The establishment of an Australian National Analytical Reference Laboratory (NARL)

 The National Analytical Reference Laboratory (NARL) was established by the Commonwealth Government within the Australian Government Analytical Laboratories (AGAL) Public Interest Programme in 1997, to help provide Australian scientists with the chemical standards they need to make reliable measurements. Reliable chemical measurements are vital to many aspects of our social and economic life including public health, environmental control, industrial productivity, trade innovation and government regulation. Mutual recognition of measurement results and the avoidance of costly disputes require the development of a structured and common system of measurement. Working-level measurements should be directly linked to national standards, which are themselves interlinked through international comparisons. Although metrology in chemistry is still in its infancy, increasing numbers of countries are establishing facilities to serve both national needs and to contribute to the international measurement system. The aim at NARL is to lead the development of an Australian chemical measurement system, which is harmonized with similar systems in other countries. This paper was presented at the Co-operation on Traceability in Analytical Chemistry (CITAC) symposium on Analytical Quality Assurance for the Twenty-first Century, held in Sydney on 15–16 October 1998. It describes the rationale for establishing NARL, the process of getting it started, the positioning, aims and strategy of NARL, the development of its work programme and plans for both national and international collaboration. If you would like more information or would like to contribute to the work of NARL please contact us at the above address.     

REMCO — The ISO council committee on reference materials

Summary The purpose of this paper is to provide readers with an insight into the work of REMCO, the world's main body for considering matters related to the production and use of reference materials. The terms of reference for REMCO and its three task groups are given. Contents of the four ISO Guides issued by REMCO illustrate the range of topics covered in the work of the committee.     

Analytical chemistry at Srgonne National Laboratory,Argonne, Illinois,USA

Journal of Radioanalytical and Nuclear Chemistry -     

Analytical strategy for the chemical characterization of biological reference materials

The analytical strategy for the elemental chemical characterization of biological reference materials followed during a recently completed Reference Material development endeavour is discussed. Characterization, the assignment of reliable values to total elemental concentrations of a wide range of elements, poses the most difficult challenge in the scheme of reference material (RM) production. A review is presented of the many factors considered that significantly impinged on the conduct and outcome of the complex analytical characterization exercise. Major considerations were: (1) analytical elemental characterization philosophy, (2) analyte selection, (3) selection of analytical methodologies, (4) statistical protocols, (5) in-house characterization, (6) assessment of material homogeneity (7) cooperative interlaboratory characterization campaign, (8) data evaluation and (9) calculation of concentration values and associated uncertainties.Contribution no. 94-47 from Centre for Land and Biological Resources Research     

A review of the DNA standard reference materials developed by the National Institute of Standards and Technology

The Standard Reference Materials Program at the US National Institute of Standards and Technology (NIST) has three human DNA standard reference materials (SRM 2390, SRM 2391a, and SRM 2392) currently available¹ (Orders and requests for information concerning these SRMs should be directed to the Standard Reference Materials Program, National Institute of Standards and Technology, 100 Bureau Drive, Stop 2321, Gaithersburg, MD 20899-2321, Telephone (301) 975-6776, FAX: (301) 948-3730.) [1, 2]. Both the DNA profiling SRM 2390 and the polymerase chain reaction (PCR)-based DNA profiling SRM 2391a are intended for use in forensic and paternity identifications, for instructional law enforcement, or for non-clinical research purposes and are not intended for clinical diagnostics. The mitochondrial DNA (mtDNA) SRM 2392 is to provide standardization and quality control when performing PCR and sequencing any segment or the entire 16,569 base pairs that comprise human mitochondrial DNA. SRM 2392 is designed for use by the forensic, medical, and toxicological communities for human identification, disease diagnosis or mutation detection.     

A review of the DNA standard reference materials developed by the National Institute of Standards and Technology

The Standard Reference Materials Program at the US National Institute of Standards and Technology (NIST) has three human DNA standard reference materials (SRM 2390, SRM 2391a, and SRM 2392) currently available [1, 2]. Both the DNA profiling SRM 2390 and the polymerase chain reaction (PCR)-based DNA profiling SRM 2391a are intended for use in forensic and paternity identifications, for instructional law enforcement, or for non-clinical research purposes and are not intended for clinical diagnostics. The mitochondrial DNA (mtDNA) SRM 2392 is to provide standardization and quality control when performing PCR and sequencing any segment or the entire 16,569 base pairs that comprise human mitochondrial DNA. SRM 2392 is designed for use by the forensic, medical, and toxicological communities for human identification, disease diagnosis or mutation detection.     

