Reference materials (E-Journal) / Стандартные образцы
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Использование висмутсодержащих стекловидных образцов для определения переходных элементов люминесцентным методом
Get PDFModern express methods of analytical control are widely used for monitoring the quality of oxide materials. However, the possibilities of these methods are currently limited by the lack of versatile homogeneous reference materials (RMs). Such RMs can be produced most effectively by vitrification methods. In this connection, glassy RMs based on bismuthborate systems are of great interest. In the earlier research, bismuth-borate RMs were used for comparison purposes in determining the composition of complex oxide systems using the X-ray fluorescence method. This work considers issues associated with the synthesis and application of bismuth-borate glassy RMs for determining the content of transition elements in oxide compounds and mixtures using luminescence analysis. Luminescence analysis was used as a research method due to its high selectivity and low detection limits with respect to elemental impurities in controlled objects (usually constituting 1 · 10–6–1 · 10–4 wt %). Bismuth-borate glassy RMs are shown to be capable of luminescence under UV radiation in the visible range at the temperature of 77 K. It is established that the introduction of the oxides of transition and rare earth elements (REE) into the RM composition leads to the quenching of the exciton emission band in the glasses studied at 77 K, as well as to the appearance of bands typical of REE ion radiation both at 77 K and at 298 K. Glassy RMs doped with transitionelement oxides are found to quench the luminescence of both bismuth and REE ions at the temperature of 77 K. On the basis of the results obtained, procedures for determining the content of quenching elements in oxide materials have been developed. The metrological characteristics of these procedures have been evaluated
Участие ФГУП «ВНИИФТРИ» в международных сличениях в области физико-химических измерений
Get PDFThis paper considers the participation of FSUE «VNIIFTRI» in international comparisons: in the field of physicalchemical measurements, particularly in pH-metry and ionometry (pX); in the sphere of measuring inorganic components in various matrices. Measurement and calibration capabilities are presented – CMC lines in the BIPM database.В статье рассмотрено участие ФГУП «ВНИИФТРИ» в международных сличениях в области физико-химических измерений (рН-метрия и ионометрия (рХ)), а также в области измерений неорганических компонентов в различных матрицах, представлены измерительные и калибровочные возможности – СМС-строки в базе данных МБМВ
Сведения о стандартных образцах утвержденных типов, срок действия свидетельств которых продлен
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О разработке референтной методики для обеспечения прослеживаемости измерений ртути в газовых средах
Get PDFTo 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 %.Для аттестации газовых смесей в диапазоне низких (.10-3-10-8 г/м3) концентраций ртути нами разработан и апробирован обеспеченный прослеживаемостью способ измерений массовой концентрации ртути в газовых средах методом масс-спектрометрии с индуктивно связанной плазмой (ИСП/МС). В основу предлагаемого способа положена схема, предусматривающая градуировку масс-спектрометра по насыщенным парам (физическая константа) чистой металлической ртути, дозируемым напрямую в поток газа-носителя - аргона для плазмы. Несомненным преимуществом данного способа является его применимость к различным газам и газовым смесям, что позволяет имитировать любую матричную среду, влияющую на результаты измерений содержания ртути при анализе другими методами. На этой основе разработана и аттестована «Методика измерений массовой концентрации ртути в бинарных газовых смесях методом ИСП/МС». Диапазон измерений массовой концентрации ртути от 0,03 до 1000 мкг/м3, относительная расширенная неопределенность измерений U- 4 %
Разработка набора стандартных образцов магнитных свойств магнитотвердых материалов на основе сплава NdFeB
