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Calibration Policy/SOP – Instrument calibration is one of the primary processes used to maintain instrument accuracy. Calibration is the process of configuring an instrument to provide a result for a sample within an acceptable range.

Policy – Calibration of Instrument & Equipment

1.0   OBJECTIVE

• • To define the policy for calibration of all master instruments and measuring devices used for measuring, monitoring and controlling of operations and process.

2.0   SCOPE

• • This SOP is applicable for the in-house or external calibration for all the master instruments, all measuring equipments, testing equipments, process control equipments used in, stores, manufacturing, Packing, Engineering, Q.C. used Pharmaceuticals plant.

• • The scope of this SOP however does not cover calibration of QC equipments like HPLC, Gas Chromatograph, pH meter, etc.

3.0   RESPONSIBILITY

• • Instrumentation Engineer : to ensure calibration of instruments as per schedule

• • Head – Utility: Compliance to calibration schedule and plan

• • Head – Quality Assurance: Compliance to procedure

4.0   DEFINITION (S)

• • Calibration: A set of operations which establish under specified conditions, the relationship between values indicated by a measuring instrument or measuring system or values represented by a material measure and the corresponding values of a quantity realized by a reference standard.

• • Accuracy: The closeness of agreement between an observed or measured value and accepted reference value.

• • Measurement standards: A measuring instrument or material, which physically defines a unit of measurement or value of a quantity.  Measurement standards should usually be traceable to a national or international standard.

• • Critical Instruments: The instrument, which gives the direct impact on the product.

• • Non-critical Instrument: The instrument, which does not have the direct impact on the product and is optional.

5.0   PROCEDURE FOR CALIBRATION OF INSTRUMENT

• • All master instruments shall be calibrated at least once in a year or as desired in case of special requirement and shall be traceable to national standard like NPL or NIST or international standards.

• • All measuring and monitoring devices / instruments are calibrated either internally or by approved external party.

• • Instruments calibrated internally shall include e.g. pressure gauge (0 to 30 kg/cm²), pressure switch, vacuum gauge, temperature sensors, digital temperature indicators, temperature controller, glass thermometers, temperature gauge, timer, tablet counter, stop watch, RH controller, pH sensor, pH meter, pH transmitter, data loggers, oxygen analyzer, RPM meter, chart recorder, micrometer, Magnehelic gauge, digital thermometer, digital Vernier caliper and conductivity transmitter.

• • On satisfactory completion of calibration, “CALIBRATED” tag shall be attached as per format mentioned in SOP.

• • Master instruments to be calibrated from external agency shall be maintained as per Annexure-I.

• • All the masters/measuring instruments that are to be calibrated from external agency shall be sent either to calibration agency or the agency shall be called for the calibration.

• • All calibrated certificates received from the external agency shall be filed separately and external calibration tag shall be affixed on respective master/measuring instrument.

• • All certificates received from external agencies shall be verified by concerned engineer responsible for calibration.

• • Calibration of newly installed measuring instruments

• • The concerned department during qualification of new equipment shall inform the Utility Department for new measuring instruments.

• • The engineer concerned with the equipment then checks for the measuring instruments on that particular equipment.

• • The engineer checks for the supplier / factory equipment calibration certificate. If available, then calibration tag is fixed.

• • Also an identification number is given to the new instrument, which is cross-referenced on the supplier’s equipment calibration certificate.

• • If the supplier equipment calibration certificate is not available then the new measuring instrument(s) is calibrated before use as per relevant SOP(s).

• • The calibrated instrument is given a new identification number, calibrated and calibration certificate is prepared for the same.

• • The new identification number is then updated in the index sheet of Additional Gauges / Instruments Calibration Planner cum Schedule (Annexure-III) and shall be subsequently updated in the Annual calibration Schedule of subsequent year.

• • In case any new master/measuring device is introduced/ added after the preparation of annual calibration plan, it shall be recorded in “Additional Gauges / Instruments Calibration Planner cum Schedule” (Annexure-III).

• • At the end of the calendar year the new addition master/measuring instrument shall be incorporated from next year schedule for calibration.

• • In case any new master/measuring device is removed after the preparation of annual calibration plan, it shall be recorded in “Deletion of Measuring Instruments Calibration Schedule” (Annexure-V). At the end of the calendar year the deletions shall be updated in schedule cum plan for next year.

• • Procedure for Equipment Log-out

• • Utility Department shall be informed about the equipment to be removed.

• • The concerned Engineer then checks for the measuring instruments on concerned equipment.

• • It shall be recorded in form “Deletion of Measuring Instruments Calibration Schedule” (Annexure-V).

• • Action to be taken if any instrument is found out of calibration limits.

• • At the time of calibration, if any instrument is found out of acceptable limit “OUT OF CALIBRATION” label shall be pasted on the equipment.

• • Investigation and Reporting shall be done as per SOP  “Handling of Out of Calibration”.

• • In such a case, additional calibrated device of the type shall be incorporated in its place till the measuring devices are received after calibration.

• • On receipt of the calibrated devices, it shall be incorporated and documented.

