Preview

Measurement Standards. Reference Materials

Advanced search
No 3 (2014)
87-91 663
Abstract
The article presents materials on the development of reference materials of asphalt concrete density (simulators). The results of calculations of certified reference material metrological characteristics with the use of certified measurement procedure, based on the method of hydrostatic weighing, are presented. The possibility of their use for evaluation of metrological characteristics of newly developed density meters of asphalt concrete PAB-1 is shown.
92-99 703
Abstract
A plant reference material (RM) was developed, which was certified in the content of fluorine-ion (% wt) in the cement raw mixture (PRM - 1 CM). Its metrological characteristics were set on the basis of results ofpotentiometric, photometric and titrimetric methods of analysis. The substantiation of the need for RM is given to increase the accuracy of results when determining fluorine in materials of cement production. The conditions are defined to use X-ray fluorescence method for estimating the material homogeneity in developing similar RMs. The interpretation of the error in residual heterogeneity in the results of analysis of powder materials and calculations of a smallest mass of representative sample is given when analyzing of such materials.
100-108 706
Abstract
The paper presents a summary of analyzing Technical Regulations of the Customs Union TR TC 029/2012 "Safety Requirements for Food Additives, Flavorings and Technological Processing Aids". Information on certified reference materials (RMs) for composition of citric acid is provided. Certified characteristics of the RM are, on the one hand, mass fraction of the base substance and, on the other hand, mass fraction of impurities - toxic elements (lead, arsenic, cadmium, mercury). The first batches of the given RMs are produced, which are registered in the State Register of the approved types of certified reference materials GS010300-2013 and GS010143-2012.

SCIENTIFIC AND METHODOLOGICAL APPROACHES, CONCEPTS

58-67 3453
Abstract
Analysis revealed, that in the area of chemical composition measurements high-purity substances may be regarded as the best measurement capabilities in the database of the International Bureau of Weights and Measures. Until now none of the countries of the world has the complete collection of high purity substances with evaluated purity level. At the present time the development of high-purity substances with evaluated values of mass fractions of the base substance is intensively going on to ensure metrological traceability to SI units using both primary methods and other instrumental methods of analysis.
68-73 679
Abstract
It is established that the carbon isotopic composition in the formation of calcium carbonate is changed depending on the magnetic field strength. The formation of calcium carbonate occurred due to the interaction of calcium hydroxide with atmospheric carbon dioxide. The profile of isotopic relations13C/12C of the newly formed calcium carbonate is approximated by the equation of the parabola for certain values of tension solenoidal magnetic field. The possibility of creating standards with a continuous series of values of the content of carbon stable isotopes based on the data suggested.

Modern methods of analysis of substances and materials

3-23 706
Abstract
Advances of elemental analysis in geology are defined by the development and improvement ofphysical, instrumental methods of chemical analysis. New instrumental methods - emission spectrometry and mass spectrometry with inductively coupled plasma (ICP) sources are the most popular in the area of elemental analysis in recent years. These methods have a very high sensitivity and wide range of elements analyzed (up to 70 items at a time). Both of these methods have been developed and demonstrate their high analytical performance only when analyzing liquids. Consequently, when using these methods in geology, solid samples must be completely transferred into liquid. This complicates the analysis, especially in the analysis of sparingly soluble objects. In some cases, analyzed geological objects are generally insoluble in acids and other solvents (e.g. such as black shales are not dissolved till the end in any acids). Naturally, there is a need to develop an analytical method, wherein the step of dissolution of the sample can be avoided. Such instrumental methods exist but are not used because of low sensitivity. Method of glow discharge mass spectrometry has the greatest potential today, but its use is hampered by lack of a recognized certified ion source capable of converting analyzed (in most cases - not conductive) geological sample into low-temperature plasma. In this paper, the glow discharge source on the basis of the hollow cathode is used as an external source. The hollow cathode has been long and successfully used in analytical practice in emission spectral analysis. However, for use in mass spectrometry, its design has been considerably modified. The analyzed sample, which was formerly in the form of powder or fine particles located at the bottom of the hollow cathode, in a new cathode is installed as a rod along the axis of the inner cathode cavity - it is the emitter of sputtered neutral particles. Hollow cathode source is set on the high resolution mass - spectrometer of ELEMENT 2 type instead of the ICP source. In sample preparation a geological sample is transformed into ultrafine state (particle size of about one micron), this thin layer of powder is applied to the emitter. Particles are held on the emitter (cathode) by van der Waals and electrostatic forces, are bombarded with argon ions, they can be also effected by electrostatic forces - between the emitter and the anode voltage of several hundred volts is applied. As a result, the charged ultra-disperse particles break away from the - emitter and diffuse into the glow discharge. Getting into the negative glow particles are heated by the electron current, then evaporate and ionize. The low-temperature plasma is formed. Mass spectral line of each element consists of many individual spikes lasting 10-30 msec. Each spike is the result of evaporation and ionization of individual particles. Mass spectral lines can be smoothed in the summation series of mass spectra. The proposed method allows direct analysis of geological samples with sensitivity ppb or less without dissolving the sample, without concentration of impurities.
24-32 660
Abstract
A method for studying the adequacy of CRM's compositions ofplants using aggregative assessment based on exploratory data analysis was proposed. It combines for each analyte such statistical estimates as adequacy of calibrations (Fischer's criterion) and quality of results of the analysis (relative bias - RB). The value of RB should not exceed ±10 % (professional criteria). This method clearly and compactly reflects the adequacy (or inadequacy) of the investigated CRM's compositions. The extent-of-equivalence of the compositions of the Chinese and Russian CRMs on data of mass spectrometry with inductively coupled plasma (MS-ICP) were confirmed by the aggregative assessments.
33-44 948
Abstract
Contents of 41 elements in the Russian standard samples of ferromanganese nodules OOPE 601, OOPE 602, OOPE 603 and ore crust OOPE 604 were identified by mass-spectrometry with inductively-coupled plasma. Content of W was firstly presented in the sample OOPE-603. Relative standard deviation for most elements was in the range of 3-10%. A description of ICP-MS technique including sample preparation procedure and other instrumental parameters were given as well as analysis of ferromanganese nodules standard samples NOD-A-1 and NOD-P-1 of U.S. Geological Survey was demonstrated for validation. Normalized to chondrite distribution curves of REE in the studied samples were shown as an indicator of the internal consistency offound concentrations. The available literature data on the content of a wide range of elements and its comparison with the matter obtained by us was produced. Measured contents of elements in the established CRM may be useful in the analytical practice to evaluate precision of results. There is a lack of relevant information on a variety of geochemically important elements in the Russian standard samples of OOPE series and the new data can be taken into account in their certification.
45-57 4690
Abstract
Abundances of 56 major and trace elements have been determined by ICP-MS for ten reference materials of different composition plants and fish tissues created at the National Institutes of China, Russia, Canada, Poland and Austria. Application of high-resolution instrument ELEMENT 2 allowed any interference to be excluded using the modes of medium and high resolution, sensitivity signal which is sufficient for measuring small and ultra abundances ofmost analytes in study samples. Real detection limits of determined elements were obtained by ICP-MS routine analysis with the autoclave preparation of samples. The obtained СИСП-МС data, complementing the elemental characteristics of RMs may be employed as the indicative values when analyzing biological materials.


ISSN 2687-0886 (Print)