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Analytical and Bioanalytical Chemistry (v.386, #4)

Advances in analytical techniques for environmental analysis by Stephen A. Wise; Damià Barceló; Philippe Garrigues; Richard Turle (pp. 765-767).

is Chief of the Analytical Chemistry Division at the National Institute of Standards and Technology (NIST) in Gaithersburg, Maryland, USA. He is an Editor of Analytical and Bioanalytical Chemistry. His research interests related to environmental analysis are: the development of chromatographic methods for determination of organic contaminants in environmental matrices, the development of Standard Reference Materials (SRMs) for organic and inorganic contaminants in environmental matrices, and environmental specimen banking procedures. is full Research Professor at IIQAB-CSIC and Head of the Environmental Chemistry Department. He has been a pioneer in the applications of LC–MS to environmental analysis, with the first publication in 1987 and a book in 1996. D. Barceló is a member of the Advisory Board of Analytical and Bioanalytical Chemistry. His scientific focus is on method development and monitoring, and the fate of priority, new, and emerging pollutants, including endocrine-disrupting compounds, by use of GC and LC coupled with advanced tandem and hybrid mass spectrometric analysis combined with bioassays, biosensors, and endocrine effect studies. is a CNRS Research Director and currently Head of the Department of Molecular Sciences (CRCM, FR 1981 CNRS) at the University of Bordeaux 1 with approximately 200 research workers involved in different aspects of chemistry (theory, analysis, environment, spectroscopy, synthesis). His own research interests are analytical aspects (chromatography and spectroscopy) of the detection of organic pollutants and the environmental fate and toxicological effects of these compounds. In recent years he has been involved in the development of biochemical markers as early warning systems for the toxicological evaluation of ecosystems by coordination of large research projects (i.e. BIOMAR, BEEP) supported by the DG Research (European Commission, Brussels). He is also an Editor of Analytical and Bioanalytical Chemistry and the present Chairman of the Division “Chemistry in the Environment” (DCE) of the European Association for Chemical and Molecular Sciences (EuCheMS). has recently taken the position of Deputy Director General-Operations of the CANMET Energy Technology Centre, Ottawa, of Natural Resources Canada. Previously, he spent 15 years with the Environmental Technology Centre of Environment Canada where he was responsible for the development of methods used in different environmental regulations. He is a member of the International Advisory Board of Analytical and Bioanalytical Chemistry and a Fellow of the Chemical Institute of Canada. He has received several awards including the Public Service of Canada Award for his contributions to the acceptance of MAP(c) technology in regulatory methods. His analytical interests are in quality assurance, accreditation, and management of laboratories.

Analytical methods for PCBs and organochlorine pesticides in environmental monitoring and surveillance: a critical appraisal by Derek Muir; Ed Sverko (pp. 769-789).

Analytical methods for the analysis of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) are widely available and are the result of a vast amount of environmental analytical method development and research on persistent organic pollutants (POPs) over the past 30–40 years. This review summarizes procedures and examines new approaches for extraction, isolation, identification and quantification of individual congeners/isomers of the PCBs and OCPs. Critical to the successful application of this methodology is the collection, preparation, and storage of samples, as well as specific quality control and reporting criteria, and therefore these are also discussed. With the signing of the Stockholm convention on POPs and the development of global monitoring programs, there is an increased need for laboratories in developing countries to determine PCBs and OCPs. Thus, while this review attempts to summarize the current best practices for analysis of PCBs and OCPs, a major focus is the need for low-cost methods that can be easily implemented in developing countries. A “performance based” process is described whereby individual laboratories can adapt methods best suited to their situations. Access to modern capillary gas chromatography (GC) equipment with either electron capture or low-resolution mass spectrometry (MS) detection to separate and quantify OCP/PCBs is essential. However, screening of samples, especially in areas of known use of OCPs or PCBs, could be accomplished with bioanalytical methods such as specific commercially available enzyme-linked immunoabsorbent assays and thus this topic is also reviewed. New analytical techniques such two-dimensional GC (2D-GC) and “fast GC” using GC–ECD may be well-suited for broader use in routine PCB/OCP analysis in the near future given their relatively low costs and ability to provide high-resolution separations of PCB/OCPs. Procedures with low environmental impact (SPME, microscale, low solvent use, etc.) are increasingly being used and may be particularly suited to developing countries.

