Calibration auditing

On the other hand, if the process must be validated in an existing facility, existing IQ and OQ information may be adequate. In this case, the validation protocol might merely refer to the data rather than require its regeneration, especially when a credible calibration/audit program had been performed for the facility and equipment after the initial IQ and OQ were performed. This part of the validation work thus might merely be referenced in the validation document. 

In addition to fulfilling the in-house requirements for quality control, state and local air monitoring networks which are collecting data for compliance purposes are required to have an external performance audit on an annual basis. Under this program, an independent organization supplies externally calibrated sources of air pollutant gases to be measured by the instrumentation undergoing audit. An audit report summarizes the performance of the instruments. If necessary, further action must be taken to eliminate any major discrepancies between the internal and external calibration results. 

The auditor who carries out the follow-up audit need not be the same as carried out the initial audit. In fact there is some merit in using different auditors in order to calibrate the auditors. 

Demonstrate that audit trails are created and maintained for Date and time of operator entries and actions that create, modify, or delete electronic records (methods, sequences, raw data, results, reports, calibrations, standards, event logs)... 

Procedures should be established to periodically monitor all operations that may have an environmental impact, and similar scheduled periodic checks should be made to ensure that procedures and operations are still in line with regulatory and other requirements. If equipment is involved in the monitoring process then procedures should also be in place to ensure correct calibration. Procedures are also needed to record any preventative or corrective actions identified and to ensure that they are completed to schedule. The whole EMS should be audited periodically to check that it is consistent with the planned policy and has been properly implemented. The details of audits should be discussed and reviewed by management at the highest level with a view to continuous improvement through the modification of both policy and procedures. 

Calibration and maintenance programs [45], challenge tests [2], accelerated shelf life tests [53], auditing [2], sensory tests [46], microbial tests [47]... 

Audits of each phase of the study should include personnel training, preparation of collection forms, application calibration, each sample collection procedure, sample transport, each type of chemical analysis, data recording, data entry, data verification and data storage. Data collection in the field is often tedious if automated logging devices are not in place. To ensure data integrity, the paper and ink used for field studies should be waterproof. Each data collection form should contain appropriate locations for information detailing the time and location of sample collection, sample transport and sample analysis. Data collection forms should be stored in an orderly fashion in a secure location immediately upon return of field teams from the field at the end of each day. It is also important for data quality for studies to collect necessary field data seven days per week when required. In our experience, poor study quality is likely when field sample and data collection do not proceed on weekends. 

Each data point must be transferred from data sheets into spreadsheets or databases. Verification of each datum should be performed by an individual who did not enter the data being verified. Audits of each phase of the study should be performed (i.e. preparation of collection forms, application calibration, each type of sample collection, sample transport, each type of chemical analysis, data recording, data entry, data verification and data storage). 

The software life cycle activities extend until retirement of the software. However, in a manner of speaking, life cycle activities extend even beyond retirement since the data must be able to be reconstructed at any time during the life of the product, i.e., the archived record must always be accessible and readable even if the software is no longer commercially available or typically employed in the laboratory. Additional software validation includes implementation of the code and integration and performance testing. There also must be system security, change control procedures, audit trails, calibration, preventative maintenance, and quality assurance. 

In addition to incorporating the preceding elements into any metrology program, periodic audits of the calibration and maintenance practices should occur. This is particularly important for systems generating data that are subject to review by... 

Part of the confusion surrounding the model testing and validation process is largely because different meanings have been attached to the terms calibration, verification, validation, and post-audit in the technical literature. As a result of the Pellston conference, I have adopted the following relationship among these terms ... 

Thus, the process of model testing and validation (considered synonymous) should ideally include the steps of calibration (if necessary), verification, and post-audit analyses. I indicate "ideally" because in many applications existing data will not support performance of all steps. In chemical fate modeling, chemical data for verification is often lacking and post-audit analyses are rare (unfortunately) for any type of modeling exercise. 

All aspects of the laboratory s work which might affect the validity of the final result should be inspected. This will include, for example, documentation, equipment, calibrations, methods, materials, record keeping, sample recording, labelling, quality control checks and log of daily checks, among many others. Some aspects, however, are outside the scope of such an audit, such as safety and security matters, which usually have separate arrangements for auditing. 

QQ Start-up routine, calibration routine, data transfer/backup, data integrity, power failure, auto lock off, human-machine interface, security access/audit trail, system stress test in event of power failure, alarm tests, operator data entry tests... 

Standardization The instrument response function can vary from analyzer to analyzer. If calibration transfer is to be achieved across all instrument platforms it is important that the instrument function is characterized, and preferably standardized [31]. Also, at times it is necessary to perform a local calibration while the analyzer is still on-line. In order to handle this, it is beneficial to consider an on-board calibration/standardization, integrated into the sample conditioning system. Most commercial NIR analyzers require some form of standardization and calibration transfer. Similarly, modem FTIR systems include some form of instrument standardization, usually based on an internal calibrant. This attribute is becoming an important feature for regulatory controlled analyses, where a proper audit trail has to be established, including instrument calibration. 

Control of the activities (control of nonconforming testing and/or calibration work, improvement, corrective action, preventive action, internal audits, management reviews)... 

Traditionally, the education that chemists and chemistry laboratory technicians receive in colleges and universities does not prepare them adequately for some important aspects of the real world of work in their chosen field. Today s industrial laboratory analyst is deeply involved with such job issues as quality control, quality assurance, ISO 9000, standard operating procedures, calibration, standard reference materials, statistical control, control charts, proficiency testing, validation, system suitability, chain of custody, good laboratory practices, protocol, and audits. Yet, most of these terms are foreign to the college graduate and the new employee. 

Any portion of the study that is a "field study" may also be audited. A field study auditor would inspect many of the same items already mentioned, but at the field site location. These include the training and experience of the field personnel, the calibration and maintenance of equipment, the field management and operations, the test substance application, and the sampling. Special problems are sometimes encountered in the field because the site is physically displaced from the main site of the study. Despite the physical displacement, the equipment must still be calibrated and maintained, the protocols and SOPs must be followed, there must be proper record-keeping, and there must be regular inspections by the QAU. 

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