Certified reference materials to support a European thematic strategy for soil protection: the EUROSOILS (IRMM-443) experience.

The recent proposal of thematic strategy for soil protection by the European Commission outlines that knowledge of problems associated with soil has increased considerably based on surveys, monitoring systems and data networks. Although this information is very useful, its value for the policy-making process is limited due to a lack of comparability. From this unsatisfying situation the need arises to develop an EU-wide monitoring system accompanied by suitable matrix reference materials.

Certification of the European Reference Soil Set (IRMM-443--EUROSOILS). Part II. Soil-pH in suspensions of water and CaCl2.

IRMM-443 re-groups a set of six European Reference Soils (EUROSOILS), which had been certified for their adsorption coefficients for atrazine, 2,4-D and lindane (Certification of the European Reference Soil Set (IRMM-443-EUROSOILS)-Part I. Adsorption coefficients for atrazine, 2,4-D and lindane. Sci Total Environ, in press).

Certification of the European reference soil set (IRMM-443--EUROSOILS). Part I. Adsorption coefficients for atrazine, 2,4-D and lindane.

The European Commission has characterised and certified a set of six European soils (the EUROSOILS) under the number IRMM-443. After a successful validation and trial period with a preliminary batch it was decided to produce a new batch of certified reference materials. Part I of this paper describes the certification of adsorption coefficients for atrazine, 2,4-D and lindane in these soils.

Mercury determination in solid phases from application of the modified BCR-sequential extraction procedure: a valuable tool for assessing its mobility in sediments.

The present paper presents a feasibility study for the evaluation of mercury mobility in sediments by application of the modified BCR three-step sequential extraction procedure (BCR-SEP). The aim of the study was to evaluate the effect of acidification, reduction and oxidation processes on mercury mobility from sediments, once the SEP was validated with other trace metals. As extractable mercury amounts were mostly found below detection limits of the advanced mercury analyser (AMA-254) used for measuring the extracts (L.

Collaborative study to improve the quality control of rare earth element determinations in environmental matrices.

In order to control the quality of rare earth determinations in environmental matrices, the Standards, Measurements and Testing Programme (formerly Community Bureau of Reference, BCR) of the European Commission has started a project, the final aim of which is to certify four types of matrices (tuna muscle, mussel tissue, aquatic plant and estuarine sediment) for their contents of a range of rare earth elements (Sc, Y and the lanthanides: La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu). The elements U and Th were added to the study. The first part of this project consisted of an interlaboratory study which aimed to test the feasibility of preparation of environmental reference materials and to detect and remove most of the pitfalls observed in rare earth determinations.

A new mussel certified reference material (CRM 477) for the quality control of butyltin determination in the marine environment.

The analytical techniques used for the determination of butyltin compounds in biological tissues are generally based on a succession of steps (e.g., extraction, derivatization, separation, detection) which are all prone to systematic errors.

Selection and evaluation of sequential extraction procedures for the determination of phosphorus forms in lake sediment.

In order to achieve comparable measurements in the determination of phosphate forms in freshwater sediments, the Standards, Measurements and Testing Programme (formerly BCR) of the European Commission has launched a project the first step of which was to select and evaluate collaboratively existing extraction procedures. This was carried out through expert consultations and a literature survey, and was followed by the organisation of a first interlaboratory study for the evaluation of four sequential extraction schemes, one of which was selected as the most promising method for achieving comparability. This scheme, a modified version of the Williams protocol, was further tested in a second interlaboratory study.

Harmonized protocol and certified reference material for the determination of extractable contents of phosphorus in freshwater sediments--a synthesis of recent works.

An analytical protocol for the determination of the extractable phosphorus contents in freshwater sediments has been harmonized through interlaboratory studies in the frame of the Standards Measurements and Testing Program of the European Commission. A homogeneous and stable sediment reference material has been prepared and certified on the basis of this protocol named SMT protocol, and will be available in spring of 2001. The SMT protocol, together with the reference material, are useful tools in the field of water management, especially at a time when quality assurance and data comparability are of paramount importance in laboratory analysis.

EUROSOILS--a set of CRMs for comparability of soil-measurements.

