Filtern
Erscheinungsjahr
- 2014 (5) (entfernen)
Dokumenttyp
- Zeitschriftenartikel (5) (entfernen)
Schlagworte
- Alkaline-manganese (1)
- Analysis (1)
- Batteries Act (1)
- Battery (1)
- Button cell (1)
- Cadmium (1)
- EU Batteries Directive (1)
- Edelmetalle (1)
- Heavy metal (1)
- Lead (1)
The objective of this work was to provide updated information on the development of the potential impact of heavy metal containing batteries on municipal waste and battery recycling processes following transposition of the new EU Batteries Directive 2006/66/EC. A representative sample of 146 different types of commercially available dry and button cells as well as lithium-ion accumulators for mobile phones were analysed for their mercury (Hg)-, cadmium (Cd)- and lead (Pb)-contents. The methods used for preparing the cells and analysing the heavy metals Hg, Cd, and Pb were either developed during a former study or newly developed. Several batteries contained higher mass fractions of mercury or cadmium than the EU limits. Only half of the batteries with mercury and/or lead fractions above the marking thresholds were labelled. Alkaline–manganese mono-cells and Li-ion accumulators, on average, contained the lowest heavy metal concentrations, while zinc–carbon batteries, on average, contained the highest levels.
KEY COMPARISON
Under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a key comparison, CCQM K55.c, was coordinated by the Bureau International des Poids et Mesures (BIPM) in 2012. Twenty National Measurement Institutes or Designated Institutes and the BIPM participated. Participants were required to assign the mass fraction of valine present as the main component in the comparison sample for CCQM-K55.c. The comparison samples were prepared from analytical grade L-valine purchased from a commercial supplier and used as provided without further treatment or purification.
Valine was selected to be representative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of low structural complexity [molecular weight range 100300] and high polarity (pKOW > –2).
The KCRV for the valine content of the material was 992.0 mg/g with a combined standard uncertainty of 0.3 mg/g. The key comparison reference value (KCRV) was assigned by combination of KCRVs assigned from participant results for each orthogonal impurity class. The relative expanded uncertainties reported by laboratories having results consistent with the KCRV ranged from 1 mg/g to 6 mg/g when using mass balance based approaches alone, 2 mg/g to 7 mg/g using quantitative 1H NMR (qNMR) based approaches and from 1 mg/g to 2.5 mg/g when a result obtained by a mass balance method was combined with a separate qNMR result.
The material provided several analytical challenges. In addition to the need to identify and quantify various related amino acid impurities including leucine, isoleucine, alanine and a-amino butyrate, care was required to select appropriate conditions for performing Karl Fischer titration assay for water content to avoid bias due to in situ formation of water by self-condensation under the assay conditions. It also proved to be a challenging compound for purity assignment by qNMR techniques.
There was overall excellent agreement between participants in the identification and the quantification of the total and individual related structure impurities, water content, residual solvent and total non-volatile content of the sample. Appropriate technical justifications were developed to rationalise observed discrepancies in the limited cases where methodology differences led to inconsistent results.
The comparison demonstrated that to perform a qNMR purity assignment the selection of appropriate parameters and an understanding of their potential influence on the assigned value is critical for reliable implementation of the method, particularly when one or more of the peaks to be quantified consist of complex multiplet signals.
Quecksilber-, Cadmium- und Bleigehalte in Gerätebatterien im Lichte der rechtlichen Entwicklungen
(2014)
Für die Schwermetalle Quecksilber, Cadmium und Blei gibt es aufgrund ihrer Gefährlichkeit gesetzliche Vorgaben für ihre Gehalte beziehungsweise ihre Kennzeichnung in Gerätebatterien. Die Bundesanstalt für Materialforschung und -prüfung hatte im Jahr 2006 rund 140 Gerätebatterien auf ihre Gehalte an diesen drei Metallen analysiert. Nachdem mit dem Batteriegesetz im Jahr 2009 die Grenz- beziehungsweise Schwellenwerte verschärft worden waren, wurde im Jahr 2011 erneut eine Stichprobe von 146 Gerätebatterien - Knopfzellen, Rundzellen, Akkus für Mobiltelefone und 9V-Zink-Kohle-Blöcke verschiedener chemischer Systeme und Hersteller - analysiert.
Für die Analysen wurden die Knopfzellen vollständig in Säure aufgelöst, die anderen Batterietypen wurden zunächst mechanisch in ihre Fraktionen zerlegt. Zur Bestimmung der Elemente kamen ICP-MS, Kaltdampf-AAS, ICP-OES und ein automatischer Quecksilberanalysator zur Anwendung.
Ergebnisse: Die Schwermetallniveaus änderten sich zwischen 2006 und 2011 insgesamt wenig. Die untersuchten AlMn-Rundzellen und Li-Ion-Akkumulatoren für Mobiltelefone enthielten 2011 die durchschnittlich geringsten Schwermetallgehalte, während die Zink-Kohle-Rundzellen durchschnittlich am stärksten belastet waren, maximal mit 41,4 mg/kg Quecksilber, 170 mg/kg Cadmium beziehungsweise 1958 mg/kg Blei. Außerdem fehlte auf der Hälfte der Batterien die erforderliche Element-Kennzeichnung mit 'Hg' beziehungsweise 'Pb'.
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.