procedure for operation and calibration of potentiometric titrator

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4 years ago

procedure for operation and calibration of potentiometric titrator

1.0 OBJECTIVE
1.1 To describe a procedure for operation & calibration of Potentiometric Titrator.
2.0 SCOPE
2.1 This procedure is applicable to the Quality control department
3.0 RESPONSIBILITY
3.1 Officer /Executive – QC

4.0 ACCOUNTABILITY

4.1 Head –QC
5.0 PROCEDURE

5.1.1 Decide which titration is to be carried out.

5.1.2 Choose proper electrode and mount it in the vessel. Connect the electrode cable at the backside of the Titrator Unit.

5.1.3 Switch “ON” the Potentiometric Titrator and system.

5.1.4 Attached the printer and put it “ONLINE”.

5.1.5 Checked the parameters of Potentiometric Titrator.

5.2 Titration for Normality:

5.2.1 First find out the Normality of the solution against which further titrations are to be
carried out.

5.2.2 Select Mode such that “NORMALITY” will appear on the display. Press ENTER,
corresponding LED will light up.

5.2.3 Select Method by pressing Method Key till desired Method appears on the display. Press
ENTER, the desired method is now selected.

5.2.4 Mounting the Interchangeable Burette—Press “FILL” to ensure that the Burette Drive Rod is at home position.

Slide the Interchangeable Burette with valve so that it engages
Properly. Keep the Reservoir on the backside of the Syringe.

5.2.5 Insert the filling tube in the Reservoir using adopter. For time being keep the dosing end
of the tube in an empty beaker.

5.2.6 The corresponding massage “RINSING EJECT” & “RINSING FILL” will be displayed
as the rinsing operation is in progress. The entire tubing, valve and syringe will be
finally filled with the solution after rinsing and the Unit will be in ready position.

5.2.7 If titration is to be carried out in pH Mode, using pH Electrode, check the calibration / or
perform the calibration using standard buffers.

5.2.8 Instrument is now ready for operation in the Normality Mode, for standardization of
Normality against Standard.

5.2.9 Weigh suitable quantity of standard substance and transfer it in the titration vessel.

5.2.10 Mount the vessel in its place. See that the Electrode and Stirrer rod are properly dipped.
Insert the dosing side tube within the vessel through capillary holder provided on the
stand.

5.2.11 Select the stirring speed by incrementing or decrementing the arrow keys.

5.2.12 Press AUX FUNCTION and ENTER the DATE / TIME, ML. EJECT STIRRER—
AUTO / CONT., BURETTE FACTOR etc.

5.2.13 Press Formula and feed the details.

5.2.14 Press REPORT and select RESULT REPORT and press ENTER.

5.2.15 Press method and go to initiate the titration.

5.2.16 Progress of titration can be seen on Display, display will show START TIME. After
stirring operation instrument will start dosing rapidly till ONSET or START value is
reached ml. dosing with corresponding mv. or pH will be displayed.

5.2.17 After achieving STOP criteria, titration will be completed and indicated with three
beeps.

5.3 Note:

5.3.1 Observe the Report before pressing CLEAR.

5.3.2 If more than 20 ml. burette volumes are required for titration, the titration will go
in HOLD Mode, carry out FILL operation and will continue titration further. This
facility is available up to 99 ml. volume.

5.4 Titration for Blank:

5.4.1 Take the Reagent Blank in beaker.

5.4.2 Select Blank Mode.

5.4.3 Select Method and its Parameters as used in Normality.

5.4.4 Run titration by pressing METHOD, GO.

5.4.5 Obtain Report.

5.5 Note:

5.5.1 Run Blank only if necessary as per assay.

5.6 Titration for Samples:

5.6.1 Take Sample in beaker.

5.6.2 Select Sample Mode.

5.6.3 Select Method and its Parameters as used in Normality.