Standard Operating Procedures calibration

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. 

Note that some organizations may not use the terminology used in this book and may not distinguish between SOPs and WIs. Standard Operating Procedures provide details of how a series of operations are carried out. An example of a SOP would be the detailed instruction for carrying out a particular analytical method. Work Instructions give details of how a specific operation is carried out. What might be classed as a WI is how to operate a particular instrument, how to estimate measurement uncertainty or how to calibrate a piece of equipment. 

Maintenance and calibration of equipment Standard operating procedures... 

An analyst, a metrologist, or a qualified contractor can perform the calibration, though all must follow the company s prescribed standard operating procedure (SOP) and acceptance criteria. The cost effectiveness of using outside contractors or an internal metrology department is dependent on company size and the number of HPLC systems in the laboratory. 

Laboratory apparatus should be periodically inspected, cleaned, maintained, and calibrated according to standard operating procedures. 

Identify and write standard operating procedures for calibration. 

Standard Operating Procedure A SOP has to be written to provide instructions for the operation, maintenance, and calibration of the new instrument. A typical SOP should include ... 

The written Standard Operating Procedures required under 58.81(b)(ll) shall set forth in sufficient detail the methods, materials, and schedules to be used in the routine inspection, cleaning, maintenance, testing, calibration, and/or standardization of equipment, and shall specify, when appropriate, remedial action to be taken in the event of failure or malfunction of equipment. The written standard operating procedures shall designate the person responsible for the performance of each operation. 

Written records shall be maintained of all inspection, maintenance, testing, calibrating and/or standardizing operations. These records, containing the date of the operation, shall describe whether the maintenance operations were routine and followed the written standard operating procedure. 

The manufacturer should verify the operation of these critical components during the installation according to their standard procedures for evaluating the proper operation of these components. Additional IQ checks will verify that the necessary documentation is available for proper operation of the chamber. These checks should confirm that standard operating procedures and equipment manuals are available. In addition, all calibrated instruments associated with the chamber should be documented in current calibration and placed on a calibration program. 

Finally, during the qualification of the facility, all systems are tested, calibrated, and cleaned. The mechanical and service infrastructure must be qualified. The operational qualification will involve practice runs. All documentation must be finalized. This includes standard operating procedures, batch records, and equipment logs. 

Specifications How good do the numbers have to be Write specifications Pick methods to meet specifications Consider sampling, precision, accuracy, selectivity, sensitivity, detection limit, robustness, rate of false results Employ blanks, fortification, calibration checks, quality control samples, and control charts to monitor performance Write and follow standard operating procedures... 

Availability of standard operating procedures. This section requires the executors to verify and list applicable operational, preventative maintenance, calibration, and equipment cleaning procedures that are available. 

While these are two separate and distinct activities, each must complement the other to ensure a quality program. Day to day quality control in the laboratory is the obligation of the chemist. The chemist develops the methods, calibrates the instruments, and with management approval develops the standard operating procedures for the laboratory. Quality control is running duplicate samples, reagent blanks, fortification samples, linearity checks and confirmatory analyses. 

Standard operating procedures (SOPs) are required for all routine activities that are critical to the successful outcome of the study including quality assurance procedures and inspections. Most of the SOPs for the field activities are written by the field scientists with guidance from the Quality Assurance Section. For the field activities, it is required that at each site there be SOPs for such things as how field plots are established and the plot boundaries marked, the maintenance of sample freezers, how to calibrate and maintain chemical balances and chemical application equipment, and how to obtain test chemicals. If an SOP for a critical item of equipment is not available, the study would be considered to be not in compliance with the principles of the GLP guidelines. The distribution of SOPs is carefully controlled so that when an SOP is changed, all outdated copies can be exchanged for the new version. 

The laboratory quality control program has several components documentation of standard operating procedures for all analytical methods, periodic determination of method detection levels for the analytes, preparation of standard calibration curves and daily check of calibration standards, analysis of reagent blank, instrument performance check, determination of precision and accuracy of analysis, and preparation of control charts. Determination of precision and accuracy of analysis and method detection limits are described under separate subheadings in the following sections. The other components of the quality control plan are briefly discussed below. 

Method development includes feasibility and optimization to meet the predefined study requirements. The appropriate standard calibrator range and concentrations of VS and QC (see discussion below) should be established for the dosage form and route of administration. The lessons learned during method development are critical for the development of specific parameters for the performance of the assay. For example, the number of validation batches and acceptance criteria should be described in a validation plan, and the standard operating procedure (SOP) should be written before conducting the pre-study validation. The correct approach should be to develop a valid (acceptable) method, rather than simply... 

For the GC/MS analysis of unknown chemicals, more or less universal procedures have to be used, because of the large variety in matrices and scheduled compounds. This requires the use of ROPs rather than of standard operating procedures (SOPs), because ROPs allow modification of procedures in the process of analysis (validation on the job). However, SOPs have to be followed for instrument calibration and validation. 

---