Introduction Calibration requirement Purpose / Importance of Calibration Definitions ISO 9001:2000 requirement Calibration of MMDs Documents & Records
Calibration RequirementRequirement by QMS & cGMP ISO 9001:2000 7.6 Control of monitoring and measuring devices cGMP: Q7A 5.0 Process Equipment : 5.3 Calibration 6.6 Laboratory Control Records USFDA: 21 CFR Part 210/211
Definition: Calibration Set of operations that establish, under specified conditions, the relationship between values of quantities indicated by a measuring instrument or measuring system, or values represented by a material measure or a reference material, and the corresponding values realized by standards.Notes: 1. The result of a calibration permits either the assignment of value measurands to the indications or the determination of corrections with respect to indications. 2. A calibration may also determine other metrological properties such as the effect of influence quantities. 3. The result of a calibration may be recorded in a document, sometimes called a calibration certificate or a calibration report.
Calibration! What is it ? A set of operations, performed in accordance with a definite procedure, that compares the measurements performed by an instrument to those made by a more accurate instrument or a standard for the purpose of detecting and reporting, or by adjustment, errors met in the instrument tested.
Purpose of CalibrationTo ensure readings from an instrument are consistentwith other instruments and to determine the accuracyof the instrument i.e. that it can be trusted for itsobserved/displayed measured value.The value of calibration for industry To ensure that products are manufactured to specifications. To demonstrate that the industry operates a quality system and technically competent and are able to generate technically valid results. To increase quality & value of product. The calibrated measuring instruments (working standards) have the assurance of an unbroken chain of national/international measuring standards.
Definitions (ISO 10012:1997) Maximum / Limits of permissible error (of a measuring instrument) Extreme values of error permitted by specifications, regulations, etc. for a given measuring instrument. Measurement process: Set of interrelated resources, activities and influences which produce a measurement. Notes: “Influences” are all factors such as those caused by the environment which may or may not be controlled or controllable and which add to the variability or the bias of the process.
Definitions (cont..) Measuring equipment: All of the measuring instruments, measurement standards, reference materials, auxiliary apparatus and instructions that are necessary to carry out a measurement.Notes: 1. This term includes measuring equipment used in the course of testing and inspection, as well as that used in calibration. 2. In the context of this part of ISO 10012, the term “measuring equipment’ is taken to encompass “measuring instruments” and “measurement standards”. Moreover, a “reference material” is considered to be a type of “measurement standard”.
Uncertainty of measurement: Uncertainty- How accurate are the measurements ? It is a measure of the quality of a measurement & provides the means to assess & minimize the risks and possible consequences of poor decision. Parameter, associated with the result of a measurement that characterizes the dispersion of the values that could reasonably be attributed to the measurand. Notes: 1. The parameter may be, for example, a standard deviation (or a given multiple of it), or the half-width of a interval having a stated level of confidence. 2. It is understood that the result of the measurement is the best estimate of the value of the measurand, and that all components of uncertainty, including those arising from systematic effects, such as components associated with corrections and reference standards, contribute to the dispersion.
Abbreviation Metrology is the science of measurement. Metrology includes all theoretical and practical aspects of measurement. NIST: National Institute of Standards and Technology (USA), BIPM: International Bureau of Weights and Measures NABL: National Accreditation Board for Testing and Calibration Laboratories
Indicator, Monitoring device and Measuring equipmentWhat is the difference? For example, a pressure gauge may be used:- as an indicator (e.g. to ensure that the pressure is present); as a monitoring device (e.g. to ensure that the pressure is stable and the process is under control); and as measuring equipment (e.g. where the accurate value of the pressure is important for the quality of product).
Calibration and verification Calibration system determines the accuracy of measurement and verification system determines the integrity of devices.
ISO Standard ISO 5725: 1994 (P-1,2 &6) Guide on precision of the test methods: Principle and applications (IS:5420 p-1) ISO 5725: 1994 (P-4) Guide on precision of the test methods: Inter Laboratory testing (IS:5420 p-2) ISO 5725: 1994 (P-3 &5) Accuracy & precision ISO 9001: 2000 & ISO 9004 : 2000 ISO 10012: 1992 (p-1): Quality Assurance requirement for measuring equipment: Meteorological confirmation system for measuring equipment. ISO 10012: 1997 (p-2): Quality Assurance for measuring equipment: Guidelines for control of measurement processes ISO guide 30 & 33
ISO Clauses1. Scope2. Normative reference3. Terms and definitions4. Quality Management System (4.1-4.2)5. Management Responsibility (5.1-5.6)6. Resource Management (6.1-6.4)7. Product Realization (7.1-7.6)8. Measurement, analysis and improvement (8.1-8.5)
TrainingServices 4.1 Control Our Processes 4.2 Control Our Documentation 5.3 Policy Objectives 5.4 5.2 Customer Focus Determine & Communicate 5.5 Authority & Responsibilities Customer 5.1 Committed Review 5.6 8.2.1 Satisfaction 5. Managed 8.2.2 System 8. Measure GOOD 6. Provide Resources 8.2.3 Processes Analyse COMPANY People 6.2 8.2.4 Product Improve ISO Buildings, Equipment, Machinery, etc 6.3 8.3 Non-conforming 7. Do What the Environment 6.4 Product Customer Wants 8.4 Data & Info Planning 7.1 Corrective Selling 7.2 8.5.2 Action Designing 7.3 Purchasing 7.4 8.5.3 Preventive Doing It 7.5 Action Calibrating 7.6 22
ISO 9001: 2000 refers where?6.0 Resource Management 6.3 Infrastructure Determine, provide and maintain infrastructure needed7.5.1 Control of production and service provision7.6 Control of monitoring and measuring devices (MMD)
7.6 Control of monitoring and measuring devices (MMD) Determine Monitoring and measurements to be made and measurement and monitoring devices needed to provide evidence of conformity of product. Calibrate of verify measuring and monitoring devices (MMD) at specified intervals or prior to use against international or national standards. Where no such standard exist record to the basis. Adjust or Re-Adjust necessary. safeguarded from adjustments that would invalidate the measurement result protected from damage and deterioration during handling, maintenance and storage.
