procedure for operation and calibration of potentiometric titrator

 

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.

5.6.4 Select Sample Data and feed the information.

5.6.5 Select formula and feed details. Use Blank & Normality as obtained in previous runs.

5.6.6 Press METHOD, GO and obtain result at the end of titration.

5.7 Note:

5.7.1 Feed “00” if no Blank is run in the constant for Blank. Run next Sample and so on.

5.8 Cleaning:

5.8.1 Dust must be cleaned by dry moping with lint free cloth.

5.9 Calibration:



5.9.1 Volume dispensing accuracy:

Fill the purified water in reagent reservoir and flush the system thoroughly. Dispense exactrly 2 ml , 5 ml and 10 ml water

into separate pre-weighed containers and weigh the mass of water.

Calculate the volume =weight of water / 0.997

 

Acceptance Criteria = the flow rate should be within + 2 % of the set value.

5.10 Frequency of calibration : Quarterly

 

6.0 REFERENCE

6.1 In House

7.0 FORMATS

: Calibration of Potentiometric Titrator

8.0 ABBREVIATIONS
8.1 QC : Quality Control
8.2 QA : Quality Assurance
8.3 QCA : Quality Control Analytical
8.4 SOP : Standard Operating Procedure

 

 

SOP for testing of ETP water

sop for Calibration and Maintenance of Laboratory Instruments and Equipment

Disposal of Residual Sample or Left Over Material

sop for for Laboratory Incident

standard operating procedure temperature monitoring

sop for drying of silica gel

sop for operation of infrared moisture balance

sop for preparation of mobile phase

sop for treated RO water

sop for Preparation and Issuance of Analysis protocol standard

sop of placebo and impurity stock solutions

sop for disposal of residual sample  

sop for handling of pharmacopoeial changes

sop for procedure for operation of ultrasonic cleaner

difference between UPLC and HPLC

sop for for Emergency Eyewash and Shower

sop for operation and calibration of total organic carbon analyzers

sop for operation of cobb tester

sop for Operation and calibration of atomic absorption spectrophotometer

sop for Operation and calibration of gas liquid chromatograph

sop for operation of humidity oven

sop for operation and calibration of serological water bath

sop for monitoring of drain trap

sop for destruction of analytical samples after testing and control samples

sop for destruction of used chemicals

Sop for Operation of suction pump

sop for Operation and calibration uv cabinet

sop for Operation and calibration of bulk density apparatus

sop for operation and calibration of shore hardness tester

sop for operation of rub proofness tester

sop for monitoring of purified water

sop for Retesting of packaging materials

sop for Retesting and resampling of raw materials

sop for Control of issuance of record of analysis green sheets

sop for Control of computer passwords

sop for sampling of packaging materials PM

sop for sampling of sterile raw material

sop for sampling of intermediates and finished products

sop for operation and calibration of friability test apparatus

sop for approval and rejection of packaging materials

sop for non conformance of RM PM and finished product

sop for collection storage and disposal of control samples

sop for trend analysis of finished products

sop for Chromatographic practices and system suitability

SOP For Good Laboratory Practices

sop for cleaning and operation of sieve shaker

general specification of packing material cartons

sop for Password for Analytical Instrument and LIMS software

sop for Rounding off numerical analytical results

sop for sampling of bulk and finished product

sop for cleaning of spillage material

sop for Handling of Reference Standard

sop for hplc column maintenance and washing

procedure for sampling and handling of bulk sample

STP for borewell generation point (raw water storage tank)

sop for preparation and standardization of 0.1M Zinc Sulphate

Operation &calibration of analytical balance (dhona)

Operation and Calibration Procedure for Disintegration Test apparatus

sop for preparation and standardization of 1 M Hydrochloric Acid

Preparation and standardization of 0.1 M ceric ammonium sulphate solution

sop for preparation and standardization of 0.05 m iodine solution

validation of volumetric solution 0.1m ammonium thiocyanate

handling of reference standard and preparation of working standard

sop for water sampling and analysis

sop for operation for validation of excel worksheets

sop for laboratory cleaning

sop for stability of volumetric solutions

sop for preparation of raw material in process finish product packing material data sheets

sop for handling of hazardous chemicals

sop for handling of glassware and allocation of identification number

sop for operation cleaning and calibration of bursting strength tester

sop for rounding off the analytical test results

procedure for Analyst Qualification

sop for operation and calibration of dissolution Apparatus

procedure for maintenance of desiccators

sop for for hplc column receipt checking id no and regeneration

safety data sheet for laboratory chemicals

procedure for handling of poisonous chemicals

sop for cleaning of sampling devices

sop for calibration procedure of instruments

sop for specification and standard testing raw material packing material and finished product

procedure for operation and calibration of potentiometric titrator

procedure for operating and calibration of digital hardness tester

procedure for disposal of expired chemicals, reagents and solvents

sop for behavior in quality control department

sop for preparation and standardization 0.1M sodium thiosulphate

sop for preparation and standardization 0.1M Disodium Edetate

preparation and standardization 0.1M Sodium Hydroxide Solution

Preparation and standardization of 0.1M Perchloric acid solution

sop for preparation 0.05M edetate disodium

sop for preparation 0.1M silver nitrate

sop for Operation and Calibration of High Performance Liquid Chromatography

sop for UV & Visible Spectrophotometer

procedure for Cleaning of laboratory glassware

Cleaning of Instrument, Instrument bench and surrounding area of Quality

Safety Precaution in Quality Control Department

Operation & Calibration of Analytical Balance

Calibration of Glassware in Quality Control Department

handling of samples received in Quality Control

Cleaning and Operation of Refrigerator

Operation, Cleaning and Calibration of water bath

Operation & Calibration of Refractometer

Operation and Cleaning of Centrifuge Apparatus

cleaning, operation & calibration of Vernier caliper

Calibration of Fourier Transform Infrared Spectrophotometer (FTIR)

Cleaning and operation of Moisture Analyzer

Cleaning & Operation of Vacuum pump in Quality Control Department

Operation and Calibration of Polarimeter

Cleaning and operation of Magnetic Stirrer

Cleaning Operation and Calibration of Melting Point

Operation Cleaning and Calibration of Muffle Furnance in Quality Control Department

procedure of operation and Cleaning of Sonicator

Operation Cleaning & Calibration of pH meter in Quality Control Department

Entry and Exit in Quality Control Department

 

 

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