On practical metrology and chemical analysis: legal,institutional and technical evolutions in the Australian national measurement system

 Economic and technological change, regional and international trade and the globalisation of industry have led to intense pressures for improvements to analytical quality, reliability and comparability. Of central importance are national traceability structures connecting chemical measurements in the field with internationally accepted measurement units and their practical realisations. Australia has a developed physical and engineering measurement system, a legislative framework for analytical traceability and, in the National Association of Testing Authorities, a recognised laboratory accreditation system. The need has been identified to develop the technical capability to perform matrix-independent reference measurements for the certification of traceable reference materials, useable as practical analytical etalons to establish metrological control systems in field measurements for amounts of substance. Recently, a unique collaborative consortium has proposed a National Analytical Reference Laboratory (NARL). The NARL is designed to be a metrological mass spectrometry facility for the transference of measurement units to more widely useable chemical measurement standards and reference materials. Received: 10 October 1995 Accepted: 26 October 1995     

The German accreditation system

 In response to the requirements of the "Global Approach" in Germany, a national accreditation system has been established based on traditional experiences in the recognition of the competence of laboratories and certification bodies. In 1991, the German Accreditation Council (DAR) was founded as a coordinating body supported by the Federal and State Ministries and German industry. In this way, it was possible to organise coordinated representation in international bodies, to offer a forum for cooperation between authorities and industry, and to provide for a structure subdivided into sectors which better fits the needs of the industrial sectors and gives them the necessary transparency and acceptance. The DAR itself does not carry out accreditations. This is done by the accreditation bodies represented in the DAR and specialised in for specific subjects, thereby having a close connection with expert groups of a high technical competence in their specific technical fields. At the end of this paper, the procedure for the assessment of the technical competence of a laboratory, an important part of the accreditation, is described.     

Can the new ISO Guide 25/EN 45001 create better confidence in laboratory operations?

 Confidence in laboratory operations is discussed based on the ongoing revision of the ISO/IEC Guide 25. Confidence is a subjective attribute, which also depends on whose interest is considered. New and better-defined quality systems and technical elements will be included, and these are beneficial to the transparency of laboratory operations, as well as to the accreditation process. The ultimate aim is, of course, to satisfy customers. The testing laboratories' industrial customers are, however, generally unfamiliar with the ISO/IEC Guide 25 and accreditation. The main reason for improved confidence in testing and calibration laboratories is foreseen to come from closer interaction between laboratories and their customers.     

Adsorption of styrene on micron-sized, monodisperse, cross-linked polymer particles in a snowman-shaped state by utilizing the dynamic swelling method

Polystyrene/styrene–divinylbenzene copolymer composite particles with different cross-linking densities were produced by seeded copolymerization for (styrene/divinylbenzene)-swollen polystyrene particles prepared by utilizing the dynamic swelling method (DSM) which was proposed by the authors in 1991. Using the cross-linked, composite particles as seeds, styrene-adsorbed (swollen) composite particles having snowman shapes were prepared by the DSM. With a decrease in the cross-linking density in the composite particles, the volume of the composite particle which was embedded in a spherical styrene phase in the snowman-shaped, styrene-adsorbed particle increased and the contact angle of the styrene phase on the composite particle decreased. In the DSM process, the absorption stage of styrene in the composite particles and the adsorption stage thereon were clearly observed. This suggests that the cross-linking density of the composite particles greatly affects the morphology of the snowman-shaped particles. Received: 13 December 2000 Accepted: 14 March 2001     

Qualification and validation of software and computer systems in laboratories

 When software and computer systems are purchased from vendors, the user is still responsible for the overall validation. Because the development validation can only be done by the developers, the user can delegate this part to the vendor. The user's firm should have a vendor qualification program in place to check for this. The type of qualification depends very much on the type and complexity of software and can go from documented evidence of ISO 9001 or equivalent certification for off-the-shelf products to direct audit for software that has been developed on a contract basis. Using a variety of practical examples, the article will help to find the optimal qualification procedure. Received: 8 August 1997 · Accepted: 12 September 1997     

