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Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (8)
- 1.6 Anorganische Referenzmaterialien (7)
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- 4 Material und Umwelt (2)
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- 1.8 Umweltanalytik (1)
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- 4.3 Schadstofftransfer und Umwelttechnologien (1)
- 5 Werkstofftechnik (1)
Die Normung von Analyseverfahren ermöglicht, dass Parameter unter standardisierten Bedingungen qualitätsgesichert ermittelt werden können. Insbesondere dann, wenn Verfahren in gesetzliche Regelwerke einfließen, ist es notwendig, dass die Ergebnisse sicher und vergleichbar sind und der Aufwand im Vollzug vertretbar ist. Derzeit werden viele Parameter in verschiedenen Verordnungen nach unterschiedlichen genormten Verfahren analysiert, was die Überwachungsarbeit erschwert und zudem unnötig teurer macht. Aus diesem Grund wir eine sogenannte horizontale Normung angestrebt, bei der geeignete Analyseverfahren auch Matrices-übergreifend genormt und anschließend EU-weit zitiert werden können. Grundvoraussetzung für die Verabschiedung als Norm ist die Validierung der Verfahren. Bereits vor einigen Jahren erteilte die EU ein Mandat an CEN (Europäisches Komitee zur Normung), um umweltrelevante Parameter Matrices-übergreifend zu validieren. Allerdings konnten nicht alle für diverse Verordnungsnovellen (z.B. Klärschlammverordnung) wichtigen Parameter im Rahmen dieses Projekts validiert werden. Aus diesem Grund wurde das aktuelle Vorhaben in den Umweltforschungsplan des BMUB aufgenommen und von der BAM durchgeführt. Im Forschungsvorhaben konnten im Bereich der anorganischen Parameter die CEN/TS 16170 (Elemente mit ICP-OES), CEN/TS 16171 (Elemente mit ICP-MS) und CEN/TS 16175-2 (Quecksilber mit CV-AFS) sowie im Bereich der organischen Parameter die CEN/TS 16181 (PAK mit HPLC und GC), die CEN/TS 16167 (PCB mit GC-MS und GC-ECD) und die CEN/TS 16190 (Dioxine, Furane und dl-PCB mit HR-GC-MS) für die Analyse von Klärschlamm, behandeltem Bioabfall und Boden erfolgreich validiert werden. Die validierten Verfahren stehen nun kurz vor der Verabschiedung als EN (Europäische Norm).
Within the scope of a project of the 'European Association of National Metrology Institutes' (EURAMET), a European metrological dissemination System (network) providing traceable reference values assigned to matrix materials for validation purposes is described and put to the test. It enables testing laboratories (TL) to obtain comparable results for measurements under the 'EU Water Framework Directive 2000/60/EC' (WFD) and thus, to comply with a core requirement of this very directive. The dissemination system is characterized by the fact that it is available to all laboratories throughout Europe which intend to perform measurements in the context of the WFD and that it can ensure sustainable metrological traceability to the International System of Units (SI) as a reference point for the measurement results. This Dissemination system is set up in a hierarchical manner and links up the level of the national metrology institutes (NMI) with that of the TLs via an intermediate level of calibration laboratories (CL) by comparison measurements. The CLs are expert laboratories with respect to the measurement of the analytes considered here (within the project, the CLs are called potential calibration laboratories (PCL)) and are additionally involved in the organization of comparison measurements within the scope of regional quality assurance (QA) systems.
Three comparison measurements have been performed to support the approach. A total of about 130 laboratories participated in this exercise with the focus on the measurement of the priority substances Pb, Cd, Hg, and Ni defined in the WFD. The elemental concentrations in the water samples roughly corresponded to one of the established environmental quality standards (EQS), the annual average concentration (AA-EQS), which is defined in the daughter Directive 2008/105/EC of the WFD. It turned out that a significant number of TLs still need to improve their measurement methods in order to be able to fulfill the Minimum requirements of the WFD, in particular, with regard to the elements Cd and Hg probably due to their low EQS values.
Furthermore, it became obvious that the hierarchical Dissemination system suggested here actually corresponds to the measuring capabilities of the three participating Groups (NMIs, PCLs, and TLs).
With the implementation of glass casting in France in the second half of the 17th century, larger mirrors could be produced. So-called tin-mercury mirrors were made by coating glass with tin amalgam. Today, many historical mirrors are partly damaged, the image quality is compromised, and the material integrity of the mirror is threatened. The transformation from tin into an oxide starts at the surface of the amalgam and proceeds down to the glass surface. The mercury dissolves as a liquid or gaseous phase. The amalgam layer is destroyed, so that conservation is necessary. Conservators must follow strict safety precautions while handling amalgam mirrors because of possible mercury emissions and corrosion of the amalgam, during which elemental mercury accumulates near the mirror frame in droplets and is emitted into the air.
In a research project, the quantity of the mercury emissions from historical mirrors was examined and a technique to decrease these emissions was developed.
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.