Analytical methodology/laboratory performance during the characterization of biological reference materials

A database from a recently completed multilaboratory characterization campaign of elemental concentration values in Biological Reference Materials has been evaluated and intercompared concerning method/laboratory performances and concentrations obtained therefrom with best estimate concentration values for a wide range of elements and materials. Performance parameters included within and between laboratory precision, accuracy (bias), element applicability and matrix effects. A brief assessment is presented of methodology/laboratory performance during this characterization exercise for the seven generic methods: atomic absorption spectrometry (AAS), atomic emission spectrometry (AES), mass spectrometry (MS), neutron activation analysis (NAA), X-ray emission spectrometry (XRES), (molecular) light absorption spectrometry (light AS) and electrochemistry (EC) coupled with a variety of sample treatment, ashing and digestion approaches.Contribution no. 94-46 from Centre for Land and Biological Resources Research     

Development of the analytical methods and reference materials program for dietary supplements at the National Institutes of Health

The need for validated analytical methods and reference materials to identify and measure constituents in dietary supplements is essential. Such methods allow for the documentation that products meet manufacturer's specifications and contain what their labels declare. In March 2003, the U.S. Food and Drug Administration issued a proposed rule that would establish specific current good manufacturing practices for dietary supplements. This proposed rule requires that companies create a quality control unit to set specifications and ensure compliance with these specifications using scientifically valid procedures. This report provides insights and lessons learned from 3 meetings the Office of Dietary Supplements (ODS) at the National Institutes of Health helped organize. These meetings were structured to (1) educate individuals about the importance and need for validated analytical methods and reference materials to identify and quantify constituents of dietary supplements; (2) identify resources required to fulfill this need; and (3) serve as a platform to obtain input from interested parties to help frame the research agenda for the Dietary Supplements Methods and Reference Materials Program within ODS. Stakeholder's opinions and views expressed at these 3 meetings are outlined in this report.     

The synthesis and characterization of pure substance reference materials for forensic, agricultural and drugs-in-sport analysis

 The paper reports work on the synthesis, purification and certification of pure substance (organic) reference materials as conducted within the National Analytical Reference Laboratory (NARL). Areas of interest include illicit drugs, agricultural and veterinary chemicals, and steroids and steroid metabolites and their deuterates. The discussion covers the prioritization of work requirements, procedures for synthesis and production, quality assurance, characterization, homogeneity, storage and stability testing, and certification of materials. Future plans for establishing traceability are also discussed.     

Reference materials for PAHs in foodstuffs: Results of the certification exercise of two coconut oil reference materials

This certification exercise was the final stage of a stepwise interlaboratory study approach, organized within the SMT-program of the EC, for the development of certified reference materials (CRMs) for the determination of PAHs in foodstuffs. The certification exercise was carried out by thirteen European laboratories using a variety of extraction and clean-up procedures and different analytical procedures. Two different coconut oil materials were certified for their mass fractions of six selected PAHs. Received: 25 May 1997 / Revised: 5 September 1997 / Accepted: 28 September 1997     

Reference materials for PAHs in foodstuffs: Results of the certification exercise of two coconut oil reference materials

This certification exercise was the final stage of a stepwise interlaboratory study approach, organized within the SMT-program of the EC, for the development of certified reference materials (CRMs) for the determination of PAHs in foodstuffs. The certification exercise was carried out by thirteen European laboratories using a variety of extraction and clean-up procedures and different analytical procedures. Two different coconut oil materials were certified for their mass fractions of six selected PAHs.     