Keywords: PCBs; Organochlorines; Pesticides; POPs; Review; Analysis; GC–ECD; GC–MS; Extraction; Sample preparation and QA/QC

Advances in analytical techniques for polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans and dioxin-like PCBs by Eric J. Reiner; Ray E. Clement; Allan B. Okey; Chris H. Marvin (pp. 791-806).

Analytical techniques for the determination of polychorinated dibenzo-p-dioxins (PCDD), polychlorinated dibenzofurans (PCDF) and dioxin-like PCBs (DLPCB) are reviewed. The focus of the review is on recent advances in methodology and analytical procedures. The paper also reviews toxicology, the development of toxic equivalent factors (TEF) and the determination of toxic equivalent quantity (TEQ) values. Sources, occurrence and temporal trends of PCDD/PCDF are summarized to provide examples of levels and concentration ranges for the methods and techniques reviewed.

Keywords: Review; Polychlorinated dibenzo-p-dioxins; PCDD; Polychlorinated dibenzofurans; PCDF; Dioxin-like PCBs; DLPCB; Extraction; Sample preparation; Analysis; Mass spectrometry; Toxicity; Environmental levels

Instrumental methods and challenges in quantifying polybrominated diphenyl ethers in environmental extracts: a review by Heather M. Stapleton (pp. 807-817).

Increased interest in the fate, transport and toxicity of polybrominated diphenyl ethers (PBDEs) over the past few years has led to a variety of studies reporting different methods of analysis for these persistent organic pollutants. Because PBDEs encompass a range of vapor pressures, molecular weights and degrees of bromine substitution, various analytical methods can lead to discrimination of some PBDE congeners. Recent improvements in injection techniques and mass spectrometer ionization methods have led to a variety of options to determine PBDEs in environmental samples. The purpose of this paper is therefore to review the available literature describing the advantages and disadvantages in choosing an injection technique, gas chromatography column and detector. Additional discussion is given to the challenges in measuring PBDEs, including potential chromatographic interferences and the lack of commercial standards for higher brominated congeners, which provides difficulties in examining degradation and debromination of BDE congeners, particularly for BDE 209.

Keywords: Polybrominated diphenyl ethers; Brominated flame retardants; Methods; Analysis; Review

Advances in the environmental analysis of polychlorinated naphthalenes and toxaphene by John R. Kucklick; Paul A. Helm (pp. 819-836).

Recent advances in the analysis of the chlorinated environmental pollutants polychlorinated naphthalenes (PCNs) and toxaphene are highlighted in this review. Method improvements have been realized for PCNs over the past decade in isomer-specific quantification, peak resolution, and the availability of mass-labeled standards. Toxaphene method advancements include the application of new capillary gas chromatographic (GC) stationary phases, mass spectrometry (MS), especially ion trap MS, and the availability of Standard Reference Materials that are value-assigned for total toxaphene and selected congener concentrations. An area of promise for the separation of complex mixtures such as PCNs and toxaphene is the development of multidimensional GC techniques. The need for continued advancements and efficiencies in the analysis of contaminants such as PCNs and toxaphene remains as monitoring requirements for these compound classes are established under international agreements.

Keywords: Chiral analysis; Separations/Instrumentation; GC; Organic compounds/Trace organic compounds; Pesticides/Endocrine disruptors

Analysis of polychlorinated n-alkanes in environmental samples by F. J. Santos; J. Parera; M. T. Galceran (pp. 837-857).

Polychlorinated n-alkanes (PCAs), also known as chlorinated paraffins (CPs), are highly complex technical mixtures that contain a huge number of structural isomers, theoretically more than 10,000 diastereomers and enantiomers. As a consequence of their persistence, tendency to bioaccumulation, and widespread and unrestricted use, PCAs have been found in aquatic and terrestrial food webs, even in rural and remote areas. Recently, these compounds have been included in regulatory programs of several international organizations, including the US Environmental Protection Agency and the European Union. Consequently, there is a growing demand for reliable methods with which to analyze PCAs in environmental samples. Here, we review current trends and recent developments in the analysis of PCAs in environmental samples such as air, water, sediment, and biota. Practical aspects of sample preparation, chromatographic separation, and detection are covered, with special emphasis placed on analysis of PCAs using gas chromatography–mass spectrometry. The advantages and limitations of these techniques as well as recent improvements in quantification procedures are discussed.

