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Measurement Standards. Reference Materials

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Vol 13, No 1 (2017)
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Reference materials

9-26 3758
Abstract
The article is devoted to the development of the state secondary measurement standard of mass fraction units and mass (molar) concentration of organic components in liquid and solid substances and materials based on gas and liquid chromatography. The composition of the state secondary measurement standard, as well as the results of evaluating metrological characteristics have been considered. The problem of ensuring the traceability of measurement results to SI units is given in the article. Two approaches are proposed for obtaining a unit from the state primary standard of mass (molar) fraction units and mass (molar) concentration of organic components in liquid and solid substances and materials based on liquid and gas chromatography-mass spectrometry with isotopic dilution and gravimetry GET 208-2014: by comparing and using transfer standards. Examples of implementing the indicated approaches used during the development of reference materials of toxic substances, namely a certified reference material for composition of p,p-DDT (p,p-DDT, CRM of UNIIM) and a certified reference material for composition of benz(a)pyrene solution in acetonitrile (C20H12, CRM of UNIIM) are given. Results of determining metrological characteristics of reference materials including standard uncertainty due to characterization and standard uncertainties due to inhomogeneity, short and long-term instabilities are described.
37-42 1061
Abstract
INTRODUCTION. Liquid penetrant testing (PT) is one of the most widely used non-destructive testing methods for detecting surface discontinuities in nonporous solid materials. This method has shown good results when looking for defects in details made of any nonporous materials including glass, ceramics, plastic, magnetic or nonmagnetic metals or alloys. Penetrant materials and check samples are the main tools for PT. The samples are used to estimate the performance of penetrant materials and to evaluate the sensitivity of the testing technology. AIM OF THE PAPER. The paper aims to evaluate the discontinuity parameters, such as cracks, in non-metal samples to determine the feasibility of using these samples to assess the sensitivity of the testing technology. METHODS. Discontinuity parameters in non-metallic check samples were determined using a microscope, and then the data was statistically processed in accordance with GOST 8.736-2011"Multiple direct measurements. Methods of measurement results processing. Main principles". RESULTS. The conducted study has showed that samples made of non-metallic material can be used to estimate the performance of penetrant families, as well as to assess penetrant testing sensitivity since the cracks in samples are virtually straight.
27-36 1817
Abstract
Introduction. The results of development of a certified reference material (CRM) of mineral composition of natural water are presented. A solution prepared from the material of the CRM specimen imitates mineral composition of natural surface water. The certified values are mass fractions of nitrate ions, chloride ions, fluoride ions, and total iron and turbidity according to formazine scale. Materials and methods. The certified values of mass concentrations of the components were determined using calculated experimental evaluation procedure;the certified turbidity value was determinedusing the certified turbidimetric method. Results. The relative expanded uncertainty (k = 2) of the certified turbidity values does not exceed 5 %, the same value for mass concentrationsis not more than 3.5 %. Relative standard uncertainty from heterogeneity does not exceed 1.0 %. The shelf life of the developed CRM is set to 3 years. Discussion and conclusion. Developed CRM was registered in the State Register of CRM's as GSO 10815-2016. The CRM is designed to control the accuracy of results of the certified characteristics measurements, including proficiency testing of laboratories using interlaboratory comparative tests. The CRM can be used for validation of measurement procedures.

Modern methods of analysis of substances and materials

43-55 1062
Abstract
Introduction. Research in a field of new sorption materials obtaining have been presented in this article. These sorbents have magnetic properties and they can be used for water purification from ions of heavy metals (HM), petroleum and petroleum products (PP). Compositional sorption material (CSM) has been made with the use of ferritized galvanic sludge (FGS) as a magnetic component and paraffin as a binder substance. Materials and methods. The following objects of the research were chosen in this work: industrial waste - galvanic sludge (GS), FGS, paraffin. Modern methods of the research have been used at work implementation: photometry, IR-spectrophotometry, scanning electron microscopy. Obtaining accurate and reliable results of the experiment were provided by the use of standard methods, established in federal environmental regulatory document (PND F), verifiable measuring instruments and standard samples. Results. FGS after a thermal processing has sorption properties in relation to ions of heavy metals Fe2+, Fe3+ and Cu2+. The material CSM can adsorb petroleum and PP. Discussion and conclusions. The sorption materials on the basis of industrial waste - GS were obtained and studied. These sorbents have magnetic properties which will be useful at water treatment; a saturated material can be extracted from a purified environment by magnetic separation.

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ISSN 2687-0886 (Print)