Multielement trace determination in SiC powders: assessment of interlaboratory comparisons aimed at the validation and standardization of analytical procedures with direct solid sampling based on ETV ICP OES and DC arc OES
| Autor: | Jürgen Hassler, Angelika Dette, Heike Traub, Ralf Matschat |
|---|---|
| Rok vydání: | 2005 |
| Předmět: |
Calibration curve
Carbon Compounds Inorganic Analytical chemistry Sensitivity and Specificity Biochemistry Analytical Chemistry Metals Heavy Electrochemistry Calibration Nanotechnology Reproducibility Chemistry Silicon Compounds Temperature Reproducibility of Results Repeatability Metals Light Reference Standards Trace Elements Certified reference materials Spectrophotometry Inductively coupled plasma atomic emission spectroscopy Analytical procedures Volatilization Inductively coupled plasma |
| Zdroj: | Analytical and Bioanalytical Chemistry. 383:1060-1074 |
| ISSN: | 1618-2650 1618-2642 |
| Popis: | The members of the committee NMP 264 "Chemical analysis of non-oxidic raw and basic materials" of the German Standards Institute (DIN) have organized two interlaboratory comparisons for multielement determination of trace elements in silicon carbide (SiC) powders via direct solid sampling methods. One of the interlaboratory comparisons was based on the application of inductively coupled plasma optical emission spectrometry with electrothermal vaporization (ETV ICP OES), and the other on the application of optical emission spectrometry with direct current arc (DC arc OES). The interlaboratory comparisons were organized and performed in the framework of the development of two standards related to "the determination of mass fractions of metallic impurities in powders and grain sizes of ceramic raw and basic materials" by both methods. SiC powders were used as typical examples of this category of material. The aim of the interlaboratory comparisons was to determine the repeatability and reproducibility of both analytical methods to be standardized. This was an important contribution to the practical applicability of both draft standards. Eight laboratories participated in the interlaboratory comparison with ETV ICP OES and nine in the interlaboratory comparison with DC arc OES. Ten analytes were investigated by ETV ICP OES and eleven by DC arc OES. Six different SiC powders were used for the calibration. The mass fractions of their relevant trace elements were determined after wet chemical digestion. All participants followed the analytical requirements described in the draft standards. In the calculation process, three of the calibration materials were used successively as analytical samples. This was managed in the following manner: the material that had just been used as the analytical sample was excluded from the calibration, so the five other materials were used to establish the calibration plot. The results from the interlaboratory comparisons were summarized and used to determine the repeatability and the reproducibility (expressed as standard deviations) of both methods. The calculation was carried out according to the related standard. The results are specified and discussed in this paper, as are the optimized analytical conditions determined and used by the authors of this paper. For both methods, the repeatability relative standard deviations were |
| Databáze: | OpenAIRE |
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