Keywords: Polychlorinated n-alkanes; Chlorinated paraffins; Extraction techniques; Sample clean-up; Environmental analysis; GC-MS

Analysis of polycyclic aromatic hydrocarbons (PAHs) in environmental samples: a critical review of gas chromatographic (GC) methods by Dianne L. Poster; Michele M. Schantz; Lane C. Sander; Stephen A. Wise (pp. 859-881).

Polycyclic aromatic hydrocarbons (PAHs) are frequently measured in the atmosphere for air quality assessment, in biological tissues for health-effects monitoring, in sediments and mollusks for environmental monitoring, and in foodstuffs for safety reasons. In contemporary analysis of these complex matrices, gas chromatography (GC), rather than liquid chromatography (LC), is often the preferred approach for separation, identification, and quantification of PAHs, largely because GC generally affords greater selectivity, resolution, and sensitivity than LC. This article reviews modern-day GC and state-of-the-art GC techniques used for the determination of PAHs in environmental samples. Standard test methods are discussed. GC separations of PAHs on a variety of capillary columns are examined, and the properties and uses of selected mass spectrometric (MS) techniques are presented. PAH literature on GC with MS techniques, including chemical ionization, ion-trap MS, time-of-flight MS (TOF-MS), and isotope-ratio mass spectrometry (IRMS), is reviewed. Enhancements to GC, for example large-volume injection, thermal desorption, fast GC, and coupling of GC to LC, are also discussed with regard to the determination of PAHs in an effort to demonstrate the vigor and robustness GC continues to achieve in the analytical sciences.

Keywords: Polycyclic aromatic hydrocarbons; Gas chromatography; Capillary columns; Mass spectrometry; Environmental samples

Analysis of nitrated polycyclic aromatic hydrocarbons by Barbara Zielinska; Shar Samy (pp. 883-890).

Many nitrated polycyclic aromatic hydrocarbons (NPAH) that are present in low concentrations in the environment and in emission sources have been shown to be mutagenic and/or carcinogenic. This paper reviews the current methods of analysis of these compounds with the emphasis on NPAH measurements in ambient particulate matter samples.

Keywords: Aerosols / Particulates; Nitro-PAH; HPLC; GCMS; LCMS

Polycyclic aromatic sulfur heterocycles as information carriers in environmental studies by Jan T. Andersson; Abdelrahman H. Hegazi; Benedikte Roberz (pp. 891-905).

Polycyclic aromatic hydrocarbons (PAHs) play a huge role in environmental analytical chemistry, both as pollutants and as markers for many processes. On the other hand, polycyclic aromatic sulfur heterocycles (PASHs; heterocyclic compounds related to PAHs) have been studied far less intensely, but such studies may lead to a great deal of information not available through the study of PAHs. Here we discuss analytical aspects of PASHs in environmental matrices and their use as information carriers. Since PASHs accompany PAHs in sampling and work-up, it is not necessary to expend much extra analytical effort in order to analyze them. This work reviews how they can provide information on diverse processes such as petroleum, industrial and vehicular pollution, and sources of air and marine pollution.

Keywords: Sulfur aromatic compounds; PASH; Markers; Environmental chemistry; Separations

Analytical methods for the determination of persistent ingredients of personal care products in environmental matrices by Aaron M. Peck (pp. 907-939).

Concern about the environmental fate and potential effects of synthetic organic chemicals used in soaps, lotions, toothpaste, and other personal care products continues to increase. This review describes procedures used for the analysis of five classes of these compounds–synthetic musk fragrances, antimicrobials, ultraviolet filters, insect repellents, and parabens–in water, sediment, sewage sludge, air, and aquatic biota. The primary focus is on sample extraction and preparation methods for these compounds. Instrumental methods commonly used for these compounds are also discussed.

