SOP Title: Calibration of Instruments and Equipment’s
- Objective:
To define written procedure for Calibration of Instruments and Equipments in Quality Control
Department.
- Scope:
This procedure is applicable for Calibration of Instruments and Equipments used for analysis in
Quality Control Department.
- Responsibility:
- Quality Control Department: To prepare and review the SOP. To follow the procedures laid down for Calibration of Instruments and Equipments in Quality Control Department as per this SOP.
- Quality Assurance Department: To review and approve the SOP and Annexures.
- Accountability:
Head Quality Control Department, Head Quality Assurance Department
- Procedure:
| 5.1 | Principles of Calibration: | |||||||||||||
| 5.1.1 | To ensure readings from instrument are consistent with other measurements. | |||||||||||||
| 5.1.2 | To determine the accuracy and precision of the instrument readings. | |||||||||||||
| 5.1.3 | To establish the reliability of the instrument that it can be trusted. | |||||||||||||
| 5.2 | General Requirements: | |||||||||||||
| 5.2.1 | List of all the Equipments/Instruments used in Quality Control Department should be available. | |||||||||||||
| 5.2.2 | Reference Standards used for calibration should be stored in designated places to prevent contamination and/or deterioration. | |||||||||||||
| 5.2.3 | The Reference Standards used for calibrations should be traceable to recognised National Standards. | |||||||||||||
| 5.2.4 | All Reference Standards, Certified Reference Materials, or Reference Materials used for calibration shall be uniquely identified by allocating reference numbers as per SOP “Handling of Reference Standards”. | |||||||||||||
| 5.2.5 | A certificate of traceability, if applicable, shall be retained to ensure traceability. | |||||||||||||
| 5.2.6 | All Equipments/Instruments shall be maintained in good operating order and according to manufacturer or maintenance requirements. | |||||||||||||
| 5.2.7 | Before starting the calibration, ensure that right standard used for calibration, check availability and validity of the required standards. | |||||||||||||
| Frequency of Calibration: | ||||||||||||||
| 5.2.8 | Calibration Schedule
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| 5.2.9 | All analytical Equipments/Instruments shall be calibrated on their due date of calibration. | |||||||||||||
| 5.2.10 | All analytical Equipments/Instruments must be re-calibrated prior to use after any major repair, maintenance or service work have been carried out. | |||||||||||||
| 5.2.11 | All critical Equipments/Instruments must be re-calibrated by the normal procedure if they are moved or if their location is changed. E.g. balance. | |||||||||||||
| 5.2.12 | Upon the receipt of new Equipment/Instrument, Calibration shall be carried out after completion of qualification prior to use. | |||||||||||||
| 5.2.13 | Instrument calibration frequency shall be decided based on manufacturer recommendation, criticality of instruments, possibility of variation in instrument internal setting etc.
E.g. pH Meter/ Weighing Balance – Daily calibration, HPLC – Quarterly calibration etc. |
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| 5.3 | ||||||||||||||
| 5.3.1 | Prepare the “Annual Calibration Schedule” as per SOP i.e. Equipment’s/Instruments Calibration, yearly according to the list of calibration to calibrate the equipments/instruments. | |||||||||||||
| 5.3.2 | Supervisor shall prepare the “Monthly Calibration Schedule” at start of every month as per Annexure by referring “Annual Calibration Schedule”. | |||||||||||||
| 5.3.3 | Supervisor or analyst shall allocate A. R. No. on the “Instrument/Equipment Calibration Register” and shall give requisition to QA department for calibration formats of instruments on the due date of calibration. | |||||||||||||
| 5.3.4 | Analytical Reference number shall be given as “CAL/YY/XXX”.
Where, ‘CAL’ stands for ‘Calibration’. ‘YY’ stands for ‘Last two digits of Current year’. ‘XXX’ stands for ‘Serial number of calibration in the current year i.e. 001, 002 and so on’. |
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| 5.3.5 | Calibration format shall be a part of individual instrument/equipment SOP and shall include details of Instrument/Equipment, calibration parameters, observation, acceptance criteria, solution preparation procedure, weight prints, reference standards details etc. | |||||||||||||
| 5.3.6 | On the day of calibration of instrument, the analyst shall affix the status label on the instrument as “Under Calibration”. | |||||||||||||
| 5.3.7 | Calibration of instruments/equipments shall be carried out as per procedure defined for calibration in the respective instrument SOP. | |||||||||||||
| 5.3.8 | Update the “Instrument/Equipment Usage Log Book” as per Annexure. | |||||||||||||
| 5.3.9 | Affix the “Calibration Status Label” as per Annexure on the Instrument/Equipment calibrated. | |||||||||||||
| 5.3.10 | Example: If the calibration frequency is 3 months for HPLC instrument, and if calibration is performed on 24/05/2023, then the next due date of calibration shall be 23/08/2023. | |||||||||||||
| 5.3.11 | Record the calibration data on the calibration format/protocols of respective instruments and also update the monthly and yearly calibration schedule. | |||||||||||||
| 5.3.12 | Supervisor/Reviewer shall verify all the data of calibration and submit to the QC Head for approval. | |||||||||||||
| 5.3.13 | If the Instrument/Equipment does not qualifies the calibration criteria, then the analyst shall report to the supervisor or Head of the Department. | |||||||||||||
| 5.3.14 | Supervisor shall initiate investigation as per SOP “Incident reporting and investigation” by filling incident form. | |||||||||||||