Proficiency testing in analytical laboratories: how to make it work

 This paper covers the role of proficiency testing schemes in providing an occasional but objective means of assessing and documenting the reliability of the data produced by a laboratory, and in encouraging the production of data that are "fit-for-purpose". A number of aspects of proficiency testing are examined in order to highlight features critical for their successful implementation. Aspects that are considered are: accreditation, the economics and scope of proficiency testing schemes, methods of scoring, assigned values, the target value of standard deviation σ_p, the homogeneity of the distributed material, proficiency testing in relation to other quality assurance measures and whether proficiency testing is effective. Stress is placed on the importance of any proficiency testing scheme adhering to a protocol that is recognised, preferably internationally. It is also important that the results from the scheme are transparent to both participating laboratory and its "customer". Received: 03 November 1995 Accepted: 20 November 1995     

Evaluating the state-of-the-practice in soil measurements in relation to environmental regulations

 The results of chemical analyses of soils show large variations due to the heterogeneity of the material, differences in pretreatment and analytical methods, and unavoidable random errors. In this article, the analytical aspects in the determination of heavy metals in soils are highlighted. Both within-laboratory and between-laboratory variation must be minimized by validation and standardization procedures, respectively, in order to keep the variations resulting from the analytical procedure at an acceptably low level. Even then, the best results will show uncertainties of 5–20%, an issue that should be recognized by governmental and legal bodies. Received: 9 November 1995 Accepted: 1 December 1995     

Metrology in chemistry: Part I. Current activities in Europe

 The paper (Parts I and II) reports the results of a survey carried out to assess the current situation in the field of metrology in chemistry within Europe and to identify future needs for work at the European level. Responses to a questionnaire covering 17 economic sectors and distributed to 17 countries plus the European Commission Joint Research Centre (EC JRC), together with input from a project group, EURACHEM and EUROMET provided the basis of the study. The questionnaire responses clearly indicated that only a minority of countries had clearly defined responsibilities for policy, funding and technical leadership. Similarly only a small number of countries was able to provide any information about levels of funding. Nonetheless, a variety of work is in progress and in some countries the effort is considerable. In other countries discussion is in progress and /or work is beginning. Part I covers the protocol for the study and reports current activities. Part II reports suggestions for future work, a strategy for metrology in chemistry and recommendations for the EC Fifth Framework Programme. Received: 11 January 1999 / Accepted: 4 January 2000     

Metrology in chemistry: Part II. Future requirements in Europe

 The paper (Parts I and II) reports the results of a survey carried out to assess the current situation in the field of metrology in chemistry within Europe and to identify future needs for work at the European level. Responses to a questionnaire covering 17 economic sectors and distributed to 17 countries plus the European Commission Joint Research Centre (EC JRC), together with input from a project group, EURACHEM and EUROMET, provided the basis of the study. Part I covers the protocol for the study and reports current activities. Part II reports suggestions for future work, a strategy for metrology in chemistry and recommendations for the EC Fifth Framework Programme.     

Conformity assessment and metrology: update on the state of affairs

A couple of years ago, ISO CASCO launched a major project of transforming all the existing ISO Guides on conformity assessment to a comprehensive series of ISO standards 17000 being now in various stages of development. As the concept of traceability underpinning all measurements has been a basic mission of metrology, a number of these standards have a direct bearing on metrology. The series is logically based on a definition standard, ISO 17000, giving, among others, a guidance which activities fall under conformity assessment. The fact that calibration does not, might have important consequences which must yet be assessed. A controversial discussion on some issues has been in progress concerning ISO 17011 on accreditation bodies which touches both on national metrology institutes (NMIs) with an accreditation function and on calibration labs at large. ISO 17040 on peer review could be used with an advantage to support mutual recognition arrangements among a limited number of bodies of a specialized expertise (e.g., CIPM MRA among NMIs under the Metre Convention). ISO 17025 has been the most important standard for the metrology community and has undergone a major overhaul taking on board the uncovered requirements from ISO 9001:2000. In general, the paper will give an update on the developments outlined above and discuss the consequences and further steps from the viewpoint of metrology.     

