1.0 PURPOSE
2.1 To define the procedure for Operation, Cleaning and Calibration of UV-Visible Spectrophotometer.
2.0 SCOPE
2.1 This standard operating procedure provides the procedure for Operation, Cleaning and Calibration of UV-Visible Spectrophotometer in quality control department.
3.0 RESPONSIBILITY
3.1 Quality Control Person shall be responsible for :
3.1.1 To initiate and preparation of standard operating procedure.
3.1.2 Training and Monitoring of standard operating procedure.
3.1.3 Final report preparation of Operation, Cleaning and Calibration of UV-Visible Spectrophotometer.
3.2 Quality Control Head shall be responsible for:
3.2.1 To confirm the content, correctness and detailing of standard operating procedure.
3.2.2 To ensure the training of this standard operating procedure to all concerned department persons.
3.2.3 To ensure the implementation of the standard operating procedure after training.
3.2.4 It is final responsibility of Quality Control Head to maintain the Operation, Cleaning & Calibration of UV-Visible Spectrophotometer.
3.3 Quality Assurance Person shall be responsible for :
3.3.1 To check the standard operating procedure.
3.4 QA Head shall be responsible for :
3.4.1 To approve new or revised standard operating procedure.
3.4.2 To ensure the implementation of the defined system.
4.0 DISTRIBUTION
4.1 Quality Control
5.0 DEFINITION (S)& ABBREVIATION(S)
5.1 Definitions :
5.1.1 Not Applicable
5.2 Abbreviations :
5.2.1 QC D : Quality Control Department
5.2.2 UVS : Ultra Violet Spectrophotometer
5.2.3 KCl : Potassium Chloride
5.2.4 H2SO4 : Sulphuric acid
5.2.5 ppm : Parts per million
5.2.6 Max. : Maximum
5.2.7 Min. : Minimum
5.2.8 K2Cr2O7 : Potassium Dichromate
5.2.9 LCD : Liquid Crystal Display
6.0 PROCEDURE
6.1 Operation:
6.1.1 This operation is applicable for the instrument mention below:
6.1.2 Name of Instrument- UV-Visible Spectrophotometer
6.1.3 Instrument ID - QCD/UVS/011
6.1.4 Make - SHIMADZU
6.1.5 Model No - UV-1800
6.1.6 Connect the instrument with the power supply and switch ON and switch on the computer.
6.1.7 Double click on UV-Probe ver. 2.52 icon on the computer screen, wait for the software initialization.
6.1.8 Wait for initialization operation, after initialization LCD will display the main windowand after initialization display the login window enter the User and password Display the Mode menu window for the operation by PC Control.
6.1.9
After
initialization display the login window enter the User ID and password than
click on ‘OK’
6.1.10 Press on the instrument enter key and then press button ‘F4’ for PC Control.
6.1.11 Display standard tool bar for selection of appropriate function such as Photometric, Spectrum, Kinetics modules, Report Generator and save file icon. Instruments connect with click on the Connect icon.
6.1.12 Photometric Mode- Click on the photometric mode for takes absorbance and select the Photometric method which is denoted by ‘M’.
6.1.13 Select the particular wavelength and ‘Add’ then select Next and the select multipoint/ single wavelength/Raw data and wavelength setting. ‘STD’ and ‘SMP’, repetition number. Fill the file name, title, analyst name, and comment save file in selected folder like product or category wise (RM, IP and FG etc).
6.1.14 Before take the reading check the all method parameter and put on the cuvette cell in Instrument compartment select ‘Auto Zero’ for blank correction then fill the conc. value. Select ‘Reading’ icon, take the absorbance all samples stepwise Such as Standard, Sample etc.
