title: Preparation and characterization of a soil reference material from a mercury contaminated site for comparability studies.
abstract: The preparation and characterization of a soil reference material (SOIL-1) from a site polluted with mercury due to the past mercury mining in Idrija, Slovenia is reported. Homogeneity tests and intercomparison exercises for total (T-Hg) and methylmercury (MeHg) were performed. In addition, selective sequential extraction was applied for Hg fractionation, and multielemental analyses were performed by k(0) standardization neutron activation analysis (k(0)-INAA) and inductively coupled mass spectrometry (ICP-MS) for other trace elements. Comparison of different analytical methods, as well as the distribution of data were critically evaluated using descriptive statistics and analysis of variance (ANOVA). Due to the nugget effect (cinnabar particles representing more than 90% of the mercury), homogeneity for T-Hg determination was difficult to achieve. The intercomparison exercise indicated that in order to obtain comparable results for total mercury (T-Hg) sample decomposition by HF must be performed. These data are then in good agreement with non-destructive methods such as k(0)-INAA. Accepted reference values calculated taking into account the results obtained by six and three laboratories, respectively, were 67.1+/-11.3 mg kg(-1) for T-Hg and 4.0+/-1.3 ng g(-1) for MeHg (95% confidence intervals). However, the results obtained for Hg fractionation displayed significant differences in the organically bound fraction and elemental Hg. Results obtained by two laboratories using totally different analytical protocols for other elements showed excellent agreement for most elements. In summary, the results obtained for the SOIL-1 sample were of sufficient quality to suggest its use for quality control in laboratories dealing with mercury contaminated soils.
authors.affiliation: Department of Environmental Sciences, Jozef Stefan Institute, Jamova 39, 1001 Ljubljana, Slovenia. david.kocman@ijs.si
authors.forename: David
authors.initials: D
authors.lastname: Kocman
authors.forename: Nicolas S
authors.initials: NS
authors.lastname: Bloom
authors.forename: Hirokatso
authors.initials: H
authors.lastname: Akagi
authors.forename: Kevin
authors.initials: K
authors.lastname: Telmer
authors.forename: Lars
authors.initials: L
authors.lastname: Hylander
authors.forename: Vesna
authors.initials: V
authors.lastname: Fajon
authors.forename: Vesna
authors.initials: V
authors.lastname: Jereb
authors.forename: Radojko
authors.initials: R
authors.lastname: Jaćimović
authors.forename: Borut
authors.initials: B
authors.lastname: Smodis
authors.forename: Justinian R
authors.initials: JR
authors.lastname: Ikingura
authors.forename: Milena
authors.initials: M
authors.lastname: Horvat
mesh_terms: D008628:Mercury / Q000032:analysis*; D008767:Methylmercury Compounds / Q000032:analysis; D012015:Reference Standards; D017524:Slovenia; D012989:Soil Pollutants / Q000032:analysis*
chemical_list: D008767:Methylmercury Compounds; D012989:Soil Pollutants; D008628:Mercury