Michael Czerwensky

Different calibration strategies for the analysis of pure copper metal by nanosecond laser ablation inductively coupled plasma mass spectrometry

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.

ICP-MS analysis of high purity molybdenum used as SI-traceable standard of high metrological quality

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.

Certification of high purity metals as primary reference materials: A challenge for multielement trace analysis

The Bundesanstalt fur Materialforschung und -prufung (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.

Multielement trace determination in high purity advanced ceramics and high purity metals

In the field of advanced ceramics two CRMs were developed in the last few years by the Federal Institute for Materials Research and Testing, one for silicon nitride and one for silicon carbide. Besides their application by industry they are appropriate to be used for the validation of special methods used for trace determination in accordance with high purity materials. This is demonstrated, for example, on ultrapure silicon carbide which was analysed by solid sampling electrothermal atomic absorption spectrometry (SS ET AAS).BAM is also certifying primary pure reference materials used as the National Standards for inorganic analysis in Germany. The crucial point of this project is the certification of the total purity of high purity materials, each representing one element of the periodic table. A variety of different analytical methods was necessary to determine the trace contents of metallic and non-metallic impurities from almost the whole periodic table in the high purity materials. The primary CRMs of copper, iron and molybdenum are used as examples to demonstrate the modus operandi, analytical effects observed by using high resolution ICP mass spectrometry (HR ICP-MS) and the results.

Use of microwave induced plasma spectrometry as detector for the determination of O, N and H traces after carrier gas hot extraction

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 0–27 μg, 35–1000 μg and 3–43 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.