| 5.3.15 | After completion of investigation, if the error observed as instrument error then affix “Out of Calibration” label on the instrument and intimate Engineering Department or service engineer to rectify the problem. | |||||||||||||
| 5.3.16 | Recalibrate the Instrument/Equipment after problem is rectified. | |||||||||||||
| 5.3.17 | If calibration fails because of analyst error then recalibrate the Instrument. Training shall be imparted to analyst and documented. | |||||||||||||
| 5.3.18 | If calibration fails because of instrument error then impact shall be assessed on previous analysed samples by checking any aberrant results or out of trend results obtained. | |||||||||||||
| 5.3.19 | If aberrant results observed then same samples shall be reanalysed as a part of investigation and results shall be documented. | |||||||||||||
| 5.3.20 | During reanalysis, if results found out of specification then detailed investigation shall be done as per SOP “Out of Specification” to confirm OOS results. | |||||||||||||
| 5.3.21 | If it is confirmed that results are out of specification limit then recall procedure shall be initiated for that batch as per SOP “Product Recall Procedure”. | |||||||||||||
| 5.3.22 | Any calibration which has been done as a part of investigation or analyst validation shall not be considered as routine calibration. | |||||||||||||
| 5.4 | Repair/Service Procedure: | |||||||||||||
| 5.4.1 | Equipments/Instruments that has been subjected to overloading or mishandling gives suspect results or has been shown to be defective or out of calibration shall be taken out of service. | |||||||||||||
| 5.4.2 | These Equipments/Instruments shall be clearly labelled as “Out Of Service – Do Not Use” to prevent use until repaired and shown by calibration or test performed correctly. | |||||||||||||
| 5.4.3 | At the conclusion of the repair/service, a service report should be completed by the engineer indicating what work has been undertaken and what work may be required in the future. | |||||||||||||
| 5.4.4 | All repair/service documentation shall be kept with the instrument history log in order to provide a concise history for each instrument. | |||||||||||||
| 5.4.5 | The “Instrument/Equipment History Card” shall be updated for any equipment where parts have been changed or replaced during the repair or service. | |||||||||||||
| 5.4.6 | If required individual instruments are then re-calibrated as per individual calibration procedures. | |||||||||||||
| 5.4.7 | Details of this re-calibration shall be recorded on calibration logs of respective instrument/equipment. | |||||||||||||
| 5.5 | Procedure for External calibration: | |||||||||||||
| 5.5 1 | Based on the calibration schedule, Quality Control Head shall communicate the calibration due date to the external agency 30 days in advance. | |||||||||||||
| 5.5 2 | Calibration from external agency should be done atleast once in a year or as per current SOP of the Equipments/Instruments. | |||||||||||||
| 5.5 3 | Any additional repair/servicing will also be conducted as and when necessary by a suitable trained engineer of the related company. | |||||||||||||
| 5.5 4 | If required necessary parts shall be replaced before calibration. | |||||||||||||
| 5.5 5 | Flexibility of calibration is ± 30 days from due date for external agency. | |||||||||||||
| 5.5 6 | Calibration reports from external/outside agencies should be properly checked for correctness, acceptance criteria and traceability certificates and stored in Quality Assurance Department. | |||||||||||||
| 5.5 7 | When external calibrations are performed, service providers that demonstrate competence, measurement capability, and traceability shall be used. | |||||||||||||
| 5.5 8 | Calibration certificates from these providers shall contain the measurement results, including a statement of compliance with an identified metrological specification. | |||||||||||||
| 5.5 9 | On the basis of calibration reports from external agencies, If required supervisor shall prepare “External Calibration Report” as per Annexure . | |||||||||||||
| 5.5 10 | QC Head shall verify and approve the reports and submit to the QA Department. | |||||||||||||
- Definitions / Abbreviations:
- Definitions :
- Calibration: Calibration is the process of testing and adjusting an instrument or test system readout to establish a correlation between the instrument’s measurement of the substance being tested and the actual concentration of the substance. It is the process adjustment or standardization of the accuracy of a measuring instrument, usually by comparison with a certified reference or standard.
- Precision: Precisionis the degree to which repeated measurements under unchanged conditions show the same result.
- Accuracy: Accuracy is the degree of closeness of measurements of a quantity to its actual true value.
- Traceability: is the ability to verify the history, location, or application of an item by means of documented recorded identification.
- Certified Reference Materials: A reference material whose property values are certified by a technically valid procedure and accompanied by or traceable to a certificate or documentation issued by a certifying organization.
- Critical Laboratory Equipment: Analytical instrumentation and equipment affecting the accuracy or precision of a test method.
- Performance Verification: The confirmation of the reliability of a previously validated methods or equipment.
- Abbreviations :
| Abbreviation | Expansion |
| QC | Quality Control |
| QA | Quality Assurance |
| QA | Quality Assurance |
| SOP | Standard Operating Procedure |
| A. R. No. | Analytical Reference Number |
| OOS | Out Of Specification |
| e.g. | Example |
| etc | Excreta |
| i.e. | That is |
*Note – Ready to use SOP available in “DOWNLOAD” Section.