Quality in the Analytical Chemistry Laboratory

Definition of Some Terms

Quality
The totality of characteristics of an entity that bear on its ability to satisfy stated or implied needs

Quality control
The operational techniques and activities that are used to fulfil the requirements for quality Planned activities designed to provide a quality product

Quality assurance
All those planned systematic actions necessary to provide adequate confidence that a product or service will satisfy given requirements for quality Planned activities designed to ensure that the quality control activities are being properly implemented Activities usually include internal blind trials, participation in external proficiency testing schemes, replicate testing, control charting, validating methods, obtaining and using suitable reference materials and the regular analysis of blanks and standards.

Quality system
The organizational structure, responsibilities, procedures, processes and resources for implementing quality management Combination of quality management, quality control and quality assurance

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 known measurand (a quantity subjected to a measurement)

Traceability
The property of a measurement whereby it can be related to appropriate national/international standards through an unbroken chain of comparisons

Implementing a Quality System

Reasons for implementing a quality system

A tool for achieving and maintaining product

quality A tool to demonstrate to own management that the product requirements are being achieved A marketing tool to provide evidence to current and potential customers of the laboratory's capability

Reasons for implementing a quality system

Streamline laboratory operation
Ensure continuing development and training of

laboratory staff Motivate and involve staff in the drive towards better laboratory practice and achievement of externally assessed standard Avoid complacency by introducing a program of continuous review and improvement

International Measurement Evaluation Program conducted by the Institute for Reference Materials and Measurements (Belgium)

Certified level: 62.3 1.3 nM

Scattered measurements of Pb in river water by different laboratories, each of which employed a recognized quality system.

Reproducible results from national measurement institutes, where the most care was taken.

Benefits from implementing a quality system

Reduce costs due to lack of quality (these are costs

arising from not doing the correct thing first time) Improvement of work environment and staff morale Improvement of internal and external customers' needs on time, at the desired quality and on budget Improvement of the efficiency and effectiveness of operations

Major components required in a laboratorys quality system

1. Replicate analysis to determine precision 2. Blanks to determine if part of the

measurement is not due to the analyte 3. Calibration for method control 4. Reference materials to check validity of methods 5. Control charts to determine system control

Major components required in a laboratorys quality system

6. Performance test samples (QC samples)

7. Training to ensure that members of staff

are competent in analysis 8. Documentation of results, methods 9. Interlaboratory comparisons 10. Quality audits and review

Blanks
1. Method blank: contains all components except analyte, and it is taken through all steps of the analytical procedure 2. Reagent blank: similar to a method blank, but it has not been subjected to all sample preparation procedures 3. Field blank: similar to amethod blank but it has been exposed to the site of sampling

Spike (Fortification)
A known quantity of analyte added to sample to test whether the response to a sample is the same as that expected from a calibration curve
% Recovery C spiked sample Cunspiked sample C added 100

Performance test samples (QC samples)

Stable, homogeneous, typical in composition to the types of sample normally examined, and available in large quantities Used to study the variation within and between batches of a particular analysis
Repeat sample: repeated later on in the batch of samples or in a different batch; analyst is aware when repeat samples are used Blind sample: type of repeat sample inserted into the batch without the knowledge of the analyst

Control chart: Visual representation of confidence intervals for a Gaussian distribution

Manufacture of Vitamin C tablets ( mg) For quality control, 25 tablets are removed at random from the manufacturing line each hour and analyzed Data point on control chart = mean value of Vitamin C in the tablet

Control chart: Visual representation of confidence intervals for a Gaussian distribution

Troubleshoot when
1 observation outside the action line 2 out of 3 consecutive measurements between the warning and action lines 7 consecutive measurements all above or below the center line 6 consecutive measurements all increasing or all decreasing, wherever they are located 14 consecutive points alternating up and down, regardless of where they are located An obvious nonrandom pattern

