| Résumé | A measurement model based on the use of a pin-cell glow discharge source coupled to a VG 9000 sector field mass spectrometer (GD-MS) for the assignment of purity of high-purity metals, i.e., mass fraction of metal matrix, w(M), is presented. A mass balance approach to the calculation requires the determination and summation of impurity mass fractions of all extraneous elements present, including non-metals and gases. It is posited that a primary method of measurement can be devised to yield direct traceability of results to the SI. The major source of uncertainty in the traceability chain stems from the need to adjust the initially estimated quantity values of each impurity element by a relative sensitivity factor 'influence quantity' , derived from ab initio calculations, and validated through comparison with those derived through use of Certified Reference Materials. It is argued that the method is sufficiently well understood that a measurement equation can be formulated for which all parameters are measured in terms of SI units; that all contributions to uncertainty of measurement can be quantitatively evaluated, underpinning the metrological traceability; and that the performance of GD-MS in CCQM key and pilot comparisons of trace elements in complex metal matrices is in conformance with claimed capabilities. The applicability of the approach to metals in the 3N to 7N range of purity shows that fit-for-purpose relative expanded uncertainties of 0.5% to 0.000 05% can be conservatively achieved for w(M). Presentation of various instrument calibration scenarios vis-à-vis impact on SI traceability of results is also undertaken with a view to eliciting further discussion of this concept within the metrological community. |
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