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Eingeladener Vortrag
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Veränderungen als "kontinuierliche Verbesserungen"? - Akkreditierungsanforderungen an Laboratorien
(2015)
Zurzeit sind einige für Laboratorien wichtige internationale Normen in Überarbeitung, darunter DIN EN ISO/IEC 17025 als die wohl wichtigste. Das wird für die Laboratorien Veränderungen mit sich bringen. Aber auch unabhängig von Normenrevisionen ändern/verschärfen die Akkreditierungsstellen ihre Anforderungen, worauf die akkreditierten Laboratorien sich einstellen müssen.
Ein Qualitätsmanagement (QMS) nach DIN EN ISO/IEC 17025 [1] für ein analytisches Labor muss technische Anforderungen (s. [2]) und Managementanforderungen umsetzen. Letztere werden hier kurz vorgestellt. Als Kompetenzbestätigung durch eine unabhängige Stelle kommt heute der Akkreditierung des Labors, für die das QMS eine Voraussetzung ist, eine wesentliche Bedeutung zu.
Ein Qualitätsmanagementsystem (QMS) nach DIN EN ISO/IEC 17025 [1] einzuführen und zu betreiben, ist für analytische Laboratorien in Deutschland heutzutage praktisch ein Muss. Es ist Voraussetzung für die Akkreditierung, und es kann eine Kunden- oder Behördenforderung sein. Von den vielfältigen Fragestellungen, die ein QMS eines Laboratoriums ausmachen, werden hier die technischen Aspekte angesprochen.
TrainMiC® is a European programme for lifelong learning on how to interpret the metrological requirements in chemistry. It is operational across many parts of Europe via national teams. These teams use shareware pedagogic tools which have been harmonised at European level through the joint effort of many experts across Europe working as an editorial board. The material has been translated into 14 different languages. This report includes four TrainMiC® presentations: 1. Uncertainty of measurement — Part I Principles; 2. Uncertainty of measurement — Part II Approaches to evaluation; 3. Statistics for analytical chemistry — Part I; and 4. Statistics for analytical chemistry — Part II
Activities for the development of reference materials started as early as 1906 at the US National Bureau of Standards (NBS). In 1912, the first iron and steel reference materials were certified for carbon content in Germany by the Royal Prussian Materials Testing Institute MPA, predecessor of BAM, the Federal Institute for Materials Research and Testing.
Analytical quality assurance
(2007)
ISO Guide 35- certification
(2007)
Large-volume instrumental photon and neutron activation analysis (IPAA resp. INAA) was used for
investigation of shredded electronic waste material. Sample masses from 1 to 150 grams were analysed
to obtain an estimate of the minimum sample size to be taken to achieve a representativeness
of the results which is satisfactory for a defined investigation task. Furthermore, the influence of
irradiation and measurement parameters upon the quality of the analytical results were studied. Finally,
the analytical data obtained from IPAA and instrumental neutron activation analysis (INAA),
both carried out in a large-volume mode, were compared. Values within the limits of satisfactory
agreement were found only partially. Analytical process control using on-site X-ray fluorescence
analysis performed during recycling of electronic waste is currently under development.
Along with the globally increasing energy demand the application of renewable energy sources is
urgently required. According to national regulations and international treaties (e.g. Kyoto Protocol)
these sources shall be sustainably available at reasonable financial effort and non-polluting during
production, use and waste treatment. Using photovoltaic sources (PV), these requirements can
clearly be met. All industry has to follow the best available technology and an integrative life cycle
approach for their products and production. PV thin film technology strictly responds to this obligation.
In order to save material resources and to minimise undesirable landfill recycling of spent PV
modules is necessary. Recycling of multi-component materials containing mixed metals typically
consists of three parts: liberation, separation, and recovery. In our study (RESOLVED an EU
Demonstration Project) the focus is on liberation and separation. The converting layer (CdTe) was
liberated (removed) from the glass carrier by sandblasting and separated subsequently from the
blast material (e.g. corundum) and other components using stepwise different separation techniques.
Both the glass substrate and CdTe are subject to re-use. The overall feasibility of the recycling
process is primarily governed by the efficiency of the procedure applied to the separation of CdTe
from the rest (blasting material, glass residues, etc.). This was performed by water-based flotation.
Several flotation procedures were studied regarding their separation yields. The distribution of
CdTe in the phases involved (flotate, water, residue) was measured using energy dispersive X-ray
fluorescence spectrometry (EDXRS) intended for future routine application and by instrumental
large-volume photon activation analysis (IPAA) as a reference procedure. The results of both analytical
methods were in satisfactory agreement.
This study was undertaken to investigate the long-term performance of hydroxyapatite (HAP) as reactive material for the removal of uranium in passive groundwater remediation systems. 237U used as a radioindicator enabled tracking the movement of the contamination front through a test column without taking samples or dismantling the apparatus. The stoichiometric ratio between uranium and HAP was found to be 1:(487±19). Uranium removal by HAP is of pseudo first-order kinetics and the rate constant was measured to be (1.1±0.1)×10-3 s-1. HAP can sorb more than 2900 mg/kg uranium. Possible reaction pathways of uranium and HAP are discussed. The data obtained enable the calculation of ideal lifetime for permeable reactive barriers (PRB) using HAP for uranium removal neglecting hydrological factors that may impair the function of PRBs.
Die BAM und ihre Referenzmaterialien - Stellenwert der nuklear- und gas- analytischen Verfahren
(2002)
This study was undertaken to investigate the long-term performance of elemental iron as reactive material for the removal of uranium in passive groundwater remediation systems. By using 237U as a radioindicator it was possible to track the movement of the contamination front through a test column without taking samples or dismantling the apparatus. The stoichiometric ratio between uranium and iron was found to be 1:(1390±62). The reaction between iron and uranium is of pseudo first-order kinetics and the rate constant was measured to be (1.1±0.09)×10-3 s-1. These data enable the calculation of ideal lifetime for permeable reactive barriers (PRB) using iron for uranium removal neglecting hydrological factors that may impair the function of PRBs.
The special importance of the analysis of non-metals in high purity metals, which will serve as national standards for elemental analysis in Germany, is illustrated for oxygen and nitrogen. The typical range of the mass fraction of oxygen and nitrogen in these materials is below 10.MU.g/g, often close to 1.MU.g/g. The two methods applied at BAM for these measurements are classical carrier gas hot extraction (HE) and carrier gas hot extraction after activation with photons (PAA-HE). The approach, the methods and their advantages and limitations are discussed. Comparative results from the measurement of oxygen and nitrogen in Cu, Fe, Ga, Pb, Sn and W are presented. (author abst.)
Zusammenfassung
The working principle of nuclear analytical methods (NAMs) is not influenced by the chemical bond. Consequently, they are independent counterparts to the well-known chemical procedures. NAMs obey fundamental laws or can be described and understood thoroughly. This qualifies them as candidates for reference methods. Although following similar nuclear reaction schemes, they comprise bulk analyzing capability (neutron and photon activation analysis) as well as detection power in surface near regions of solids (ion beam techniques). Prominent features of NAMs are sensitivity, selectivity, multielement determination and linearity of the calibration function covering a concentration range of several orders of magnitude. Moreover, ion beam techniques allow depth profiling with nm-resolution in several cases while the ion microprobe additionally offers a lateral resolution in the wm-scale. As NAMs require expensive apparatus (nuclear reactor, accelerator in radioactive control areas) their availability is restricted to a small number of suitably equipped institutes. However, they are able to solve complex analytical tasks, take part in key comparisons and play an essential role in the certification of reference materials.