2 95.5% n
3 99.7% n

Standard Operating Procedures

State what steps will be taken and how they will be carried out

Quality manual
Details in the laboratorys quality system need to be written down so that everyone in the laboratory can see what the system is and what is expected of them

Activities included in a quality manual

The type of analyses the laboratory carries out Who is qualified to carry out the analyses The work procedures to be followed Environmental requirements necessary to carry out the work How reports should be written How equipment should be calibrated What standards should be used How samples should be stored

Activities not included in a quality manual

Charges made for work carried out The laboratorys terms and conditions of contract The terms of employment of staff Fire and emergency procedures Room numbers and telephone numbers of laboratory staff Who is responsible for stocking the stationery cupboard Whose turn it is to make tea

Quality audit (QA)

A continuing process of testing the quality systems in use in the laboratory to check if the systems are effective, documented, and being adhered to by the working staff Will check that you have been carrying out the job as set down in the laboratorys written procedures The responsibility of the quality manager

Quality system review (QSR)

Periodic reexamination of the laboratorys quality systems to check if the systems are still appropriate Responsibility of the laboratory management

Standards organizations and their requirements

The most widely recognized and used QA protocols and standards in chemical testing fall into three groups and are applied according to individual needs of laboratories: ISO/IEC 17025:2005 (International Organisation for Standardisation / International Electrotechnical Commission) ISO 9001:2000 OECD Principles of Good Laboratory Practice (GLP) (Organisation for Economic Cooperation and Development)

ISO/IEC 17025:2005
Standard which addresses the technical competence of laboratories to carry out specific tests and calibrations and is used by laboratory accreditation bodies worldwide as the core requirements for the accreditation of laboratories. International standard that contains all the requirements that testing and calibration laboratories have to meet if they wish to demonstrate that they operate a quality system, are technically competent and are able to generate technically valid results.

ISO 9001:2000

The standard that relates primarily to quality management, for facilities carrying out production, or providing services, including chemical analysis

OECD Principles of GLP

Guidelines concerned with the organizational processes and conditions under which laboratory studies related to certain regulatory work are carried out

ISO/IEC 17025:2005 Management Requirements

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. Organization Management system Document control Review of requests, tenders and contracts Sub-contracting of tests and calibrations Purchasing services and supplies Service to the customer Complaints Control of non-conforming tests Improvement Corrective Action Preventive Action Control of Records Internal Audits Management Reviews

ISO/IEC 17025:2005 Technical Requirements

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. General Personnel Accommodation and environmental conditions Test and calibration methods and method validation Equipment Measurement traceability Sampling Handling of test and calibration items Assuring the quality of test and calibration results Reporting of results

GLP
GLP Principles (expanded sense) set of requirements covering the organization of test facilities and conditions to ensure the generation of high quality and reliable test data for specific objectives GLP (limited sense) set of practice in the chemical laboratory that controls the laboratory activities and conditions that affect the accuracy of analytical data.

GLP for Accuracy and Reliability of Data

Component of GLP QA Program Laboratory Conditions Objective of the GLP

To ensure consistent quality of data To ensure that laboratory conditions are optimized to obtain the desired performance of the test method. Test Samples To preserve the identity and integrity of the samples Test To To ensure that an acceptable test Measurements method will produce the expected performance Record To enable retrieval of undistorted Management information whenever required

GLP for accuracy and reliability of analytical data is a culture in the laboratory to ensure that the target quality standard of analytical work is achieved.
GLP includes: Implementing standard operating procedures Proper maintenance and calibration of equipment Correct practices of laboratory personnel in performing analytical work Efficient management of laboratory records

National accreditation bodies

Produce more detailed quality requirements for laboratories, usually based on the general criteria set out in ISO, EN, BS and any appropriate national standards and offer to assess laboratories against these quality requirements
UK: National Measurement Accreditation Service (NAMAS) Philippines: Philippine Accreditation Office (PAO)