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S Theocharopoulos

Publications and source records attributed to S Theocharopoulos.

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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. For this purpose, the first European soil sampling inter-comparison test was organised as a project under the Standards, Measurement and Testing Programme of the European Commission. The aim of this project was to analyse and to compare the existing guidelines, the degree and the state of standardisation in this field in the European countries, and to compare their results when applied on the same test area under comparable conditions by representative sampling teams. The results of the project in general demonstrate that sampling and sample preparation errors reach about the same order of magnitude as errors caused in the chemical analysis. However, there are great differences depending on the elements investigated and their concentration ranges, as well as on pedological and land-use conditions in the test area. Consequently, sampling and sample preparation require the same attentiveness and equivalent measures for quality assurance (QA) and quality control (QC) as the chemical analysis, which has not been the case up to now. Insufficient comparability of the results is illustrated by the fact that different participants arrive at different conclusions for up to 61% of tested soil quality criteria (e.g. threshold levels). The methods and results of the project are presented in detail in the six following papers within this volume. The following 13 papers present some key studies and specific contributions of the participants, as well as synoptical papers of the invited experts in standardisation and accreditation.

Environmental Monitoring↗

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. on the north-west rolling footslope of the Jura mountain chain that has a temperate climate. The area is known to be airborne polluted by emissions of a non-ferrous metal recycling plant. The geology is dominated by Jurassic limestone and (decarbonated) loess loam. The land use is deciduous forest (beech, oak) in the upper part and traditional cherry orchards with permanent grassland which have mostly been converted into arable land. The detailed soil survey distinguishes four different soil mapping units in the test area of 0.61 ha. The reference sampling was performed in a 190-m-long and 20-40 m large transect area following four devices: (1) composite samples (0-10 cm and 0-20 cm), each from 25 stratified single samples of 61 squares of 10 x 10 m; (2) hypotheses and soil horizon-based composite samples at nine locations; (3) horizon-related samples from the four described soil profiles representing the mapping units; and (4) three soil cores with 5-cm interval samples taken in the major land use units. Altogether 301 reference soil samples were taken.

Environmental Monitoring↗

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. The participant group included the leading soil analysis laboratories in Europe; the test site at Dornach (CH) was well suited for the purpose and showed high metal gradients and differentiated land use. The analytical methods (wavelength-dispersive X-ray fluorescence spectrometry and solid-state Zeeman AAS) used in the study showed stable performance characteristics within the confidence interval of the certified reference materials used for the measurement quality control over the entire project period. Additionally, double-blind tests on split samples showed agreement of data in very narrow limits thus demonstrating the reliability of the reference database.

Databases, Factual↗

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. The detected deviations were related to the methodological details of the individual strategies. The comparative evaluation concept consisted of three steps: The first step was a comparison of the participants' samples (which were both centrally and individually analysed) between each other, as well as with the reference data base (RDB) and some given soil quality standards on the level of concentrations present. The comparison was made using the example of the metals cadmium, copper, lead and zinc. As a second step, the absolute and relative deviations between the reference database and the participants' results (both centrally analysed under repeatability conditions) were calculated. The comparability of the samples with the RDB was categorised on four levels. Methods of exploratory statistical analysis were applied to estimate the differential method bias among the participants. The levels of error caused by sampling and sample preparation were compared with those caused by the analytical procedures. As a third step, the methodological profiles of the participants were compiled to concisely describe the different procedures used. They were related to the results to find out the main factors leading to their incomparability. The outcome of this evaluation process was a list of strategies and methods, which are problematic with respect to comparability, and should be standardised and/or specified in order to arrive at representative and comparable results in soil contamination studies throughout Europe. Pre-normative recommendations for harmonising European soil sampling guidelines and standard operating procedures have been outlined in Wagner G, Desules A, Muntau H, Theocharopoulos S. Comparative Evaluation of European Methods for Sampling and Sample Preparation of Soils for Inorganic Analysis (CEEM Soil). Final Report of the Contract SMT4-CT96-2085, Sci Total Environ 2001;264:181-186. Wagner G, Desaules A, Munatu H. Theocharopolous S, Quevauvaller Ph. Suggestions for harmonising sampling and sample pre-treatment procedures and improving quality assurance in pre-analytical steps of soil contamination studies. Paper 1.7 Sci Total Environ 2001b;264:103-118.

Environmental Monitoring↗

Harmonisation and quality assurance in pre-analytical steps of soil contamination studies--conclusions and recommendations of the CEEM Soil project.

The paper summarises the project's results and consequences including expert's statements. Based on sampling strategies and methodological details which have been recognised to be critical for the comparability of the results of soil contamination studies, recommendations are given towards harmonisation of soil sampling guidelines, improvement of quality assurance of pre-analytical steps and inclusion of soil sampling into accreditation systems. Recommended approaches to improve QA and QC in soil sampling are: harmonised guidelines; specified SOPs; written sampling (strategy) plans; defined qualification and experience of sampling personnel; sampling records; regular interlaboratory comparisons (proficency tests) for sampling; and inclusion of sampling and sample preparation into accreditation procedures. Needs for further research in the field of pre-analytical phases of soil contamination studies are outlined and further R&D projects are encouraged.

Accreditation↗