Analytical quality control by solid sampling GFAAS in the production of animal tissue reference materials: lead and cadmium in bovine liver reference materials

Summary The function of solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) in the laboratory-internal preparation, production and standardization of bovine liver reference material is described. Analytical quality assurance was achieved by using a wet digestion decomposition procedure and GFAAS (WD-GFAAS) as well as three different methods of SS-GFAAS. It will be shown, that SS-GFAAS is an adequate and efficacious method of analytical quality control in the production of reference materials. Details are given about the preliminary steps of sample selection and preparation, applying SS-GFAAS both as a screening method and for the detection of contamination during the production of the reference materials. The element contents of the four bovine liver materials measured after decomposition with nitric acid in the open system by GFAAS and also by Flame-AAS, using the slotted tube atom trap, are compared statistically with the results obtained by SS-GFAAS. In solid sampling analyses three different systems were applied: a solid sampling ZAA-spectrometer with platform-boat, a D₂AA-spectrometer with solid sampling graphite tube and platform-drawer and an autoprobe-D₂AA-spectrometer with solid sampling autoprobe and graphite tube.     

Analytical dependences between first order derivatives at the critical point of a pure substance

The finiteness and positive value of the slope of the saturation curve at the critical point according to its location in the region of a thermodynamic surface restricted by the curves of inversion and saturation are substantiated. It is shown that any two derivatives of the first order formed with respect to volume, internal energy, entropy, enthalpy, and the Helmholtz energy, one of which is taken at a fixed value of pressure and the other at a fixed value of temperature, are equal in the critical state. New sets of the critical conditions for a pure substance are obtained.     

Fit-for-purpose shellfish reference materials for internal and external quality control in the analysis of phycotoxins

The need for reference materials for quality control of analysis of foodstuffs has been stressed frequently. This has been particularly true in the phycotoxins field, where there is a great shortage of both pure calibration standards and reference materials. Worldwide there are very few independent bodies that produce certified reference materials for phycotoxins, the main producers currently being the National Research Council Canada and the Japanese Food Research Laboratory. Limited availability of contaminated shellfish and algae, as well as the time and knowledge necessary for the production of adequate reference materials, continuously lead to limited editions of certified reference materials and even more limited production of in-house reference materials. The restricted availability of in-house quality control materials promotes the rapid use of the limited certified reference materials, which in turn hampers the production of the suite of materials required globally for complete protection of public health. This paper outlines the various options that analysts can pursue in the use of reference materials for internal and external quality control, with a view to optimising the efforts of both reference materials users and reference materials producers. For this purpose, the logical sequence is reviewed from the discovery of a new bioactive compound in shellfish, through initial method development up to regulation for food safety purposes including accepted reference methods. Subsequently, the requirements for and efforts typically spent in the production and characterisation of laboratory reference materials, certified reference materials and other test materials used in inter-laboratory studies or proficiency testing, in the area of marine biotoxins are evaluated. Particular emphasis is put on practical advice for the preparation of in-house reference materials. The intricate link between reference material characterisation and method performance is outlined to give guidance on the appropriate in-house method validation in the rapidly developing field of phycotoxins.      

Preparation and characterization of organic calibration solutions for development of certified reference materials at the National Metrology Institute of Japan

Certified reference materials (CRMs) are playing an increasingly important role in environmental monitoring in Japan. The National Metrology Institute of Japan (NMIJ)/National Institute of Advanced Industrial Science and Technology (AIST) has been developing CRMs of organic calibration solutions since 2003, and has issued several NMIJ CRMs. The development of these materials was conducted at the NMIJ in cooperation with candidate material producers. The freezing-point depression method was principally adopted for assessment of the purity of starting materials to give reliable certified values. Gas chromatography with flame ionization detection (GC–FID) and/or high-performance liquid chromatography (HPLC), which are based on independent principles and whose levels of accuracy are well evaluated, were applied in combination with other methods to avoid any possible analytical bias. Purity assessment is outlined for two typical examples, 1,1-dichloro-2,2-bis(p-chlorophenyl)ethane (p,p′-DDD) and 1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane (p,p′-DDT), which were used as starting materials for a CRM under development. Methods adopted for gravimetric preparation and ampouling of solutions were qualified and optimized to reduce the uncertainties of certified values due to these factors. Furthermore, a new experimental scheme for assessment of stability and preparation variation is proposed for the proper estimation of uncertainties. Presented at BERM-11, October 2007, Tsukuba, Japan.     

第12届全国大学生化学实验邀请赛物理化学实验试题解析

介绍了第12届全国大学生化学实验邀请赛无机及分析化学实验操作试题的命题思路,总结实验成绩,分析实验操作考试中存在的主要问题。