Crystallization of isotactic polypropylene in a temperature gradient

The crystallization of isotactic polypropylene films was investigated in constant and in time-dependent temperature gradients. The temperature gradient influences a spherulitic pattern as well as an internal structure of spherulites. The gradient can accelerate conversion of the melt into spherulites although it has no effect on spherulitic nucleation. The acceleration of the local conversion results from a contribution of spherulites nucleated in colder parts of a sample. The observed effects intensify with the increase of the temperature gradient and they are also enhanced by a higher crystallization temperature. Received: 2 August 2000 Accepted: 21 February 2001     

Different approaches to legal requirements on validation of test methods for official control of foodstuffs and of veterinary drug residues and element contaminants in the EC

 In order to ensure food consumer protection as well as to avoid barriers to trade and unnecessary duplications of laboratory tests and to gain mutual recognition of results of analyses, the quality of laboratories and test results has to be guaranteed. For this purpose, the EC Council and the Commission have introducedprovisions – on measures for quality assurance for official laboratories concerning the analyses of foodstuffs on the one hand and animals and fresh meat on the other, – on the validation of test methods to obtain results of sufficient accuracy. This article deals with legal requirements in the European Union on basic principles of laboratory quality assurance for official notification to the EC Commission and on method validation concerning official laboratories. Widespread discussions and activities on measurement uncertainty are in progress, and the European validation standards for official purposes may serve as a basis for world-wide efforts on quality harmonization of analytical results. Although much time has already been spent, definitions and requirements have to be revised and further additions have to be made.     

Accreditation in the United Kingdom: responding to needs or 'changing the goalposts'?

 The requirements for establishing the competence of organisations involved in testing, calibration, certification and inspection, and the criteria for their assessment and accreditation are specified in international guides and European standards. As these guides and standards are intended for use by a range of organisations and accreditation bodies, operating in different disciplines, they are written in general terms in order to be widely applicable. It follows that some interpretation of the requirements is needed in order to address the different ways in which both organisations and accreditation bodies operate. This may be seen by accredited organisations as providing an opportunity for accreditation bodies to 'change the goalposts'; the needs of these organisations and of their clients must be accommodated as far as possible, without diminishing the value of, or undermining confidence in, accreditation. The United Kingdom Accreditation Service has been listening to its customers, reviewing its activities and is offering a more flexible pragmatic approach to assessment and accreditation; some of the new developments are described.     

Quality (r)evolution – guidelines and practical implementation of quality management: the U.S. perspective

 All clinical laboratories in the United States were required for the first time in 1992 to comply with universal minimum regulations: the Clinical Laboratory Improvement Amendments of 1988 (CLIA'88). The CLIA'88 regulations precipitated revolutionary and evolutionary changes based in both total quality management and continuous quality improvement principles. The regulations specify minimum requirements for personnel, quality control, and proficiency testing. Under quality assurance, the requirements are more individualized and allow laboratories to meet the needs of their customers while being in compliance with the regulations. Biannual inspection is integral to CLIA'88. However, laboratories can choose other federally approved, "deemed" professional organizations, with regulations equivalent to CLIA'88. Selection of one of these organizations allows for some flexibility in the application of the requirements, and eliminates having federal CLIA'88 inspectors perform the inspection. Since CLIA's inception in 1992, inspectors have noted a decline in the number of deficiencies cited. An improved level of proficiency testing performance also indicates that better quality test results are being provided to clinicians. The quality evolution and revolution will continue in the United States, and a major impetus will be health care reform's mandate to reduce cost. Received: 13 December 1995 Accepted: January 1996     

The relationship between accreditation status and performance in a proficiency test

In the FAPAS proficiency testing scheme, participants are asked to state whether the analytical method used was accredited or not accredited. It is thus possible to compare the stated accreditation status with performance in the scheme. For this purpose, fifty qualifying examples of analyte-test material combination were selected at random from the reports from the year 2006. The accredited/non-accredited subsets of results from each example were subjected to a statistical analysis to determine whether any significant differences between the distributions of results could be detected. Outliers were removed from the datasets before the main statistical tests and considered separately. The inlying data were subjected to non-parametric tests for differences in central tendency and dispersion. A few significant examples were found, but could be reasonably attributed to chance. Among the inliers there were no grounds to reject the overall null hypothesis, that is, that accreditation has no effect on performance. However, the proportion of outliers was about twice as high among the non-accredited group.     

