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.

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.
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.

6.0 ABBREVIATION

6.1 °C = Degree centigrade
6.2 % = Percentage
6.3 gm. = Gram
6.4 ml = Millilitre

ANNEXURE-I Q.A. Department Instrument  Calibration Record

Name of the Instrument          :   AUTO TITRATOR      Make                                      :          Model No                               :

A)  TITRATOR CALIBRATION :

Sr. No. Wt of PHP in mg Burette reading at Ep1 in ml          Limit :    Linearity                            : NLT 99.0%                       Correlation coefficient         : NLT 0.99000%          Remarks                          :          Calibration date                :              Calibration due date          :          Calibrated by                   :          Checked  by                    :

B)  BURETTE CALIBRATION :

V set ml Mass g V actual ml Deviation V actual – V set ml Relative error % Deviation X100 Set ml           Limit :    Relative error   : Not more than 0.15%                        Deviation         : +/ - 30 ul          Remarks                           :         Calibration date                  :             Calibration due date            :         Calibrated by                     :         Checked  by                      :

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