6.1.15 Select the Report Format for print out and save data.
6.1.16 Spectrum Mode-Click on the spectrum mode for display of spectrum method status icons.
6.1.17 To set the wavelength range, enter in the start box maximum wavelength and in end box minimum wavelengths. Select measuring mode in absorbance or transmittance
6.1.18 Select scan speed Medium in list display .Set the sampling intervals 1.0 in Spectrum Method. Check all parameter in spectrum method, and then correct ‘Baseline’ correction by blank. Take the standard and sample graph stepwise by click on Start icon. After completion scanning select the ‘Active’ icon for view of spectrum graph. Move cursor with right click on graph selects labeling of product and particular lambda (nm).
6.1.19 Select the Report Format for print out and when saving a spectrum file in each data set as per requirement in Peak area table , Point pick table, Peak pick table data file.
6.1.20 Kinetics Method: Click on the kinetic mode for takes absorbance and select the kinetic method which is denoted by ‘M’.
6.1.21
Click on auto timing mode to set the
total measurement time.
6.1.22
Set the wavelength and total time
for single wavelength.
6.1.23
Click the instrument parameter tab.
Select absorbance for measuring mode.
6.1.24
After the auto zero take the sample
absorbance, by pressing of Start icon. Ensure the
time axis X-axis and Y-axis.
6.2
Cleaning Of Instrument :
6.2.1
Instrument should be free from dust
and moisture every time.
6.2.2
Cuvette should be cleaned and dried
after every analysis.
6.2.3
Do not Unnecessary on or off
instrument because it losses lamp energy.
6.2.4
After cleaning of cell with water,
rinse by methanol.
6.2.5
Dry the cell with help of tissue
paper.
6.3
Calibration of Instrument :
6.3.1
The
UV Spectrophotometer shall be calibrated for following parameters:
6.3.1.1 Maintenance
of Instrument
6.3.1.1.1
Press key Mainte.
6.3.1.1.2
Now
Display will show maintenance parameter.
6.3.1.1.3
Press Numeric key
(2) to start Instrument base line correction.
6.3.1.1.4
Select
key and press enter.
6.3.1.1.5
Now
base line correction starts. It will take 17 minutes to complete.
6.3.1.1.6
After
base line correction, press numeric key (4) to start ‘λ’ recalibration
6.3.1.1.7 
Select key and press enter.
6.3.1.1.8
Now
‘ λ’ calibration is start, it will take
1 minute to complete.
6.3.1.2
Control of
Absorbance
6.3.1.2.1
Preparation of
solutions :
0.005M H2SO4 Solution:
Dilute 5.4 ml of concentrated sulphuric acid to 1000 ml with purified water (Solution-A)
Further dilute
100 of Solution A to 2000 ml with purified water to give a 0.005M sulphuric
acid solution (Solution B).
Potassium dichromate Solution
(60ppm) :
Dry potassium
dichromate at 130 °C up to constant weight. Weigh 57.0 mg to 63.0 mg of K2Cr2O7
and dissolve in sufficient 0.005M sulphuric acid solution to produce 1000 ml.
Potassium dichromate Solution
(600ppm):
Dry potassium
dichromate at 130 °C up to constant weight. Weigh 57.0 mg to 63.0 mg of K2Cr2O7
and dissolve in sufficient 0.005M sulphuric acid solution to produce 100 ml.
6.3.1.2.2
Enter
the following parameter in the instrument:
Measuring Mode Absorbance
Wavelength
Range 400 nm to 200 nm
Scan Speed Medium
6.3.1.2.3
Fill
the potassium dichromate solution (60ppm) into the sample cell of
spectrophotometer and place in the sample compartment. Take absorbance at 235,
257, 313 & 350nm using 0.005M sulphuric solution as blank.
6.3.1.2.4
Calculate
the specific absorbance value of 1-cm cell at 235,257,313 & 350nm. The
tolerance limits of the specific absorbance for each wave length are given in
Table-I.
6.3.1.2.5
Fill
the potassium dichromate solution (600ppm) into the sample cell of
spectrophotometer and place in the sample compartment. Take absorbance at 430nm
using 0.005M sulphuric solution as blank.