Compliance with GLP standards and management in analytical laboratories: current status

 Analytical laboratories in Japan, operating more often as departments within a company than as independent contractors, have to contend with different good laboratory practice (GLP) standards. Problems also occur in the analytical laboratories which must comply with GLP, good manufacturing practice (GMP) and good clinical practice (GCP) regulations within the same facility. The status of these GLP-complied analytical laboratories is reviewed with regard to assurance program, validation method, laboratory information management, and security systems. The differences in the responsible authorities and scopes under the six GLPs are also briefly described. Analytical tests in GLP are not itemized as a test for accreditation. Therefore, the accreditation of analytical laboratories in Japan is currently granted as a part of ISO 9000 approvals. Received: 27 September 1996 Accepted: 11 November 1996     

MiC in Chemistry Curriculum at the University of Tartu: the current status

The introduction of MiC (Metrology in Chemistry) into the Chemistry Curriculum at the University of Tartu using a two-stage approach is described. As the first stage the topics of MiC are first touched at the beginning of the first analytical chemistry lecture course in the 3rd semester. The emphasis there is on the measurement uncertainty (MU) and its practical estimation (based on the ISO GUM approach). The main purpose of this is to make it clear from the beginning that MU is an integral part of any measurement and to enable the students to estimate MU in the laboratory courses of analytical chemistry (3rd and 4th semesters). As the second stage, MiC is treated in more detail in a dedicated course where also topics, such as reference materials, interlaboratory comparisons, standardization, quality management, accreditation, etc are covered. Received: 6 November 2001 Accepted: 6 December 2001     

Accreditation: a challenge

 This paper describes a real accreditation case from VTT Chemical Technology in Finland. The laboratory has acquired accreditation according to ISO/IEC Guide 25 and EN 45001 for a variety of organic and inorganic environmental tests. The present paper summarizes the reasons for applying for accreditation and selecting the test methods, gives the costs involved, and describes some future developments and views. Also, some details of laboratory intercomparisons and quality system structures are briefly reported.     

The development of a National Accreditation System in South and Southern Africa

 In South African industry there is a strong appreciation of Quality Assurance. More than 1400 companies have been certified as complying with ISO 9000, and this, of course, has resulted in a strong demand for accredited calibration and test facilities. Work on the development of a national calibration service started in 1976, and the South African National Calibration Service (SANCS) was inaugurated in 1980 with 13 calibration laboratories. The early maturity of the SANCS can be judged by the fact that by 1984 it had the technical capability to establish a mutual recognition agreement with a European country. It now has a total of some 191 accredited laboratories, 139 calibration laboratories and 52 testing laboratories. In 1993, the SANCS signed mutual recognition agreements with the CNLA (Taiwan) and the European Co-operation for the Accreditation of Laboratories (EAL). In 1994 it entered the field of testing laboratory accreditation and is already experiencing a strong influence therefrom, and in 1997 it changed its name to National Laboratory Accreditation Service (NLA). In May 1995, the NLA was appointed by the Department of Trade and Industry to establish a South African National Accreditation System (SANAS). Progress with this work up to the present time has been substantial.     

Proficiency testing in analytical chemistry, microbiology, and laboratory medicine – working group discussions on current status, problems, and future directions

Working group (WG) discussions on proficiency testing (PT) held at the joint Eurachem/ EQALM workshop, Borås, Sweden, 24–26 September 2000 are summarized. The discussions focused on aspects of PT and accreditation (WG 1), general aspects of PT in analytical chemistry (WG 2), microbiology (WG 3), and laboratory medicine (WG 4), incorporation of measurement uncertainty into PT schemes (WG 5), international harmonization of PT schemes (WG 6), and the role of PT in the international structure of chemical measurement (WG 7). Current status, problems and future directions are identified. Each WG contained a majority of participants experienced in the subject being covered by that WG, and a few participants with different expertise. This was done to promote cross-fertilization of ideas between sectors, a key objective of the workshop. The WG issues reflected the content of the keynote lectures and some issues were covered from different perspectives by more than one group.