• • If the instrument remains unfit for use, the instruments shall be removed by a new calibrated instrument.

• • If any of the measuring devices found to be out of order during operation, the same shall be taken for correction and calibration.

• • It shall be further incorporated only if the result found to be satisfactory. In case, the correction is not done, it shall be replaced by another calibrated measuring devices.

• • Calibration of Instrument after Location Change

• • If the location of measuring instrument is changed from one equipment to another, the same shall be done after approval from QA.

• • A planned deviation shall be filled for the same.

• • A remark of change of location shall be mentioned on the certificate.

• • At the time of recalibration of the instrument, the calibration certificate and the tag will be updated as per the new equipment code number and it’s location.

• • Instrument / Equipment Calibration Frequency:

• • Frequency of calibration is based on criticality of measurement; risk associated with failure or inaccuracy, history of equipment as per reliability or manufacturers recommendations.

• • The calibration frequency is 6 months/ half yearly for critical equipments and for equipments directly related to process and not more than 12 months/ yearly for non-critical equipments.

• • In house calibration of equipments shall be done within 7 days of its the schedule date.

• • Calibration from external party shall be completed within 15 days of its scheduled due date.

e.g. If a gauge has a schedule calibration date of 06.01.2013 and has a frequency of one year, then the next calibration shall done within ±7 days of scheduled date.

• • In case, the calibration of any measuring devices is not be completed as planned due to unforeseen reasons, it shall then be completed in the next 15 days for in house calibrated instruments and 30 days period outside calibrated instruments respectively.

• • The activity shall be controlled through a “Request for Extension Calibration Date of Instrument/ Gauge” (Annexure-VI).

• • Documentation of Calibration of Instrument & Equipment

• • All instruments shall be calibrated in-house or from the external agency as per the Annual calibration plan (Annexure II).

• • Utility department based on the frequency of various measuring devices shall prepare the Annual calibration plan.

• • The plan shall be verified by Utility head and approved by Head, Plant and Head, Quality Assurance.

• • Based on the Annual calibration Plan, Annual Calibration Plan and Schedule (Annexure-II) shall be prepared by Utility department.

• • The schedule shall be verified by Head, Utility and Approved by Plant Head and Head, Quality Assurance.

• • The calibration of the measuring devices shall be performed as per respective SOP.

• • For each in-house calibration, a calibration certificate shall be generated as per format defined in Annexure-VI.

• • For those measuring devices, which are calibrated from external agency, the certificate number shall be same as mentioned in the test certificate issued by the external agency.

• • The in-house calibration certificate number shall be in the format CAL/XXX/YY/NNN

The pattern for the certificate number shall be given as follows:

CAL     : Stands for calibration certificate.

/           : stands for forward slash

XXX     : Department code where instrument is available.

/           : stands for forward slash

YY       : Year of calibration e.g. 23 for 2023

/           : stands for forward slash

NNN    : Serial number of the certificate starting from 001

Example -1: First calibration certificate issued in year 2023 for the utility shall be: CAL/UTC/23/001.  The serial number of the certificate is the sequence in which the calibration is performed.

• • During preparation of calibration certificate details like serial number, range, least count, calibration date and due date shall be recorded along with acceptance criteria, details of standard instrument, reading before and after calibration wrt standard.

• • The variation observed from the reading of master instruments during calibration of instruments like Temperature controllers, temperature indicator, chart records, RPM meters, RH controller, Temperature and RH indicator, ampere meter, volt meters, frequency meter, level transmitter, pressure transmitter, pressure gauges, temperature gauge, shall be a corrected as per the standard input value of the master instrument. This shall be recorded in the calibration certificate (Annexure-VI).

• • All the calibration certificates / records shall be archived in QA for a period of not less than five years from end of the calibration year. (Refer SOP  “Document and Data Control”).

ANNEXURE – I – LIST OF MASTER INSTRUMENT

ANNEXURE – II – ANNUAL CALIBRATION PLAN AND SCHEDULE

Department:                                                                                                          Year:

ANNEXURE – III – ADDITIONAL GAUGES / INSTRUMENTS CALIBRATION SCHEDULE CUM PLANNER

ANNEXURE – IV – Format for Calibration Certificate

Instrument : ………………………………………………………… Certificate No.: ………………….………………..

Make: …………………………………………………………………. SOP Ref. No.: …………………………………..…

Instrument ID: …………………………………………….………… Serial No.: …………………………………………

Range: ……………………………………………….….………        Cal. Date: …………………………………………..

Least Count: ……………………………………………….… ..       Due Date: …………………………..………………

Acceptance Criteria: ……………………………………..……..      Location: …………………………………

Unit of Measurement: …………………..……………………..

Remarks: …………………………………………………………………………………………………………………………..

 Environmental Condition during Calibration: Temp. ……… (ºC) Relative Humidity ……… (%)

Detail of Standard Instrument Used for Calibration:

CONCLUSION: The instrument is CALIBRATED / NOT CALIBRATED under the specified limits.

ANNEXURE – V – Deletion of Measuring Instruments Calibration Schedule

ANNEXURE – VI – Request for Extension Calibration Date of Instrument / Gauge