6.3.1.2.6
Calculate
the specific absorbance value of 1-cm cell at 430nm. The tolerance limits of
the specific absorbance for each wave length are given in Table-I.
6.3.1.2.7
Fill
the record in calibration format, Format
No.: QC/CC/I-002-F02.
6.3.1.3
Resolution Power :
6.3.1.3.1 Prepare 0.02 % v/v solution of toluene in hexane :
Dilute
1 ml of toluene to 100 ml with Hexane, further dilute 1 ml of above solution to
50 ml with Hexane.
6.3.1.3.2
Enter
the following parameter in the instrument:
Measuring Mode Absorbance
Wavelength
Range 275 nm to 260 nm
Scan Speed Medium
6.3.1.3.3 Record
the Spectrum in the range 260 nm to 275 nm of the 0.02 % v/v Toluene solution
using Hexane in reference cell.
6.3.1.3.4 Read
the absorbance at the maximum at about 269 nm to that at the minimum at about 266
nm and the ratio of absorbance should not be less than 1.5.
6.3.1.3.5 Fill the record in
calibration format, Format No QC/CC/I-002-F02.
6.3.1.4
Limits of Stray
Light :
6.3.1.4.1
Prepare
1.2 % w/v solution of KCl in water.
6.3.1.4.2 Fill
the above potassium chloride solution in the sample cell of path length of 1 cm
and measure the absorbance at 200 nm using purified water as blank. The
absorbance should be greater than 2.0 AU.
6.3.1.4.3 Fill
the record in calibration format, Format
No.: DII/QC/CC/I-002-F02.
6.3.1.5
Control
of Wavelength :
6.3.1.5.1 Control
of wavelength shall be checked with Holmium Perchlorate solution or
alternatively Holmium Oxide filter shall be used.
6.3.1.5.2 Prepare
4 % w/v solution of holmium oxide in
1.4M perchloric acid.
1.4 M HClO4 (1.4 M perchloric acid )
Dilute 11.5 ml of perchloric acid (70
% w/w) to 100 ml with water.
4 % w/v solution of holmium oxide
Dissolve 0.4 g of Holmium oxide in 5
ml of 1.4 M perchloric acid with the aid of heating on a water-bath, cool and
dilute to 10 ml with the same solvent.
6.3.1.5.3 Enter
the following parameter in the instrument :
Measuring
Mode Absorbance
Wavelength
Range 600 nm to 200 nm
Scan Speed Medium
6.3.1.5.4 Fill
the above solution in the sample cell of spectrophotometer and place in sample
compartment.
6.3.1.5.5 Start
the scanning, and take the printout.
6.3.1.5.6 Check
the maxima. It should appear at 241.15 (±1nm), 287.15 (±1nm), 361.5 (±1nm) and
536.3nm (±3nm).
6.3.1.5.7 Fill
the record in calibration format, Format
No.: QC/CC/I-004.
6.3.2
All chemicals /reagents use in the
calibration should be AR Grade /Spectroscopy.
6.4
Compare the results with acceptance
criteria; Fill the calibration status in tag on the instrument.
6.5
Report any discrepancy observed
during calibration of the instrument to Head QC or his authorized
representative, and notify the defect to Engineering Department / Service
Engineer to rectify the defect. Affix ‘Under Maintenance’ label on the
instrument.
6.6
Frequency: Calibration frequency is quarterly.
6.7
TABLE
1 - (Acceptance criteria for calibration of UV-VIS Spectrophotometer)
8.0
REFERENCE(S) &
FORMAT(S)
8.1
Reference :
8.1.1 Manufacturer instructions / Manual,
Indian pharmacopoeia.
8.2 Formats
:
8.2.1 Format I : Log Book for UV-Visible Spectrophotometer
8.2.2 Format II : Calibration
Record of UV-Visible Spectrophotometer
9.0 REVISION HISTORY
9.1
Refer SOP for SOP Format X
(Format for Document History sheet) as attached.
END OF THE DOCUMENT
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