An overview is given on the development, properties, and application of the European reference soil set--the EUROSOILS. The introduction of this new type of reference material has, for the first time, enabled comparison of data related to the interaction of chemical substances with the soil, and thus, improvement of soil quality. Because of their unforeseen success, a second generation of EUROSOILS had been produced and the range of application extended to other types of measurement related to the soil matrix--soil pH, carbon and nitrogen content, particle-size distribution and cation-exchange capacity.

Recent developments in the field of environmental reference materials at the JRC Ispra.

The production of reference materials for environmental analysis started in the Joint Research Centre at Ispra/Italy in 1972 with the objective of later certification by the BCR, but for obvious budget reasons only a fraction of the total production achieved at Ispra ever reached certification level, although all materials were produced according to the severe quality requirements requested for certified reference materials. Therefore, the materials not destinated to certification are in growing demand as inter-laboratory test materials and as laboratory reference materials, for internal quality control, e.g.

Role of water reuse for enhancing integrated water management in Europe and Mediterranean countries.

Recycling water is an important aspect of water resource and environment management policies, ensuring reliable alternative water resources, reducing environmental pollution and achieving a more sustainable form of development. This paper focuses on wastewater reuse as a strategy for integrated water management. Key economic, financial, regulatory, social and technical factors that help to make water reuse projects successful are reviewed.

Certification of the extractable contents of Cd, Cr, Cu, Ni, Pb and Zn in a freshwater sediment following a collaboratively tested and optimised three-step sequential extraction procedure.

Sequential extraction procedures have been used during the last decades to study and determine trace element mobility in aquatic sediments. However, the results obtained are operationally defined and, therefore, the significance of the analytical results is related to the extraction scheme used. So, there is a need for suitable reference materials for this type of study to enable the validation of the methodologies and to control the quality of the measurements.

A new organic-rich soil reference material certified for its EDTA- and acetic acid- extractable contents of Cd, Cr, Cu, Ni, Pb and Zn, following collaboratively tested and harmonised procedures.

There is an increasing requirement for assessment of the bioavailable metal fraction and the mobility of trace elements in soils upon disposal. One of the approaches is the use of leaching procedures, but the results obtained are operationally defined; therefore, their significance is highly dependent on the extraction protocol performed. So, for this type of study, there is a need for reference materials that allow the quality of measurements to be controlled.

Application of a modified BCR sequential extraction (three-step) procedure for the determination of extractable trace metal contents in a sewage sludge amended soil reference material (CRM 483), complemented by a three-year stability study of acetic acid and EDTA extractable metal content.

This paper provides additional data on a sewage sludge amended soil certified reference material, CRM 483, which was certified in 1997 for its EDTA and acetic acid extractable contents of some trace metals, following standardised extraction procedures. The additional work aimed to test the long-term stability of the material and the applicability of an improved version of the BCR three-step sequential extraction procedure on the sewage sludge amended soil (CRM 483). The paper demonstrates the CRM 483 long-term stability for EDTA and acetic acid extractable contents of Cd, Cr, Cu, Ni, Pb and Zn and gives the results (obtained in the framework of an interlaboratory study) for the extractable contents of the same elements in the CRM 483, following the BCR three-step sequential extraction scheme.

Collaborative evaluation of the analytical state-of-the-art of platinum, palladium and rhodium determinations in road dust.

In order to control the quality of platinum, palladium and rhodium determinations in road dust, the Standards, Measurements and Testing Programme (formerly BCR) of the European Commission has started a project, the final aim of which is to certify a road dust reference material for its contents of platinum group elements. The first part of this project consisted of an interlaboratory study, which aimed to test the feasibility of the preparation of a candidate road dust reference material and to detect and remove most of the pitfalls observed in platinum, palladium and rhodium determinations. This paper presents the main results of this interlaboratory study carried out prior to the certification campaign.

Development of a harmonised phosphorus extraction procedure and certification of a sediment reference material.

A harmonised procedure for the determination of the forms of phosphorus in freshwater sediments, developed in the frame of the European Programme, Standards, Measurements and Testing (SMT) has been used for a certification campaign for a reference material. This operationally defined scheme is a good compromise between method performance and reproducibility. Furthermore, the method is rather simple to implement and could be used by water managers on a routine basis.

