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Measurement Standards. Reference Materials

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No 1 (2015)
23-33 1033
Abstract
The approaches for creating reference materials of glycine with certified values of nitrogen and base material mass fractions GSO 10272-2013 have been presented. Created certified reference material is intended for calibration and graduation of measurement equipments based on the different physical-chemical methods of analysis, as well as for check of error of measurement procedures. Besides GSO 10272-2013 can be used tor evaluating the purity of the components of medicinal preparations in pharmaceutical industry. GSO 10272-2013 will be used as an object for key comparisons in 2015.
39-50 829
Abstract
One of the most important stages of the developing certified reference materials (CRM) of solid natural samples is to describe a particle size distribution of prepared powders. The particle size distribution affects the degree of material homogeneity and the value representative of the analytical sample mass. The collection of CRMs was being produced at the Vinogradov Institute of Geochemistry SB RAS through a long time span; therefore the grain-size compositions of the CRM powders were measured by different instrumental methods and assessed at different scales. The laser diffraction analyzer HELOS/BR was employed to accurately and rapidly measure the grain-size composition of CRM natural sample powders. New measurements confirm that the particle size distribution of CRMs of magmatic and metamorphic rocks and sediments of Lake Baikal developed 45 and 25 years ago, accordingly have not changed fundamentally. The multimodal distributions ofparticle sizes of investigated CRMs clearly reflect the differences in mineral and chemical compositions. Aggregating of the particles of different composition and origin during long-term storage of powders is not observed. The measurement results of particle size compositions of the CRM powders show a slight dependence on the weight put into the device, as well as its mineral composition. The homogeneity of the substance of studied standard samples was confirmed by low quantities of representative sub-samples (0.075-0.100 g) for a wide range of elements determined by modern instrumental analytical methods. The use of laser diffraction analyzers type HELOS could help to certify the particle size composition of CRM powder as repeatable metrological characteristic.
34-38 641
Abstract
A state standard sample (GSO) of lactic acid content to testify and control accuracy and precision of procedures for determining lactic acid weight concentration in food was developed. It goes to the making of graduation, calibration and adjustment of measuring devices. Metrological characteristics for standard sample of lactic acid content - inhomogeneity and instability errors - were determined.

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Modern methods of analysis of substances and materials

3-15 764
Abstract
The paper describes the results of standardless quantitative XRD phase analysis (QPA) of 5 reference samples of elemental composition of sulphidic ore and technological products from Olimpiada gold deposit. The conformance between measured mineral composition and certified elemental composition is evaluated. Possibilities of the standardless QPA for determination of phase composition of the reference samples are discussed.
16-22 694
Abstract
A comparison of two methods for measurement of the free carrier recombination lifetime in the unpassivated samples of high resistivity n-type silicon single crystalls (reference samples of "GIREDMET") was made. The methods were based on the photoconductivity decay measurements (High frequence and /-PCD). Effective recombination lifetime value in the range 1-1500 /is were achieved by changes of the sample thickness from 0,4 to 10 mm. Bulk recombination lifetime was calculated using the relation between the effective recombination lifetime and the sample thickness. It was shown that random and systematic errors for two methods are of the same order.


ISSN 2687-0886 (Print)