TY - CONF A1 - Phukphatthanachai, Pranee A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - How to quantify the exact amount and establish metrological traceability of sulphur in biodiesel by ICP-IDMS and in copper samples by ICP-IDMS, GDMS, LA-ICP-MS, and LA-ICP-IDMS N2 - The quantification of the exact amount of sulphur is a big challenge due to a lack of SI-traceability and inconsistent results, when different methods are compared. Therefore, a reference procedure is required which allows SI-traceable values. In this work three procedures were developed for the quantification of the total sulphur amount in biodiesel by using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS), pure copper metals and copper alloys by ICP-IDMS and external calibration for GDMS and LA-ICP-MS at low concentration levels. The most critical parts of the sulphur quantification were sulphur purification and pre-concentration. Sulphur-matrix separation procedures were developed to serve both sample types. For biodiesel samples the sulphur was purified and matrix separated by an anion exchange chromatographic procedure. The analytical procedure was fully validated by the use of a certified reference material, a step-by-step validation and an inter-laboratory comparison at CCQM key comparison level. In the case of copper samples, the copper matrix was separated from sulphur by adding ammonia which forms a complex with the copper while releasing the sulphur prior to a chromatographic separation using a weak cation resin. After that the sulphur fraction was further purified by chromatographic means using first an anion ion exchange method and second a chelating resin. The method was validated by appropriate certified reference materials. The developed procedures enable sulphur measurements at the low g·g-1 level with sufficiently low measurement uncertainties (< 2 %, Urel). The external calibration was performed to produce reliable measurement results for the routine analytical techniques GDMS and LA-ICP-MS. Matrix-matched reference materials whith exactly known amount of sulphur obtained by ICP-IDMS beforehand, were used as calibrators to quantify sulphur in copper samples. The metrological traceability to the SI for the mass fraction of sulphur is established for all presented procedures by an unbroken chain of comparisons, each accompanied by an uncertainty budget. T2 - CCQM Workshop on Advances in Metrology in Chemistry and Biology CY - Sèvres, France DA - 09.04.2019 KW - Copper KW - Sulfur KW - IDMS KW - SI traceability PY - 2019 AN - OPUS4-47931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -