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Production of inorganic RM
(2016)
Beschrieben wird anhand von Beispielen die Vorgehensweise der BAM bei der Zertifizierung von Referenzmaterialien
The fully revised ISO/REMCO Guide 35 comprehensively covers most of the aspects of preparing, homogenising, and characterising reference materials.
Special attention is paid to certified RM and the expression of their traceability, as well as the evaluation of the measurement uncertainty of the assigned value(s).
Discussions in science, politics and public media about microplastic in the Environment and its unclear effects for animals and humans are common these days.
Although microplastic findings in water, soil and even air are well known, no general estimations about the quality or quantity of microplastic particles in environment exit. Research is necessary to develop reliable and traceable, harmonized protocols for sampling, sample preparation and fast, but accurate analysis for qualitative and quantitative measurement of microplastic in various environmental matrices. For development of such reliable and traceable methods, the use of microplastic reference materials is necessary to assess various concepts. These microplastic reference particles should be an appropriate reflection of the microplastic particles found in environment.
Due to the high use in industrial products six polymers seem to be relevant in environment as microplastic particles: polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET), polyamide (PA) and polyvinylchloride (PVC). The raw source of These thermoplastic materials are pellets or granulate with dimensions of 1 to 5 mm in diameter. Most common they own a regular cylindrical shape or are prolate sphericals. These can be bought cost-efficient by various polymer producers. But discussions in microplastic research topic lead to particle sizes down to 1 μm. Furthermore, various unregular shapes and geometries of the particles have to be considered as well as an oxidized surface. In the present work we engage the acquisition and production of
realistic reference material. Different aspects should demonstrate the complex and difficult task of generating approriate, cost-efficient and well-defined reference materials. The particle size distribution by using
different particle sizing methods as well as individual particle shapes are documented. Different material properties were addressed. PE, PS and PA were chosen as typical and relevant microplastic with opposite individual material characteristics in density and glass Transition temperature. The easiest possibility for acquisition of small microplastic particles is the purchase of polymer emulsion particles (20 to 150 μm).
An alternative possibility to produce small microplastic particles is milling under liquid nitrogen conditions in cryo mills. Particles purchased or self-made differ strongly in shape and size depending on production method.
SETAC
COMAR, where do you go?
(2018)
Currently BAM is making efforts to recode COMAR, the database for CRMs and reshape its profile as a database intended for qualitatively top-of-the-market CRMs. These efforts are highlighted and placed into the broad perspective of the international RM markets. A link to EPTIS, the database for PT schemes as a blueprint for the recoding is provided.
Surface analysis is still gaining importance, as most modern technology is in essence surface and thin film technology. In microelectronics and optics but also in many fields of energy storage and conversion, thin surface layers or structured surfaces are key components. Optical surface measurements are useful because of their reliability, robustness, and scalability – properties, which are especially desirable in a production environment. However, many of these methods take require considerable effort in data analysis. Spectroscopic ellipsometry (SE) is maybe the prime example of this class of methods. To combine the advantages of SE with metrological trueness and traceability, we combine it in a group of other methods, such as electron microscopy, instrumental surface analysis, X-ray diffraction.
This presentation will give an overview on the principles of SE, its available quantities and the general properties of this measurement technique. Several examples from current and past projects of BAM-6.7 will show how a measurement community involving ellipsometry can benefit many fields of interest, from polymer science to energy applications. In the context of creating a “measurement landscape”, standardisation and standard compliance play an important role. The efforts of BAM in standardisation and accrediting of ellipsometry will be shown demonstrating the possible impact on quality assurance in different fields of technology.
Reference materials are essential, when the accuracy and reliability of measurement results need to be guaranteed in order to generate confidence in the analysis.
These materials are frequently used for determining measurement uncertainty, for validation of methods, suitability testing and quality assurance. Especially direct solid sampling methods require reference materials for calibration.
They guarantee that measurement results can be compared to recognized reference values.
This presentation gives an overview about the use of GDMS in various certification procedures. Because it represents a fast, sensitive, multielement analyses technique without extensive sample preparation it plays a special role for the purity determination of high purity standards. Various calibration strategies and the preparation of traceable matrix matched calibration standards will be discussed.
For the certification of analyte content in matrix materials mainly techniques with solvent sample preparation are used. Here GD-MS is used to identify possible loss or contamination with analytes during the sample preparation step. Typically used acids to dissolve matrices lead to interferences in the ICP- mass spectrometric detection of various analytes and their quantification. Here GD-MS as direct method can also add an important contribution in the certification process.