Filtern
Dokumenttyp
Schlagworte
- Copper (2)
- Reference material (2)
- Aluminium alloy (1)
- CCQM-K42 (1)
- CRM (1)
- Calibration (1)
- Carrier gas hot extraction (1)
- Certification (1)
- Determination of oxygen (1)
- ECRM (1)
Organisationseinheit der BAM
The preparation and analysis of the oxygen mass fraction of three pure copper reference materials (BAM-379/1, BAM-379/2, BAM-379/3) intended for the calibration of spark emission spectrometry are described here. Data of homogeneity testing and round robin certification in collaboration with 12 independent laboratories from metalworking industry and research are reported. Problems with the establishment of traceability in this special case are discussed.
Three methods for direct solid sampling of bulk material namely IR laser ablation, glow discharge and spark OES, were compared with respect to analytical figures of merit obtained for elemental analysis with atomic spectrometry. Matrices investigated were copper, pressed doped copper powder, and magnesium alloys. For the vast majority of analytes, statistical equivalence regarding precision (usually ≤ 5%) and the performance of the calibrations between the compared methods was demonstrated.
The degree of equivalence within the participating national metrology institutes for the measurement results of the mass fractions of the analytes Cr, Cu, Fe, Mn and Zn in an aluminium alloy was assessed. This interlaboratory comité consultatif pour la quantité de matière key comparison (CCQM-K42) was organised as an activity of the Inorganic Analytical Working Group of CCQM. In total seven laboratories participated, six of them for all analytes. Measurands were the mass fractions of the analytes in a range of 0.05 and 0.2%. As an outcome the consistency of the results for all elements investigated was acceptable, hence satisfactory comparability was established. An aluminium based certified reference material—undisclosed to the analysts which one it was—was used as test sample. For the purpose of this study homogeneity was tested at BAM. Each laboratory was free to choose any analytical method they wanted to use for the analysis. Consequently various methods of measurement were employed: instrumental neutron activation analysis, X-ray fluorescence spectrometry (XRF) using fused cast-bead method combined with reconstitution technique, inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry. Metrological traceability of the measurement results to the SI unit had to be demonstrated. Therefore, methods such as spark OES or XRF (without fused cast-bead technique)—both of them being most important methods for the analysis of metals and alloys in industrial laboratories—could not be used in the frame of the key comparison.