Keywords: HHCB; Sunscreen agents; Triclosan; Triclocarban; DEET; Emerging compounds

Multi-residue analytical methods using LC-tandem MS for the determination of pharmaceuticals in environmental and wastewater samples: a review by Meritxell Gros; Mira Petrović; Damià Barceló (pp. 941-952).

Multi-residue analytical methodologies are becoming the preferred and required tools against single group analysis, as they provide wider knowledge about the occurrence of pharmaceuticals in the environment necessary for further study of their removal, partition and ultimate fate. However, simultaneous analysis of compounds from different groups with quite different physico-chemical characteristics requires a compromise in the selection of experimental conditions, which in some cases are not the best conditions for all the analytes studied. In this article, an overview of analytical methodologies focusing on the simultaneous determination of acidic, neutral and basic compounds belonging to different therapeutical classes is presented. The state-of-the-art of LC-MS/MS for multi-class analysis is reviewed, highlighting the specific requirements for such analysis.

Keywords: Multi-residue methods; Pharmaceuticals; Environmental analysis; Tandem mass spectrometry

Environmental analysis of fluorinated alkyl substances by liquid chromatography–(tandem) mass spectrometry: a review by Marta Villagrasa; Maria López de Alda; Damià Barceló (pp. 953-972).

Fluorinated alkyl substances (FASs) are widely distributed contaminants that have been found in many environmental, human and biological samples throughout the world. Perfluorochemicals are used in many industry and consumer products, such as polymers and surfactants, because they have unique and useful properties (they are stable, chemically inert and generally unreactive). However, these compounds have also been found to be toxic, persistent and bioaccumulative. In recent years various analytical methods have been developed for the analysis of FASs in environmental samples. Most of these methods are based on liquid chromatography coupled to mass spectrometry (LC–MS) or tandem mass spectrometry (LC–MS/MS), since this is considered to be the technique of choice. This article reviews the various LC–(tandem)MS methods described so far for the analysis of FASs in water, sediment, sludge and biota samples. It discusses the main experimental conditions used for sample pretreatment and for analysis as well as the most relevant problems encountered and the limits of detection achieved.

Keywords: Perfluorochemicals; Fluorinated alkyl substances; Liquid chromatography–mass spectrometry; Environmental analysis

Determination of antimicrobial residues and metabolites in the aquatic environment by liquid chromatography tandem mass spectrometry by M. Silvia Díaz-Cruz; Damià Barceló (pp. 973-985).

Antimicrobials are used in large quantities in human and veterinary medicine. Their environmental occurrence is of particular concern due to the potential spread and maintenance of bacterial resistance. After intake by the organisms, the unchanged drug and its metabolized forms are excreted and enter wastewater treatment plants where they are mostly incompletely eliminated, and are therefore eventually released into the aquatic environment. The reliable detection of several antimicrobials in different environmental aqueous compartments is the result of great improvements achieved in analytical chemistry. This article provides an overview of the more outstanding analytical methods based on liquid chromatography tandem mass spectrometry, developed and applied to determine antimicrobial residues and metabolites present in surface, waste, and ground waters.

Keywords: Antimicrobials; Pharmaceuticals; Solid-phase extraction; Liquid chromatography tandem mass spectrometry; Water analysis

Potential of liquid chromatography/time-of-flight mass spectrometry for the determination of pesticides and transformation products in water by Juan V. Sancho; Óscar J. Pozo; María Ibáñez; Félix Hernández (pp. 987-997).

Until now, time-of-flight (TOF) mass analysers have only been very rarely used in pesticide residue analysis (PRA) of water samples. However, the inherent characteristics of TOF MS make these analysers well-suited to this field, mainly for qualitative purposes. Thus, the high sensitivity obtained from full-scan acquisition in comparison to other MS analysers and the high resolution of TOF MS suggest its suitability for screening purposes; it also increases the multiresidue capabilities of methods based on it and decreases the chance of recording false positives. Although these characteristics can also be helpful for quantification, confirmation and elucidation, some limitations on the use of TOF for these purposes have been observed. These limitations are more noticeable when dealing with samples containing very low analyte concentrations, which is the normal situation for PRA in water. The use of hybrid quadrupole–time-of-flight instruments (QTOF) minimises the limitations of TOF, facilitating the simultaneous detection and unequivocal confirmation of pesticides found in the sample. Additionally, the acquisition of accurate product ion full-scan mass spectra can help to elucidate the structures of unknown compounds. In this paper, the potential of TOF and QTOF hyphenated to liquid chromatography for PRA in water is explored, emphasizing both the advantages and limitations of this approach for screening, quantification, confirmation and elucidation purposes. Emphasis is placed on the determination of polar pesticides and transformation products—the analytes that fit well with LC–API–(Q)TOF MS technology.

Keywords: Time of flight; Hybrid quadrupole–time-of-flight; Mass spectrometry; Pesticide residue analysis; Transformation products; Water

Aluminium speciation in environmental samples: a review by Janez Ščančar; Radmila Milačič (pp. 999-1012).

Because of its toxic effects on living beings, Al may represent an environmental hazard, particularly under increased acidic conditions. Growing environmental concern over the presence of increased Al concentrations in soil solutions and fresh waters resulted in the development of numerous analytical techniques for the determination of Al species. Al has a very complex chemistry that is significantly influenced by pH. Different Al species are present in environmental solutions, and many of them are unstable. Contamination of samples and reagents by extraneous Al represents an additional problem in speciation of Al at trace concentrations. Due to these reasons quantitative determination of particular chemical forms of Al is still a very difficult task for analytical chemists. The most important analytical methodologies of the last decade and new trends for the speciation of Al in environmental samples are comprehensively reviewed here.

Keywords: Al speciation; Environmental samples; Analytical methodologies

Comprehensive two-dimensional gas chromatography (GC×GC) in environmental analysis and monitoring by Ognjen Pani; Tadeusz Górecki (pp. 1013-1023).

Compared to conventional one-dimensional gas chromatography (1D-GC), comprehensive two-dimensional gas chromatography (GC×GC) offers increased peak capacity, improved resolution and enhanced mass sensitivity. In addition, it generates structured two-dimensional (2-D) chromatograms, which aids in the identification of compound classes. Sample preparation procedures can often be minimized, or even eliminated in some cases, due to the superior separating power offered by the technique. All of these advantages make GC×GC a very powerful tool in environmental analysis involving the determination of trace levels of toxic compounds in complex matrices. This review paper summarizes and examines the historical and recent GC×GC applications in environmental analysis and monitoring.

Keywords: Comprehensive two-dimensional gas chromatography (GC×GC); Environmental analysis; PCBs/PCDDs/PCDFs; Pesticides; Air analysis

Biosensors as useful tools for environmental analysis and monitoring by Sara Rodriguez-Mozaz; Maria J. Lopez de Alda; Damià Barceló (pp. 1025-1041).

Recent advances in the development and application of biosensors for environmental analysis and monitoring are reviewed in this article. Several examples of biosensors developed for relevant environmental pollutants and parameters are briefly overviewed. Special attention is paid to the application of biosensors to real environmental samples, taking into consideration aspects such as sample pretreatment, matrix effects and validation of biosensor measurements. Current trends in biosensor development are also considered and commented on in this work. In this context, nanotechnology, miniaturisation, multi-sensor array development and, especially, biotechnology arise as fast-growing areas that will have a marked influence on the development of new biosensing strategies in the near future.

Keywords: Biosensors; Environmental analysis; Review; Trends

Pressurized liquid extraction in environmental analysis by Michele M. Schantz (pp. 1043-1047).

A critical evaluation of recent literature utilizing pressurized liquid extraction (PLE) for environmental analysis is presented by compound class. Overall, the extraction efficiency of PLE, using the appropriate solvent, temperature and pressure for extraction, is similar to that of Soxhlet extraction. PLE has been used for some classes of compounds that are thermally labile (e.g., explosives) and may require acidic conditions for extraction (e.g., organometallic compounds). References to recent applications are presented emphasizing studies which utilize unspiked, natural matrices and studies that compare PLE to alternate extraction techniques.

Keywords: Pressurized liquid extraction; Pressurized fluid extraction; Accelerated solvent extraction; PLE; PFE; ASE

Applications of microwave-assisted processes (MAP™) to environmental analysis by Jacqueline M. R. Bélanger; J. R. Jocelyn Paré (pp. 1049-1058).

