Abstract
Cyanides are among the most important inorganic pollutants to be tested and monitored in environmental compartments. They can be distinguished and determined as free cyanide, weak acid dissociable cyanide or as total cyanide. However, in any case obtained, measurement results are operationally defined referring to the applied analytical method. In 2011, the International Standard ISO 11262 has been published which specifies a normative analytical method for the determination of total cyanide in soil. The objective of the project described in this paper was to provide the first soil reference material (CRM) certified for its mass fraction of total cyanide on the basis of this standard. A total of 12 German laboratories with proven experience in the determination of cyanides in environmental samples participated in the certification study. Measurement results were evaluated in full compliance with the requirements of ISO Guide 35. Taking into account the results of the inter-laboratory comparison as well as the outcome of the homogeneity and stability studies, a certified mass fraction of total cyanide of 21.1 mg/kg and an expanded uncertainty (k = 2) of 1.3 mg/kg were assigned to the material. The reference material has been issued as CRM BAM-U114.
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References
ISO 11262 (2011) Soil quality—Determination of total cyanide. International Organization for Standardization, Geneva, Switzerland
EN ISO/IEC 17025 (2005) General requirements for the competence of testing and calibration laboratories. CEN Management Centre & CENELEC Central Secretariat, Brussels, Belgium
ISO 11465 (1993) Soil quality—Determination of dry matter and water content on a mass basis. Gravimetric method. International Organization for Standardization, Geneva, Switzerland
ISO Guide 35 (2006) Reference materials—General and statistical principles for certification. International Organization for Standardization, Geneva, Switzerland
Bremser W, Becker R, Kipphardt H, Lehnik-Habrink P, Panne U, Töpfer A (2006) Stability testing in an integrated scheme. Accred Qual Assur 11:489–495
SoftCRM v. 1.2.2 (download: www.eie.gr/iopc/softcrm/index.html); for details see: Bonas G, Zervou M, Papaeoannou T, Lees M (2003) “SoftCRM”: a new software for the Certification of Reference Materials. Accred Qual Assur 8:101–107
ISO/IEC Guide 98–3 (2008) Uncertainty of measurement—Part 3: Guide to the expression of uncertainty in measurement (GUM:1995). International Organization for Standardization, Geneva, Switzerland
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The authors are very grateful to all participating laboratories for their efforts and valuable contributions to the presented certification project.
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Published in the topical collection Reference Materials for Chemical Analysis with guest editors Hendrik Emons and Stephen A. Wise.
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Scharf, H., Bremser, W. Certification of a reference material for determination of total cyanide in soil to support implementation of the International Standard ISO 11262:2011. Anal Bioanal Chem 407, 3219–3223 (2015). https://doi.org/10.1007/s00216-014-8149-1
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DOI: https://doi.org/10.1007/s00216-014-8149-1