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Measurement Standards. Reference Materials

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Vol 15, No 2 (2019)
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Standards

7-13 577
Abstract
Emteborg H. et al. Cooperation in publicly funded reference material production. Accred Qual Assur. 2018;23(6):371-377. DOI.org/10.1007/s00769-018-1349-1.

 

15-24 896
Abstract

The article studies the development of transfer measurement standards in the form of high-purity metals (Ag, Cd, Co, Cr, Cu, Fe, Ge, Mn, Mo, Ni, Pb, V, Zn). The evaluation of the mass fraction of the main component (MDOK) is performed by an indirect method (100 %o minus the sum of impurities). The impurity composition of the reference measurement standard materials was determined by mass spectrometry with inductively coupled plasma, reductive and oxidative melting using the State primary measurement standard of mass (molar) fraction and mass (molar) concentration of the component in liquid and solid substances and materials, based on coulometry, GET 176. The relative expanded uncertainty of MDOK (k = 2, P = 0,95) in the reference measurement standards was less, than 0,01 %o, in gravimetrically prepared solutions of the reference measurement standard it was less than 0,05 %o in most cases. The solutions of the reference measurement standards were used in the determination of certified values of metal mass fraction and mass concentration in reference materials for composition of mono-element solutions of approved types. The relative expanded uncertainty of certified values (k = 2, P = 0,95) of reference materials variedfrom 0,22 %o to 0,54 %o. Thus, it was demonstrated that metals can be used as reference measurement standards for storing a unit of the mass fraction of the main component and transferring it during characterization of reference materials for composition of solutions of the corresponding chemical elements. This work was performed within the research project «Research in the field of measurements of physicochemical composition and properties of substances, aimed at the development of State transfer measurement standards in the form of high-purity substances for reproduction and transfer of the units, characterizing chemical composition of solid substances» under the code «Purity» (2015-2017) and research and development project «Research in the field of measurements ofphysicochemical composition and properties of substances, aimed at the development of State transfer measurement standards in the form of high-purity substances for reproduction and transfer of the units, characterizing the chemical composition of solid substances and the development of reference measurement procedures» under the code «Purity-2» in the field of physicochemical measurements of composition and properties of inorganic components in solid substances (metals and salts) and food safety indicators under the code «Purity-2b» (2017-2019).

Information. News. Events

Reference materials

25-38 809
Abstract

In this article considers the models of random parameter and random walk as alternative approaches for estimating the mean standard deviation associated with heterogeneity during both the evaluation of the metrological characteristics of reference materials, the quality control of samples prepared from moist solid substances.

For the random parameter and random walk models, the behaviour of the basic statistical criteria is described, including the overall mean, standard deviation, standard deviation of the mean and function, obtained both for real experimental data and theoretical measurement results simulated according to the Monte Carlo method. It is shown that the application of the ANOVA method for evaluating the standard deviation associated with heterogeneity should be additionally validated for the materials, whose basic statistical criteria fall under the random walk model.

39-50 851
Abstract

This paper describes key stages in the development and investigation of a high-precision certified reference material (CRM) for the composition of potassium dichromate solution. The proposed reference material (RM) exhibits metrological traceability to the units of the International System of Units (SI). Not requiring additional preparation before use, the CRM is convenient for use as a titrant in redox titration.

The metrological characteristics of the developed CRM were determined by the direct primary method of coulomet-ric titration using the State Primary Standard GET 176. The interval of permissible certified values of the molar concentration of potassium dichromate in the CRM under study is found to vary from 0.098 mol/dm3 to 0.102 mol/ dm3. The relative expanded uncertainty (k = 2) of the certified value ofpotassium dichromate molar concentration is calculated to be 0.024 %, with relative standard uncertainties caused by long-term and short-term instability each being equal to 0.0044 %. The shelf life of the developed CRM is found to be 1 year, provided that storage conditions are ensured. A procedure for measuring the molar concentration ofpotassium dichromate is described, along with the equipment used. A comprehensive uncertainty budget for the measurements is assembled.

The developed CRM is included into the State Register of Certified Reference Materials under the number GSO 10992-2017. The CRM can be used for transferring the mass (molar) concentration unit of a component to RMs and chemical reagents via oxidation-reduction reactions; the verification and calibration of measuring instruments (MI), as well as control of metrological characteristics during MI trials including type approval; MI graduation; validation of measurement procedures; control of measurement results when determining the mass (molar) fraction and mass (molar) concentration of components in liquid and solid substances and materials.

Modern methods of analysis of substances and materials

51-61 879
Abstract

To certify gas mixtures in the range of low (10-3-10-8 g/m3) mercury concentrations, we have proposed and tested a traceable method for measuring the mass concentration of mercury in gaseous media by inductively coupled plasma mass spectrometry (ICP/MS). The proposed method is based on a scheme that provides for the mass spectrometer calibration for saturated vapors (physical constant) of pure metallic mercury, dosed directly into the carrier gas stream - argon. The undoubted advantage of this method is its applicability to various gases and gas mixtures, which allows you to simulate any matrix medium that affects the measurement results of mercury content when analyzed by other methods. On this basis, «Methods of measuring the mass concentration of mercury in binary gas mixtures by ICP/MS» were developed and certified. The measurement range of mercury mass concentration is from 0,03 to 1000 pg/m3, the relative expanded uncertainty of measurements U- 4 %.



ISSN 2687-0886 (Print)