Certified Reference Material
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1 Bundesanstalt für Materialforschung und -prüfung (BAM) in cooperation with the Committee of Chemists of the GDMB Gesellschaft der Metallurgen und Bergleute e.v. Element Certified Reference Material Refined Lead Certified Values Mass fraction 1) in % Uncertainty 2) in % As Bi Sb Sn in mg/kg in mg/kg Ag Cd Cu Ni Te Tl Zn ) Unweighted mean value of the means of accepted sets of data, each set being obtained by at least 4 laboratories and/or with different methods of measurement. The values are traceable to the SI (Système International d Unités) by the use of pure substances of known stoichiometry for calibration. 2) Estimated expanded uncertainty U with a coverage factor of k = 2, corresponding to a level of confidence of approx. 95 %, as defined in the Guide to the expression of uncertainty in measurement, (GUM, ISO/IEC Guide 98-3:2008). This certificate is valid until 03/2048. Sample description The Reference Material is available in the form of discs (approx. 40 mm diameter and 40 mm height). Recommended Use The CRM is intended for establishing or checking the calibration of spark optical emission spectrometers for the analysis of samples of similar matrix composition. The minimum sample size for wet chemical analysis is 0.1 g.
2 Values for information Element Mass fraction in mg/kg Al < 2.1 In < 0.5 Instructions for Use Before use, the surface of the material must be prepared by milling or turning on a lathe. For wet chemical analysis chips have to be prepared by turning or milling of the sample surface. An area 8mm in diameter in the centre of the discs should be avoided for spark optical emission spectrometry. Transport and Storage The material should be stored in a dry and clean environment at room temperature. Transport under normal ambient conditions. Metrological Traceability The values are traceable to the SI (Système International d Unités) via calibration using pure metals or substances of known stoichiometry. All values were confirmed in an inter-laboratory comparison using spark optical emission spectrometry. Participating Laboratories Aurubis AG, Hamburg, Germany Bundesanstalt für Materialforschung und -prüfung (BAM), Berlin, Germany Berzelius Stolberg, Stolberg, Germany Hoppecke Batterien GmbH & Co. KG, Brilon-Hoppecke, Germany Johnson Controls Sachsen-Batterien GmbH & Co. KG, Zwickau, Germany Johnson Controls, VB Autobatterie GmbH & Co. KGaA, Hannover, Germany Muldenhütten Recycling und Umwelttechnik GmbH, Freiberg, Germany Recyclex Harz-Metall GmbH, Goslar, Germany TAB-IPM d.o.o., Žerjav, Slovenia ThyssenKrupp Steel Europe, Duisburg, Germany WESER METALL GmbH, Nordenham, Germany Technical Report A detailed technical report describing the analysis procedures and the treatment of the analytical data used to certify is available on request or can be downloaded from BAM website ( Page 2 of 5 pages
3 Means of Accepted Data Sets Certified values values for information Mass fraction in % mass fraction in mg/kg mass fraction in mg/kg Line No. As Bi Sb Sn Ag Cd Cu Ni Te Tl Zn Al In M s M s i The laboratory mean values have been examined statistically to eliminate outlying values. Where a --- appears in the table it indicates that an outlying value has been omitted. A data set consists of at least 4 but usually 6 single values of one laboratory. M : mean of laboratory means s M : standard deviation of laboratory means s : averaged repeatability standard deviation (square root of the mean of laboratory variances) i Page 3 of 5 pages
4 Analytical Method used for Certification Element Line Number Method As 1, 3, 4, 6, 7, 8, 9, 10, 11 ICP-OES, dissolution with tartaric acid/hno 3 2 ICP-OES, dissolution with HNO 3 /tetraborate Bi 1, 2, 3, 4, 5, 6, 8, 9, 10 ICP-OES, dissolution with tartaric acid/hno 3 7 ICP-OES, dissolution with HNO 3 /HF Sb 1, 4, 5, 6, 7, 8, 9, 10, 11 ICP-OES, dissolution with tartaric acid/hno 3 2 ICP-OES, dissolution with HNO 3 /tetraborate 3 ICP-OES, dissolution with HNO 3 /HF Sn 1, 2, 3, 4, 8, 9, 10, 11, 12 ICP-OES, dissolution with tartaric acid/hno 3 5 ICP-OES, dissolution with HNO 3 /tetraborate 6 FAAS, dissolution with HNO 3 /HF 7 ICP-OES, dissolution with HNO 3 /HF Ag 1, 3, 4, 5, 7 ICP-OES, dissolution with tartaric acid/hno 3 2, 9 FAAS, dissolution with tartaric acid/hno 3 6 ICP-OES, dissolution with HNO 3 /HF 8 ICP-OES, dissolution with HNO 3 /tetraborate Cd 1, 2, 3, 5, 6, 8, 9, 10, 11 ICP-OES, dissolution with tartaric acid/hno 3 4 ICP-OES, dissolution with HNO 3 /HF 7 ICP-OES, dissolution with HNO 3 /tetraborate 10 ETAAS, dissolution with HNO 3 /HF Cu 1, 2, 3, 4, 5, 6, 8, 9, 12 ICP-OES, dissolution with tartaric acid/hno 3 7 ETAAS, dissolution with HNO 3 /HF 10 ICP-OES, dissolution with HNO 3 /HF Ni 1, 2, 3, 4, 5, 6, 7, 8, 12 ICP-OES, dissolution with tartaric acid/hno 3 9 ETAAS, dissolution with HNO 3 /HF 10 ICP-OES, dissolution with HNO 3 /HF Te 2 ICP-OES, dissolution with HNO 3 /tetraborate 3 ICP-OES, dissolution with HNO 3 /HF 4, 5, 6, 7, 8, 9, 10, 11 ICP-OES, dissolution with tartaric acid/hno 3 12 ETAAS, dissolution with HNO 3 /HF Tl 1, 2, 3, 4, 8 ICP-OES, dissolution with tartaric acid/hno 3 6 ETAAS, dissolution with HNO 3 /HF 7 ICP-MS, dissolution with HNO 3 /tetraborate Zn 1, 2, 3, 4, 6, 8, 9, 10 ICP-OES, dissolution with tartaric acid/hno 3 7 FAAS, dissolution with HNO 3 /HF Page 4 of 5 pages
5 Element Line Number Method Al 1 ICP-OES, dissolution with HNO 3 /tetraborate 2, 3 ICP-OES, dissolution with tartaric acid/hno 3 In 1 ICP-OES, dissolution with HNO 3 /tetraborate Abbreviations: ETAAS Electrothermal atomic absorption spectrometry FAAS Flame atomic absorption spectrometry ICP-OES Inductively coupled plasma - optical emission spectrometry ICP-MS Mass spectrometry with inductively coupled plasma Accepted as BAM-CRM on Bundesanstalt für Materialforschung und -prüfung (BAM) Dr. F. Emmerling Dr. S. Recknagel Head of Department 1 Head of Division 1.6 Analytical Chemistry; Inorganic Reference Materials Reference Materials BAM holds an accreditation as a reference material producer according to ISO Guide 34 in combination with ISO/IEC This accreditation is valid only for the scope as specified in the certificate D-RM DAkkS is a signatory of the multilateral agreement (MLA) between EA, ILAC and IAF for mutual acceptance. This Reference Material is offered by: Bundesanstalt für Materialforschung und prüfung (BAM) Richard-Willstätter-Str. 11, Berlin Phone: Fax: sales.crm@bam.de Internet: Page 5 of 5 pages
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