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The traceabiiity requirements for certification analyses of reference materials are much more stringent than for routine analysis, where certified matrix reference materials (CRM) can be used for calibration and to establish traceabiiity. Although the ISO-Guides related to CRM production and certification are not fully clear concerning calibration, many established CRM-producers do not accept matrix-CRMs for calibration in case of certification analyses, e.g. to avoid circular reasoning. These requirements limit the methods used for certification to those that can be calibrated using Standards of known high purity and stoichiometry or mixtures of such Standards. Powerful solid sampling techniques such as glow discharge mass spectrometry (GD-MS) or spark-optical emission spectrometry (SOES), where usually compact CRMs are used for calibration, seem not be applicable for certification analyses. Especially GD-MS is a powerful tool for trace element determination of solid samples. Beside metallic impurities the use of specific gas mixtures enables also the determination of interesting nonmetallic impurities such as sulfur and phosphorus. Within BAM a calibration approach, was developed which enables to use mixtures of Standards of known high purity and stoichiometry also for GD-MS. Analogue to matrix adaption in solution based techniques, the calibration approach is based on doped pressed powder pellets.
Approach and application on the certification analyses of copper and Steel CRMs are presented.
The EU RoHS Directive (2002/95/EC of the European Parliament and of the Council) bans the placing of new electrical and electronic equipment containing more than agreed levels of lead, cadmium, mercury, hexavalent chromium, polybrominated biphenyl (PBB) and polybrominated diphenyl ether (PBDE) flame retardants on the EU market. It necessitates methods for the evaluation of RoHS compliance of assembled electronic equipment. In this study mounted printed circuit boards from personal computers were analyzed on their content of the three elements Cd, Pb and Hg which were limited by the EU RoHS directive. Main focus of the investigations was the influence of sample pre-treatment on the precision and reproducibility of the results. The sample preparation steps used were based on the guidelines given in EN 62321. Five different types of dissolution procedures were tested on different subsequent steps of sample treatment like cutting and milling. Elemental analysis was carried out using ICP–OES, XRF and CV–AFS (Hg). The results obtained showed that for decision-making with respect to RoHS compliance a size reduction of the material to be analyzed to particles ≤1.5 mm can already be sufficient. However, to ensure analytical results with relative standard deviations of less than 20%, as recommended by the EN 62321, a much larger effort for sample processing towards smaller particle sizes might be required which strongly depends on the mass fraction of the element under investigation.
The preparation, analysis and certification of a new certified glass reference material (CRM) for multi-element determination in soda–lime–silica glass is described. The CRM BAM-S006 is available in the form of discs (thickness: 5 mm, diameter: 40 mm) as well as in form of cullet. Certified properties are the mass fractions of 19 main, minor and trace elements. The certified values are based on the results of 18 laboratories which participated in the certification inter-laboratory comparison. The CRM is intended for establishing or checking the calibration of x-ray spectrometers for the analysis of samples of similar matrix composition as well as for wet chemical analysis.
This work presents the development and certification of the world’s first certified reference material (CRM), BAM-S014, for a lithium nickel manganese cobalt oxide (LiNi0.33Mn0.33Co0.33O2 or Li-NMC 111) cathode material—an integral component in high-energy-density lithium-ion batteries that power electric vehicles (EVs), portable electronics, and stationary energy storage systems. By providing certified mass fractions for 11 elements, this CRM addresses a critical need for accurate and traceable elemental analysis, supporting quality control and regulatory compliance in the global battery industry. Ensuring reliable and harmonized measurements supports the efficient use of resources, including the reuse of recycled materials, and ultimately helps maintain product performance and safety. The values were assigned through an interlaboratory comparison involving 16 participating laboratories and various analytical techniques such as inductively coupled plasma optical emission spectrometry (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), X-ray fluorescence (XRF) spectrometry, and combustion analysis. In addition to chemical characterization, the certification process includes homogeneity and stability testing of the candidate material. Details are provided on the analytical methods used for chemical characterization and the calculation of the uncertainties of the certified mass fractions. In addition to detailing the development of the CRMs, this work provides an overview of ongoing standardization activities in Li-component analysis, thereby guiding the calibration of analytical methods and contributing to the establishment of globally accepted standards for evaluating energy storage materials and advancing sustainable mobility and clean energy solutions.
High-and medium entropy alloys have been investigated for more than two decades and their potential keeps being evaluated. Their “baseless” character distinguishes them from classic alloys that are characterized by one main element, such as steel – Fe based. The question has arisen whether our analysis methods are suited for alloys without a base element and is has been found that they are within the limitations of the methods. This dataset shows the compatibility between inductively coupled plasma optical emission spectrometry, combustion analysis, x-ray fluorescence analysis and energy dispersive x-ray spectroscope, measured in the scanning electron microscope. Four alloys from the well-studied Co-Cr-Fe-Ni medium entropy family have been used as testing materials.
