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The Bundesanstalt fuer Materialforschung und -pruefung, BAM (Federal Institute for Materials Research and Testing) continues to establish a system of primary reference materials to meet the demands of metrological traceability. The materials act as national standards in the field of elemental analysis. For all elements of the periodic table -excepting those that are gases or radioactive- two different kinds of reference materials are being certified. The substances are of very high purity and of defined stoichiometry. Pure elements and metals are used as far as possible. They are certified by determining the trace contents of most elements of the periodic table at very low levels using different trace element analysis methods. Recent application of these methods is described and examples of the certification of some pure metals (copper, iron and lead) are given. (author abst.)
ICP-MS analysis of high purity molybdenum used as SI-traceable standard of high metrological quality
(2005)
The need, concept and technical approach for the certification of SI-traceable standards of high metrological quality for chemical analysis of the elements is briefly explained. As an example of problems occurring in the certification of these standards, special technical aspects related to the analysis of high purity Mo by ICP-MS, namely blank reduction for Na, Li and Ni by protective coating of the cones with silicon, as well as dealing with the interferences from the Mo matrix, are discussed.
The Bundesanstalt für Materialforschung und -prüfung (Federal Institute for Materials Research and Testing) (BAM) is establishing a system of primary reference materials to meet the demands for metrological traceability and to act as national standards in the field of elemental analysis. For all elements of the periodic table - except those that are gases or radioactive - two different kinds of reference materials are being certified. One is for analyte calibration (Type A) and one for problems concerning matrix matching (Type B). These substances are of very high purity and of defined stoichiometry. As far as possible, pure elements and metals rather than pure compounds are used. The certification of both types of material requires most elements of the periodic table to be certified at very low levels using trace element analysis methods. The application of these methods is described and examples of the certification of copper and iron are given.
Low-temperature electron-paramagnetic-resonance study of extrinsic and intrinsic defects in CuGaSe2
(1999)
The determination of O, N and H using a microwave induced plasma coupled to carrier gas hot extraction was exploratory investigated. The signal intensities versus time of blanks and calibration materials were recorded. To check for interferences the signal intensities versus wavelength were recorded at the times just before increase and at the maximum of the time dependent analytical signal. O, N and H were investigated at their prominent wavelengths of 777 nm, 174 nm and 486 nm, respectively. Calibration was performed for O, N and H in the ranges of 027 µg, 351000 µg and 343 µg respectively. For concentration values in the middle of the linear part of the investigated calibration interval, a relative precision of 5% at 13 µg, 2% at 74 µg and 0.6% at 23 µg for O, N and H respectively was found. The maximum matrix load to the plasma used was found to be 150 µg min-1. From the signal to noise ratio and the sensitivity obtained, instrumental limits of detection (3s) of 0.01 µg for O, 1 µg for N and 0.1 µg for H were found. Assuming a typical sample mass of 1 g this corresponds to relative LODs of 0.01 µg g-1, 1 µg g-1 and 0.1 µg g-1 for O, N and H respectively.
Within the National Metrology Institutes (NMIs) and designated laboratories, an interlaboratory comparison, CCQM-P107, was conducted to verify the degree of international comparability concerning the results of purity analysis. The mass fractions of Ag, Bi, Cd, Cr, Ni, Tl at the lower mg/kg-level in a high purity zinc material were determined, but the real measurand in metrological sense was the sum of the six mass fractions. Homogeneity was investigated by glow discharge mass spectrometry, reference values were obtained using isotope dilution mass spectrometry. Six NMIs participated, contributing eight independent data sets. The agreement amongst the results of the participants, their median and the agreement with the reference values were usually excellent and in almost all cases below the target uncertainty of 30% relative. In this manner, the accuracy of results and the comparability between the participants was demonstrated to be established.
In this work, different calibration strategies for the determination of trace elements in pure copper metal by nanosecond laser ablation ICP-MS were investigated. In addition to certified reference materials (CRMs), pellets of doped copper powder were used for calibration. The micro homogeneity of the CRMs as well as the solution-doped pellets was sufficient to use them as calibration samples in combination with a laser spot size of 200 µm. In contrast, pellets doped with analytes in solid form showed a significant heterogeneity. For most of the investigated analytes and copper CRMs the measured mass fractions were within ± 20% of their certified values when other copper CRMs were used as calibration samples. When solution-doped powder pellets were used as calibration samples a systematic trend towards mass fractions below the certified values was observed for nearly all elements determined in the analysed CRMs. Thermal fractionation effects during the ablation of the solution-doped pellets were suspected as the extent of the fractionation depends on the irradiance, whereas fractionation is reduced at higher irradiance.