Investigations on the water content of candidate reference material CRM 679 cabbage powder.

The determination of the residual water content by thermal methods and especially by Karl Fischer titration in a candidate reference material of the European Commission (candidate CRM 679 cabbage powder) is described and discussed.

On the presence of PCDD/Fs and other chlorinated hydrocarbons in the second generation of the European Reference Soil Set--the EUROSOILS.

The second generation of the European Reference Soil-Set, the so-called EUROSOILS, has been introduced recently. The presence of organic micro-pollutants in this new type of reference materials has already been studied for polycyclic aromatic hydrocarbons, triazines, phenylureas and other pesticides. The already large amount of data concerning the level of different contaminants, the elemental composition and matrix properties is completed by a survey by means of GC/MS on the polychlorinated dibenzodioxins/furans (PCDD/Fs) and other chlorinated hydrocarbons.

River sediment (S-37)--a new analytical quality control material ensuring comparability of chlorinated hydrocarbon analysis during an international environmental study in China.

A sediment reference material (S-37) was prepared as analytical quality control material to be used within an international project on polychlorinated hydrocarbon analysis in two Chinese rivers. The raw material was sampled during a cruise on Yangtse River and transported afterwards to the JRC Ispra for further processing. The material was treated according to the general principles applicable for candidate reference material production.

Quantitative evaluation of the CEEM soil sampling intercomparison.

The aim of the CEEM soil project was to compare and to test the soil sampling and sample preparation guidelines used in the member states of the European Union and Switzerland for investigations of background and large-scale contamination of soils, soil monitoring and environmental risk assessments. The results of the comparative evaluation of the sampling guidelines demonstrated that, in soil contamination studies carried out with different sampling strategies and methods, comparable results can hardly be expected. Therefore, a reference database (RDB) was established by the organisers, which acted as a basis for the quantitative comparison of the participants' results.

Comparative soil sampling in the Dornach site (Switzerland) for soil three-dimensional pollution description.

Fifteen institutions from 13 European countries and Switzerland participated in a comparative test sampling at the Dornach site, near Basel in Switzerland. They received the site description and were asked to develop their own sampling plans, based on their national guidelines for a three-dimensional description of the Pb, Zn, Cu and Cd pollution, with a maximum of 15 samples. The comparative sampling test took place in late August 1997.

European soil sampling guidelines for soil pollution studies.

The soil sampling guidelines used in European countries (ESSG), as kindly provided by the national institutions which participated in the project, have been recorded, studied, evaluated and presented in this paper. The aim has been to ascertain what soil sampling guidelines exist in Europe; to detect similarities and differences (comparable results), advantages and deficiencies; to identify incompatible strategies and evaluate how methodologies might affect data quality; to investigate sources of deviations or uncertainties; to improve comparability and representativeness of soil sampling; to investigate the need for harmonised sampling guidelines; and to develop suggestions for standard operating procedures (SOP). Soil sampling guidelines throughout Europe differ as to whether they are applied by law, or used throughout the country.

Objectives, concept and design of the CEEM soil project.

Within the member countries of the European Union, different strategies and guidelines for the sampling and the preparation of soils are used to investigate soil contamination. As a consequence, there is reasonable doubt that the results gained by applying these different strategies and methods are comparable. In general, the relative contribution of sampling and sample preparation to the total uncertainty in soil contamination studies is a subject of speculation than of knowledge.

Analytical aspects of the CEEM soil project.

In the past, exercises aiming at an assessment of data uncertainty in environmental analysis were usually restricted to the analysis step, while sampling and pre-analytical sample treatment was largely ignored. Collaborative studies on the quantification of sampling errors require, besides a suitable and well characterized test site, the availability of a reference laboratory for the analysis of all of the samples taken in the context of the study by all participants and also test methods which do not contribute large and variable uncertainties due to long and complex analytical methodologies. Here we summarize the major analytical aspects of a European project on the identification and quantification of sampling influences on the determination of lead, cadmium, copper and zinc in soil.

Description of the test area and reference sampling at Dornach.

The selected test area for the comparative evaluation of European methods on sampling and sample preparation of soils (CEEM Soil) at Dornach near Basel (Switzerland) is located at approximately 400 m a.S.l.