SOP for Calibration of Potentiometric Titrator (Metrohm)

1.0 OBJECTIVE

To check that the instrument performs satisfactorily and gives accurate and reproducible results.

2.0 SCOPE

This SOP is applicable for operation and Calibration Auto titrator Metrohm.

3.0 RESPONSIBILITY

Officer/ Executive - Quality Control

4.0 ACCOUNTABILITY

Manager - Quality Control

5.0 PROCEDURE

5.1 Operation

5.1.1 Check that the power supply to the instrument is switched "OFF" before cleaning.
5.1.2 Clean the instrument with a clean dry cloth every day.
5.1.3 Check that the instrument is connected to the stabilized power supply.
5.1.4 Switch "ON" the main power supply switch of instrument and printer.
5.1.5 On desktop double-click on “tiamo1.2” Icon. Screen shows “tiamo1.2” it will initialize program and devices.
5.1.6 Preparation message appears. Press “OK” to all.
5.1.7 Four option will appear on the left side screen show. Workplace; Database, Method, Configuration.
5.1.8 Click on workplace option. Four windows are seen. Run; Method; Report; Live Display 1
5.1.9 Click on “Tools/ manual Control”. Select Dosing device and go to preparation function. Press Start. The burette tip should point in a waste beaker. This step rinses the burette and removes any possible air bubble.
5.1.10 Before doing Titration Check Electrode Input, Dosing Device, & Stirrer to be used in the Method (selected for Titration)
5.1.11 In Workplace on RUN window click on METHOD to select the appropriate Method
5.1.12 Weigh the Standard / Sample in a Beaker and add the appropriate solvent, place it on the magnetic stirrer to be used & put the magnetic paddle into it. Dip appropriate Electrode assembly along with Dispensing Tip in the Beaker just above the Stirrer Bar.
5.1.13 Enter Sample Name, Batch No., LNB Ref Analyst Name & Sample size ( For Assay also enter the Equivalent Weight also)
5.1.14 Click on START a window with sample detail will appear on the Screen Press OK.
5.1.15 Titration proceeds. After the titration is over burette goes for filling and then report appears in the report window.
5.1.16 As the experiment is over, remove the beaker, wash the electrode properly.
5.1.17 Record the observations in usage log book (Annexure - II)

5.2 Report Print

5.2.1 Click on “Data Base”
5.2.2 Open the appropriate Data Base
5.2.3 Select the report to be print
5.2.4 Click on “Tool’s on the menu
5.2.5 Open “Report Templates”
5.2.6 For Report of “Blank” determination select Titer Template
5.2.7 For Report of “Titer” Determination select Titer / Titer with statistics
5.2.8 For “Short Report” of Assay Determination Select 1 Template & for “Detail Report” of Assay Determination Select 2 Template.
5.2.9 After selecting appropriate Template Click on “Open”.
5.2.10 Click on “PDF” a PDF file will be created, save it or take print out.

5.3 Calibration

5.3.1 Go to “Tools” on menu
5.3.2 Click on “Manual Control”
5.3.3 Select Dosing Device ½ whichever connected with Burette
5.3.4 Click on Add Fixed Volume
5.3.5 Fix Volume of 5/10ml
5.3.6 Put Dosing Tip in the Beaker & press Start
5.3.7 Weigh the Mass of the Water dispensed in the Beaker
5.3.8 Repeat it for 5 times & calculate Max Relative Error should be < 0.5%
5.3.9 Collect the dispensed volume in a tarred beaker (Beaker should be cleaned and dried). Determine the dispensed volume in ml as follows:
                                                 (Wt, of the beaker + sample) - Wt. of beaker
Dispensed Volume (ml) = --------------------------------------------------------------
                                                               0.99602 (density of water)

5.3.10 Calculate the relative error % as follows:
     Volume on Display (ml) - Dispensed Volume (ml)
------------------------------------------------------------------------ x 100
                         Volume (ml)

5.3.11 Record the observations in calibration record as per Annexure – I.
5.3.12 Frequency of calibration - Once in three months.

5.4 Precaution

5.4.1 Keep instrument in a dust free area and keep the surrounding dry.
5.4.2 Rinse the Electrodes and Burette tip before and after each titration with water/Solvent.
5.4.3 When not in use keep electrodes in the holder with Storage solution and Burette tip wet.
5.4.4 Check the levels of electrolytes in electrodes regularly and replenish.
5.4.5 For Non-Aqueous Titration Check Molecular Sieve should be in light brown colored. If it is dark brown replace them fresh molecular sieve.
5.4.6 In case of errors refer instruction manual or execute Diagnosis Program.
5.4.7 For exchange unit containing NaOH apply grease to piston every week.

6.0 ABBREVIATIONS

6.1 SOP - Standard Operating Procedure
6.2 NaOH - Sodium Hydroxide
6.3 ML - Milliliter

ANNEXURE - I

INSTRUMENT CALIBRATION RECORD OF AUTO TITRATOR

Asset ID  No.	:		Ref.  SOP No.	:
Make	:		Model No.	:

Burette No. _________________

S. No.	Volume on Display (ml) X	Tare weight of the beaker (gm) (b)	Weight of the beaker with sample (gm) (a)	Dispensed volume in (ml) Y  (a-b)     0.99602	Relative Error %
					X - Y    ----------  x 100           X

Date of calibration                :

Frequency                            :  Once in three months

Tolerance                             : + 0.5%

Remarks: This instrument is working/not working satisfactorily as per SOP.

                                                                                                           _______________________  

Date of Calibration                    Calibrated by (Name/sign)                  Checked by (Name/sign)/on 

ANNEXURE – II 

AUTOTITRATOR USAGE LOG

Date	Product/ Material Name	Batch No./Lot No.	Time		Analysis performed	Analyzed by	Checked by	Remarks
			Started at	Completed  at

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