SOP for Calibration of Autotitrator
1.0 OBJECTIVE
To calibrate the equipment for reliable and accurate results.
2.0 SCOPE
This procedure is applicable to the Autotitrator as per operating procedure.
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3.0 RESPONSIBILITY
3.1 Doing: Technical Assistant
3.2 Checking: Executive/ Asst. Manager
4.0 ACCOUNTABILITY
Head of the Department
5.0 PROCEDURE
5.1 Frequency: Once in a 3 month.
5.2 Operate the instrument as per operating procedure.
5.2.1 Take potassium hydrogen phthalate previously dried at 1050C for 2 hrs. as the primary standard for titration.
5.2.2 Set the instrument parameter in MET mode.
5.2.3 Take 5 different accurate weight of primary standard varying from 0.1 to 0.3 gm.
5.2.4 Perform titration using standard 0.1 N Perchloric acid.
5.2.5 Refill the burette after each titration.
5.2.6 Report the results in the given format as Annexure-I.
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5.2.7 Calculate the linearity and correlation coefficient.
5.2.8 Linearity should not be less than 99.0%
5.2.9 Correlation coefficient should not be less than 0.9900%
5.2.10 The performance of the instrument is satisfactory if the obtained Linearity and Correlation Coefficient is within the given limit.
5.3 Calibration of the Burette.
5.3.1 Use 27°C water for calibration.
5.3.2 Mount the burette tip firmly on a stand rod. It must not be moved during the test.
5.3.3 Set dispensing and filling rate of the burette to “max”.
5.3.4 Take a dried beaker and tare the beaker.
5.3.5 Discharge the volume into the beaker and read off the value on the burette.
5.3.6 Press <FILL> Key.
5.3.7 Weigh the dispensed volume.
5.3.8 Repeat 5 discharges of different volume. Select size of the volume in random.
5.3.9 Calculate the V actual dispensed volume.
CALCULATION:
V ACTUAL = MASS X FACTOR OF WATER AT 27°C (1.0045)
V actual = Discharged volume in ml, calculated from the weighing data
MASS = Mass read off on the balance in gm.
5.3.10 Note down the reading in the provident format (Annexure-II).
5.3.11 Maximum relative error of the 20 ml Exchange unit should be 0.15% and the deviation should be +/ - 30 ul.
5.3.12 The performance of burette is satisfactory if the obtained Relative error and deviation should are within the given limit.
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6.0 ABBREVIATION
6.1 °C = Degree centigrade
6.2 % = Percentage
6.3 gm. = Gram
6.4 ml = Millilitre