The use of microwave-assisted extraction has gained wide acceptance as a powerful tool for the recovery of environmental contaminants and their subsequent analysis. This paper reviews the historical and fundamental basis of the technology. It also provides a cursory review of the current state-of-the-art and literature (2000–2006) in the area of environmental analysis in addition to providing a critical review of the level of efforts being devoted to its further development.

Keywords: Microwave-assisted processes (MAP); Microwave-assisted extraction (MAE); Microwave sample preparations; Environmental contaminants analysis; Extraction of environmental contaminants

SPME in environmental analysis by Gangfeng Ouyang; Janusz Pawliszyn (pp. 1059-1073).

Recent advances in the use of solid-phase microextraction (SPME) in environmental analysis, including fiber coatings, derivatization techniques, and in-tube SPME, are reviewed in this article. Several calibration methods for SPME, including traditional calibration methods, the equilibrium extraction method, the exhaustive extraction method, and several diffusion-based calibration methods, are presented. Recent developed SPME devices for on-site sampling and several applications of SPME in environmental analysis are also introduced.

Keywords: Solid-phase microextraction; Environmental analysis; Calibration

Sampling of water, soil and sediment to trace organic pollutants at a river-basin scale by Alain Hildebrandt; Sílvia Lacorte; Damià Barceló (pp. 1075-1088).

Sampling is considered a crucial step in the analysis of organic compounds in the environment. This review describes field sampling techniques and provides detailed step-by-step procedures for collection and preservation of all major environmental matrices (water, sediment and soil) integrated as part of the river-basin water cycle. Attention is given to the prerequisites for obtaining reliable samples, and the practical issues of sample collection (planning, field sampling, sampling strategies and equipment and data quality assessment) are considered. Considering the heterogeneity of environmental matrices, special considerations for each matrix are given to solve typical problems and to find the most appropriate solutions to ensure the quality of the sample. The procedures described in the next sections are commonly used protocols that reflect true field conditions and current state-of-the-art techniques used in the sampling of organic compounds. The aim is to signify the importance of sampling to the overall analytical procedure. Finally, quality control issues to be considered in environmental sampling are given.

Keywords: Sampling; Environment; Trace; Organic; Pollutant

Determination of complex mixtures of volatile organic compounds in ambient air: an overview by D. K. W. Wang; C. C. Austin (pp. 1089-1098).

This article reviews developments in the sampling and analysis of volatile organic compounds (VOCs) in ambient air since the 1970s, particularly in the field of environmental monitoring. Global monitoring of biogenic and anthropogenic VOC emissions is briefly described. Approaches used for environmental monitoring of VOCs and industrial hygiene VOC exposure assessments are compared. The historical development of the sampling and analytical methods used is discussed, and the relative advantages and disadvantages of sorbent and canister methods are identified. Overall, there is considerable variability in the reliability of VOC estimates and inventories. In general, canister methods provide superior precision and accuracy and are particulary useful for the analysis of complex mixtures of VOCs. Details of canister methods are reviewed in a companion paper.

Keywords: Air analysis; Volatile organic compound; VOC; Environmental monitoring; Industrial hygiene; Canister; Sorbent; GC/MS

Determination of complex mixtures of volatile organic compounds in ambient air: canister methodology by D. K. W. Wang; C. C. Austin (pp. 1099-1120).

Canister methodology is applicable to 150 polar and nonpolar VOCs found in ambient air from parts-per-billion by volume (ppbv) to parts-per-million (ppmv) levels, and has been validated at parts-per-trillion (pptv) levels for a subset of these analytes. This article is a detailed review of techniques related to the collection of volatile organic compounds (VOCs) in evacuated Summa and fused-silica-lined canisters, and their analysis by gas chromatography/mass spectrometry (GC/MS). Emphasis is placed on canister cleaning, VOC stability in canisters, sample dilution, water management, and VOC cryogenic and sorbent preconcentration methods. A wide range of VOC preconcentration and water management methods are identified from the literature, and their relative merits and disadvantages are discussed. Examples of difficulties that commonly arise when processing canister samples are illustrated, and solutions to these problems are provided.

