. And document the details in the equipment log.
2.0 Calibration of UV/
2.1 PERFORMANCE
CHECK:
2.1.1 Do the baseline and
background correction as per the model and operating procedure of the UV/ VIS
Spectrometer available in the respective unit.
2.1.2 The following parameters shall be checked
for performance verification.
2.1.3 Control
of wavelengths.
2.1.4 Control
of absorbance.
2.1.5 Limit of stray light.
2.1.6 Wavelength
accuracy.
2.1.7 Resolution.
2.2 CONTROL OF WAVELENGTHS:
2.2.1 Preparation of
Perchloric acid solution: Dilute 8.5 ml of 70 % perchloric acid to
100ml with water.
2.2.2 Preparation of
Holmium perchlorate solution: Weigh accurately about 0.2 g of
Holmium oxide in a 5 ml volumetric flask, dissolves, and dilutes
to volume with a perchloric acid solution. Keep
the solution for about 24 hours for solution
stabilization.
2.2.3
Scan the Holmium perchlorate solution between 200 nm and 600
nm against perchloric acid as blank.
2.2.4
Check the wavelength absorbance at 241.15 nm, 287.15 nm,
361.5 nm, and 536.3 nm and record observed wavelength absorbance in performance
check of UV/VIS Spectrophotometer format.
2.3 CONTROL OF ABSORBANCE:
2.3.1 Preparation of potassium dichromate solution: Dissolve 0.0057 g to 0.0063 g of
Potassium dichromate was previously dried at 130°C for 4 hours,
in 0.005M sulphuric acid and diluted to 100 ml with the same 0.005M sulphuric
acid.
2.3.2 Scan
the potassium dichromate solution between 200 nm and 400 nm against 0.005M
Sulphuric acid as blank.
2.3.3 Check
the wavelength absorbance 235 nm, 257 nm, 313 nm, and 350 nm and calculate the
specific absorbance.
Specific absorbance = ---------------------------------- Wt. of K2Cr2O7 (in grams)
2.3.4 Record
the Specific absorbance in the Performance check of UV/VIS Spectrophotometer
format.
2.4 LIMIT OF STRAY LIGHT:
2.4.1 Preparation
of potassium chloride solution: Dissolve 1.2 g of potassium chloride,
Previously dried at 105°C for 4 hours, and dilute to 100 ml
with water.
2.4.2 Scan
the potassium chloride solution between 190 nm and 220 nm against water as
blank.
2.4.3 Check the absorbance between 198 nm and 202 nm, and record the observation in Performance check of UV/VIS Spectrophotometer format.
2.5 WAVELENGTH ACCURACY:
2.5.1 Take the D2 peak spectrum between 660 nm and 650 nm.
2.6 RESOLUTION:
2.6.1
Preparation of Stock solution: Transfer 0.2 ml of
Toluene into a 10 ml volumetric
The flask containing about 5 ml of n-hexane dissolves and dilutes to volume with n-hexane.
2.6.2 Preparation of 0.02 %v/v solution: Transfer 1.0 ml of the above
stock solution into a 100 ml volumetric flask containing about 50 ml of
n-Hexane, dissolve, and dilute to volume with n-Hexane.
2.6.3 Scan
the solution between the range of 250 and 300 nm against n-Hexane as blank. Measure
the absorbance of the solution maxima at 269 nm and minima at 266 nm.
Resolution = -----------------------------
Absorbance at 266 nm
2.7 ACCEPTANCE CRITERIA:
2.7.1 Control of wavelengths:
Wavelength
Tolerance
241.15 ± 1.0
287.15 ± 1.0
361.5 ±1.0
536.3 ± 3.0
2.7.2 Control of absorbance:
Wavelength Specific absorbance
235 nm 122.9 to 126.2
257 nm 142.8 to 146.2
313 nm 47.0 to 50.3
350 nm 105.6 to 109.0
2.7.3 Limit of stray light:
The absorbance at 200 nm should be more than 2.0
2.7.4 Wavelength accuracy:
The wavelength accuracy should be between 655.8 and 656.4 nm
2.7.5 Resolution:
The ratio of the absorbance should be more than 1.5.
2.8 SCHEDULE:
2.8.1 The performance of the equipment is once in at the time of major spares break down.
2.8.2 If the performance check is failed, inform the service engineer.
2.8.3 In case of any performance check failure, raise a deviation report, and investigate the correctness of previous results and the releases.
2.8.4 Enter the calibration details in the calibration tag and break down details in the Instrument malfunction record.
REFERENCE:
* Instrument Manual of Uv-Visible SpectrophotometerREVISION HISTORY
END O F THE DOCUMENT
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