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Paper des Monats
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The CCQM-K88 key comparison was organized by the Inorganic Analysis Working Group of CCQM to test the abilities of the national metrology institutes to measure the mass fraction of lead in lead-free solder containing silver and copper. National Metrology Institute of Japan (NMIJ), National Institute of Metrology of China (NIM) and Korea Research Institute of Standards and Science (KRISS) acted as the coordinating laboratories. The participants used different measurement methods, though most of them used inductively coupled plasma optical emission spectrometry (ICP-OES) or isotope-dilution inductively coupled plasma mass spectrometry (ID-ICP-MS). Accounting for relative expanded uncertainty, comparability of measurement results was successfully demonstrated by the participating NMIs for the measurement of the mass fraction of lead in lead-free solder at the level of 200 mg/kg.
It is expected that metals at mass fractions greater than approximately 100 mg/kg in lead-free solder containing silver and copper can be determined by each participant using the same technique(s) employed for this key comparison to achieve similar uncertainties mentioned in the present report.
BAM Federal Institute for Materials Research and Testing certified three gold-based reference materials (CRMs) suitable for X-ray fluorescence spectrometry (rose gold, white gold, yellow gold). The mass fractions of the alloying elements gold, silver and partially copper, nickel and zinc were certified. Characterization of the CRMs was performed using wet chemical methods and fire assay.
Production of inorganic RM
(2016)
Beschrieben wird anhand von Beispielen die Vorgehensweise der BAM bei der Zertifizierung von Referenzmaterialien
Die Bundesanstalt für Materialforschung und -prüfung (BAM) produziert seit vielen Jahren zertifizierte Referenzmaterialien und ist seit 2016 auch als Referenzmaterialhersteller nach ISO Guide 34 akkreditiert.
Vor jeder Zertifizierungskampagne eines zukünftigen Referenzmaterials, welches im Batch zertifiziert wird, steht ein Homogenitätstest. Dabei spielt die Richtigkeit des verwendeten Analysenverfahrens nur eine untergeordnete Rolle. Viel wichtiger ist, dass ein Verfahren mit möglichst hoher Präzision eingesetzt wird. Wichtig ist außerdem, dass die für den Homogenitätstest eingesetzte Probemenge der Mindestmenge des ZRMs bei der zukünftigen analytischen Nutzung des Materials entspricht.
Für kompaktes Material bieten sich Röntgenfluoreszenzanalyse (RFA) und Funkenemissionsspektrometrie (FOES) als Analysenverfahren an. Die RFA kann darüber hinaus auch für pulverförmige Materialien eingesetzt werden.
Im Vortrag werden verschiedene Beispiele für die Verwendung der genannten Analysenmethoden für Homogenitätsuntersuchungen aus der Praxis eines Referenzmaterialherstellers beschrieben.
The analysis of non-metals normally is carried out using elemental analysers which require reference material for calibration. In the lecture the CRM-program of BAM suitable for non-metal-analysis is presented. There are CRMs available with non-metal contents in the low ppm up to the high percent region.
CRM (Certified Reference Material) BAM-U116/CGL306 “Cyanide in soil” was produced within a framework of cooperation between CGL (Central Geological Laboratory) of Mongolia and Federal Institute for Materials Research and Testing (BAM) of Germany in 2013-2017. The CRM BAM-U116/CGL306 represents a mixture of a sandy soil collected from a contaminated former gasworks area in the Berlin region (Germany) and an unpolluted sandy soil from Nalaikh region (Mongolia).
The bulk candidate material for this reference material was prepared at CGL CRM Laboratory exclusively destined to the preparation of reference materials and equipped with modern technical equipment. Homogeneity, stability and shelf life were studied in full compliance with ISO Guide 35. The CRM was evaluated as sufficiently homogeneous. Statistical evaluation of certification analysis
was software packages SoftCRM and ProLab Plus. Certified value of total cyanide of the CRM is 12.0 mg/kg and expanded uncertainty was assigned as 0.8 mg/kg. The intended purpose of this material is the verification of analytical results obtained for the mass fraction of total cyanide in soils and soil-like materials applying the standardized procedure ISO 11262:2011. As any reference material, it can also be used for routine performance checks (quality control charts) or validation studies.
The analysis of Zinc layers on Iron sheets is one of the most essential application of Glow Discharge - Optical Emission Spectrometry (GD-OES). Since the year 2000 for this application calibration of GD-OES instruments mostly included the set of the six calibration samples CZ 2009-CZ 2014 from CKD. These CRMs are no longer available. Furthermore, in this application the analysis of Al and Mg became essential. To overcome this lack of calibration materials, the working group VDEh FA II.47 decided to organize the production and characterization of a new set of certified reference materials.