Keywords: Air analysis; TO-14, TO-14A, TO-15; Volatile organic compound; VOC; Environmental monitoring; Industrial hygiene; Canister; Summa; Fused-silica-lined; Sorbent; Water management; GC/MS

Certified reference materials for inorganic and organic contaminants in environmental matrices by Franz Ulberth (pp. 1121-1136).

Chemical measurements often constitute the basis for informed decision-making at different levels in society; sound decision-making is possible only if the quality of the data used is uncompromised. To guarantee the reliability and comparability of analytical data an intricate system of quality-assurance measures has to be put into effect in a laboratory. Reference materials and, in particular, certified reference materials (CRMs) are essential for achieving traceability and comparability of measurement results between laboratories and over time. As in any other domain of analytical chemistry, techniques used to monitor the levels and fate of contaminants in the environment must be calibrated using appropriate calibration materials, and the methods must be properly validated using fit-for-purpose matrix-matched CRMs, to ensure confidence in the data produced. A sufficiently large number of matrix CRMs are available for analysis of most elements, and the group of chemicals known as persistent organic pollutants, in environmental compartments and biota. The wide variety of analyte/level/matrix/matrix property combinations available from several suppliers enables analysts to select CRMs which sufficiently match the properties of the samples they analyse routinely. Materials value-assigned for the so-called emerging pollutants are scarce at the moment, though an objective of current development programmes of CRM suppliers is to overcome this problem.

Keywords: Certified reference materials; CRM; Environmental chemistry; Quality assurance; Quality control; Uncertainty; Traceability

Standard Reference Materials^® (SRMs) for measurement of inorganic environmental contaminants by Rolf Zeisler; Karen E. Murphy; Donald A. Becker; W. Clay Davis; W. Robert Kelly; Stephen E. Long; John R. Sieber (pp. 1137-1151).

NIST has developed an extensive collection of environmental SRMs, starting with fuel and biologically related materials in the late 1960s and now encompassing all sectors of environmental research. Advances in analytical methodology, including multi-element isotope-dilution mass spectrometry (IDMS) and expanded instrumental neutron-activation analysis (INAA) capabilities, enable value assignment based on fewer but better-characterized independent analytical techniques. The special advantages of IDMS for determination of S and Hg and for multi-element characterization of small-sample air particulate matter (SRM 2783) by IDMS and INAA are emphasized. Developments in materials production include the issuance of fresh-frozen biological materials and of jet-milled natural-matrix materials with improved homogeneity, including highly homogeneous air particulate matter and sediment SRMs for small-sample analytical techniques.

Keywords: Cryogenic processing; Homogeneity; Instrumental neutron-activation analysis; Isotope-dilution mass spectrometry; Mercury; Optical-emission spectrometry; Sulfur; Trace elements; X-ray fluorescence spectrometry

Standard reference materials (SRMs) for determination of organic contaminants in environmental samples by Stephen A. Wise; Dianne L. Poster; John R. Kucklick; Jennifer M. Keller; Stacy S. VanderPol; Lane C. Sander; Michele M. Schantz (pp. 1153-1190).

For the past 25 years the National Institute of Standards and Technology (NIST) has developed certified reference materials (CRMs), known as standard reference materials (SRMs), for determination of organic contaminants in environmental matrices. Assignment of certified concentrations has usually been based on combining results from two or more independent analytical methods. The first-generation environmental-matrix SRMs were issued with certified concentrations for a limited number (5 to 10) of polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs). Improvements in the analytical certification approach significantly expanded the number and classes of contaminants determined. Environmental-matrix SRMs currently available include air and diesel particulate matter, coal tar, marine and river sediment, mussel tissue, fish oil and tissue, and human serum, with concentrations typically assigned for 50 to 90 organic contaminants, for example PAHs, nitro-substituted PAHs, PCBs, chlorinated pesticides, and polybrominated diphenyl ethers (PBDEs).

Keywords: Reference materials; Standard reference materials; Hydrocarbons (halogenated | polycyclic); Organic compounds / trace organic compounds; Certified reference materials

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Analytical and Bioanalytical Chemistry (v.386, #4)