BAM Forschungsberichte ohne Nummerierung
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- Dangerous goods (1)
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- Lead isotopic composition (1)
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Lead (Pb) isotope amount ratios are commonly used in applications ranging from archaeology and forensic sciences to terrestrial and extra-terrestrial geochemistry. Despite their utility and frequency of use, only three certified isotope amount ratio reference materials are currently available for Pb: NIST SRMs 981, 982 and 983. Because SRM 981 has a natural Pb isotopic composition, it is mainly used for correcting instrumental mass discrimination or fractionation. This means that, at present, there are no other certified isotope reference materials with natural Pb isotopic composition that could be used for validating or verifying an analytical procedure involving the measurement of Pb isotope amount ratios.
To fill this gap, two new reference materials, both certified for their Pb isotopic composition, have been produced together with a complete uncertainty assessment. These new reference materials offer SI traceability and an independent means of validating or verifying analytical procedures used to produce Pb isotope amount ratio measurements.
ERM-EB400 is a bronze material containing a nominal Pb mass fraction of 45 mg/kg. ERM-AE142 is a high purity solution of Pb with a nominal mass fraction of 100 mg/kg. Both materials have been specifically produced to assist analysts in verifying or validating their analytical procedures. Note that while one of these reference materials requires the chemical separation of Pb from its matrix (ERM-EB400), the other does not (ERM-AE142). Details on the certification of these isotope reference materials are provided in this report.
For the classification, safe handling and use of the chemicals, special standardized testing procedures have been developed and are used worldwide. Safety experts must be able to fully rely on the precise execution of the respective laboratory tests and assessments. In this context, interlaboratory tests are a crucial element of a laboratory's quality system. Participation in interlaboratory tests is explicitly recommended by the standard ISO/IEC 17025.
The present document reports the results of the interlaboratory test 2015-2016, which was performed on the test method DIN EN 15188:2007 “Determination of the spontaneous ignition behaviour of dust accumulations”. It was organized by BAM in the frame of the co-operation project CEQAT-DGHS Centre for Quality Assurance for Testing of Dangerous Goods and Hazardous Substances.
The test method DIN EN 15188:2007 is applied to characterize the self-ignition behaviour of combustible dusts. The experimental basis for describing the self-ignition behaviour of a given dust is the determination of the self-ignition temperatures (TSI) of differently-sized volumes of the dust sample by isoperibolic hot storage experiments (storage at constant oven temperatures) in commercially available ovens. The results measured this way reflect the dependence of the self-ignition temperatures on the volume of a dust accumulation.
The interlaboratory test 2015-2016 on the method DIN EN 15188:2007 is the latest in a systematic stepwise built up series of method validation interlaboratory tests and internal laboratory investigations. The aim of this interlaboratory test was to determine measurement uncertainties of the modified method DIN EN 15188 for different substances, covering a sufficiently wide range of self-ignition behaviours in the scope of the DIN EN 15188 of the four basket test to extrapolate to storage volumes up to 1000 m³ and the single basket test for a basket volume of 1000 cm³.
The precision of the four basket test and the single basket of the modified method DIN EN 15188 can be assessed as acceptable for the four sample materials investigated in the current interlaboratory test 2015-2016. It was possible to derive a functional equation for the measurement uncertainty U depending on the storage volume V. The measurement uncertainty cannot be ignored and must be considered, if TSI results should be used in practice.