CALIBRATION OF AUTO TITRATOR

  1. CALIBRATION OF POTENTIOMETRIC   :
  2. pH Calibration for electrode:
  3. Configuration Screen displays the status of pH calibration beside calibration icon or initially     when application is installed, screen shows “pH not Calibrated”.
  4. To calibrate instrument click <Calibration> icon.Application opens calibration screen.Click <Calibrate> click. The first step in calibration is standardization.Dip electrode in neutral buffer, wait till the electrode potential displayed in mV text box stabilizes.
  5. Click <ok> button once potential value is steady.
  6. Repeat the same steps for Acid buffer and Base buffer (PH-4.01, pH 7.00, pH – 10.01). For buffer pH 4.01 the slope 1 should be between 80 to 120%.
  7. For buffer pH 10.01 the slope 2 should be between 80 to 120%. The activity cannot proceed further if the error is observed during calibration.
  8. During shutdown always press restart switch so extra titrant will be dispense in Titrant bottle.
    1. Calibration of KF titrator:
      1. Calibration procedure for Karl Fischer (KF) Assembly:

Neutralization: Take 30-40 ml of dried methanol in K.F. vessel. Place the vessel on magnetic stirrer and connect dispensing tube, electrode and filter dryer to the vessel. Reset the instrument. Select method no.5 for neutralization and titrate the methanol against K.F reagent. Allow the instrument to be in leak rate mode for 5 minutes.

Water Factor:

Added one drop of ultra pure water to the neutralized methanol with the help of syringe (weight the water introduce in K.F. vessel) and titrate the moisture against the K.F. reagent using concentration method no-1, Run the sample in triplicate and calculate the %RSD and it shall not be more than 1.0%.

Secondary Standardization:

For Moisture Content: Weigh accurately 150 mg of Disodium Tartrate & transfer it in to magnetic stirrer vessel, start the stirrer and run the method. Result will be displayed and print automatically. Run the sample in single and calculate the moisture content and it should be between 15.46 and 15.86.

  1. Prepare the calibration tag and affix it on the equipment.
    1. Enclose the old calibration tag with the record.
    1. If the variation is not within the specified tolerance limits then inform to the department head and label the equipment with tag ‘OUT OF CALIBRATION’ and further proceeded by raising the deviation.
    1. Do not use equipment until all errors are rectified. After rectification, again calibrate the equipment & record the observation.
    1. Frequency: 3 months ± 5 days
    1. Cleaning
      1. Do not let treated methanol in the Auto titrator Vessel.
      1. Wash the Auto titrate vessel after use.
      1. Clean the burette with the methanol.
      1. Clean the instrument with dry lint free cloths.
    1. Preventive Maintenance :

 Preventive maintenance shall be performed once in a year by the service engineer if required.

Bhanu Pratap Singh

BHANU PRATAP SINGH IS EXPERIENCED IN PHARMACEUTICAL, AUTHOR AND FOUNDER OF PHARMACEUTICAL GUIDESLINE (WWW.PHARMAGUIDESLINE.COM), A WIDELY READ PHARMACEUTICAL BLOG SINCE 2019. EMAIL:- INFO@PHARMAGUIDESLINE.COM

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