7.6 Control of monitoring and measuring devices (MMD) When the equipment (MMD) is found not to conform to requirements, the organization shall assess and record the validity of the previous measuring results. The organization shall take appropriate action on the equipment and any product affected. Records of the results of calibration and verification shall be maintained. When computer software used in the monitoring and measurement, the ability of to satisfy the intended application shall be confirmed.
How can we do to meet the requirement? Selection of Instrument Least count / Resolution required Calibration Frequency of calibration
Indicator, monitoring and measuring devicesFor example, in some industries, a pressure gauge may be used:- as an indicator (e.g. to ensure that the pressure is present); as a monitoring device (e.g. to ensure that the pressure is stable and the process is under control); and as measuring equipment (e.g. where the accurate value of the pressure is important for the quality of product).
Least count /Resolution requirementLeast count /Resolution requirement is as required for processEg-1. Temperature measurement 51 -55°C Assume Least count is 1°C Measurement accuracy is ± 1°C Measurement : 51,52,53,54,55 ie 2 out of 5 value likely to out of range 2/5=40%Eg-2. Temperature measurement 51 -70°C Assume Least count is 1°C Measurement accuracy is ± 1°C Measurement : 51,52,53.. 69,70 ie 2 out of 20 value likely to out of range 2/20=10%
Least count /Resolution requirementIdeal tolerance limit is 1/10 = 10% For case-1 51-55 or 53 ± 2°C 1/10th of 2 is ± 0.2°C or at least 1/5th ± 0.4°C For case-1 51-70 or 60.5 ± 9.5°C 1/10th of 10 is ± 0.95°C or at least 1/5th ± 1.95°C
Acceptance criteria / permissible limit Instrument accuracy can be / acceptance criteria = measurement accuracy or finer but not higher.
CONTROL OF MMDsWhat we do, Identify the instruments, Equipments used for process, analysis and etc, List with equipment code Record the resolution, limit of permissible error etc Calibration frequency & Schedule Calibration – External / Internal Record the calibration activity.
CONTROL OF MMDs at MDPL SOPs for calibration List the Standards used for calibration Statuary requirement if any Traceability to standard / master used Maintain relevant record SOP for OOC
CONTROL OF MMDs at MDPL Calibration to cover the entire range of MMD At least 5 to 6 points to establish linearity Additional points at operational range Record the calibrated spare installed during calibration of MMD if any
Record for calibration Format for raw data / certificate Refer Standard used Review / Compare result with permissible error Value before and after calibration Readjusted if any Remark: Correction required / error is to be added with the value / reading Enter the Status :Passes / fails Inform the user to add correction Status Label.
Evaluation of External Agency Service provider to be evaluated / audited NABL accreditation System / standard followed SOP and standards Masters NIST Qualification & Competence of person Maintain audit report , approved service provider list, contract etc
Verification of External certificateHave a check list for verification Is agency SOP reviewed & accepted Is followed as per SOP & referred Is it in the specified format Covered the range of MMD Check for all info like Code no, range resolution, correction, status ….. Review evidence – stamp and sign & date.
Q7A: 5.3 Calibration Control, weighing, measuring, monitoring, and testing equipment critical for ensuring the quality should be calibrated according to written procedures and an established schedule. Equipment calibrations should be performed using standards traceable to certified standards, if they exist. Records of these calibrations should be maintained. The current calibration status of critical equipment should be known and verifiable. Instruments that do not meet calibration criteria should not be used. Deviations from approved standards of calibration on critical instruments should be investigated to determine if these could have had an effect on the quality of product manufactured using this equipment since the last successful calibration.
Q7A: 6.6 Laboratory Control Records Periodic calibration of laboratory instruments, apparatus, gauges, and recording devices
4.2 Documentation (ISO 10012-2: 1997) Document should be specific. It should state responsibility and action to be taken. Document the Performance of the Measurement processes. Guidance: Specification of measuring instrument Measurement procedure Instruction for the operator Validation report Verification report Measurement uncertainty Limits of permissible error Details of and/ or listing of computer program used
4.3 Measurement processes (ISO 10012-2: 1997) The performance characteristic required for the intended use should be characterized Eg. Uncertainty in use Stability Range Resolution Repeatability Reproducibility Skill level of the operator. Should specify master used, condition of use, other factor affecting the reliability of measurement.
4.10 Indicated failure of a controlled measurement processes. When Indicates failure to meet the specification, take necessary corrective action and document. Decreasing the interval between the check Repairing or eli9minating unstable or unreliable instrument Extending the time span over which the measurement made Decreasing the uncertainty acceptable or increasing the accuracy required for instrument Increasi8ng the number of influence quantities being checked Upgrading the operator competence
4.13. Records of control of measurement processes. Sufficient records should be maintained to demonstrate compliance Full description: Identification of Equpt., code, Standard used, operating condition, operator Relevant data / values including measurement uncertainty Action taken Readjusted if any Date of activity, verification program Identification of verification and document Person performed the activity Qualification of person.