Get PDFIntroduction The introduction indicates the need for the use of permanent magnets in various technology fields. The necessity of measuring the limit magnetic hysteresis loop for the correct calculation of magnetic system parameters is considered. The main sources of error when measuring boundary hysteresis loops are given. The practical impossibility of verifying blocks of magnetic measuring systems element-by-element is noted. This paper is devoted to the development of reference materials (RMs) for the magnetic properties of hard magnetic materials based on Nd2Fe14B, a highly anisotropic intermetallic compound.Materials and measuring methods Nd-Fe-B permanent magnets were selected as the material for developing the RMs. RM certified values were established using a CYCLE‑3 apparatus included in the GET 198‑2017 State Primary Measurement Standard for units of magnetic loss power, magnetic induction of constant magnetic field in a range from 0.1 to 2.5 T and magnetic flux in a range from 1·10–5 to 3·10–2 Wb.Results and its discussion Based on the experimentally obtained boundary hysteresis loops, the magnetic characteristics were evaluated, the interval of permitted certified values was set, the measurement result uncertainty of certified values was estimated, the RM validity period was established and the first RM batch was released.Conclusion On the basis of conducted studies, the RM type for magnetic properties of NdFeB alloy-based hard magnetic materials was approved (MS NdFeB set). The developed RM set was registered under the numbers GSO 11059–2018 / GSO 11062–2018 in the State RM Register of the Russian Federation
О многопараметрических стандартных образцах для метрологического обеспечения в области контроля параметров покрытий
Get PDFThe present work analyses the state and development prospects of metrological support and standardization of in the field of measuring surface density, thickness and chemical composition of coatings. The main characteristics of the State Primary Measurement Standard GET 168-2015 and developed multiparameter reference materials are described.В представленной статье проведен анализ состояния и перспектив развития метрологического обеспечения и стандартизации в области измерений поверхностной плотности, толщины и химического состава покрытий. Приведены основные характеристики государственного первичного эталона ГЭТ 168-2015 и разработанных многопараметрических стандартных образцов
Разработка стандартных образцов в области физико-химического анализа. Стандартные образцы состава водных растворов ионов алюминия, индия, магния, никеля и титана
No full textThis paper presents information on the development and certification of reference materials (CRM) for the composition of aqueous aluminium, indium, magnesium, nickel, and titanium solutions.CRMs are represented by aqueous solutions containing aluminium, indium, magnesium, nickel, and titanium ions. CRMs have been packed into 5, 10 and 25 cm3 glass ampoules, as well as into 50 and 250 cm3 polypropylene vessels. The certified values of metal mass concentrations were established according to the preparation method.The certified value of the mass concentration of metal ions in the CRMs under study is found to vary within the range of 0.95–1.06 g/dm3. Both the relative expanded uncertainty (under k= 2) of the certified mass concentration and the relative standard uncertainty due to instability do not exceed the values of 0.8 % and 0.069 %, respectively. The developed CRMs are shown to have the shelf life of 3 years provided that standard storage conditions are ensured. The developed CRMs are included into the RF State Register of Certified Reference Materials under the following numbers: CRM 11122–2018, CRM 11123–2018, CRM 11124–2018, CRM 11125–2018, and CRM 11126–2018. The CRMs produced by the All-Russian Research Institute for Optical and Physical Measurements (VNIIOFI) are characterized by the values of expanded uncertainty comparable to those of world leaders in the production of similar materials
Разработка метрологического обеспечения для количественных ЯМР-анализаторов
Get PDFThe first part of the article presents the history of creating quantitative NMR analyzers of oil content and humidity of oil crop seeds and their by-products. The developed NMR analyzers differ from similar devices in the availability of metrological support (reference materials (RMs) of approved type) and an extended range of moisture measurement (5–20)%. The main metrological characteristics of the developed NMR analyzer are given. The second part of the article deals with problems solved in the process of carrying out the scientific research work on the development of metrological support for quantitative NMR analyzers. Based on the tasks set, the most optimal substances imitating oil and water components contained in the oil crops and their by-products were selected. The imitation substances in question provide long-term stability of the developed RMs, erewhile being chemically inert to each other, environmentally safe? and allowing an imitation of oil and water in oil crops and their by-products. Organosilicon fluids with (35–40) ms and (95–130) spin-spin relaxation times of protons ms are proposed as an oil imitator. To imitate water, a one-component self-vulcanizing organosilicon compound, which is applied to paper strips with a thin coat, is used in the developed type-approved RMs. In conclusion, the article presents perspective directions of developing RMs of mass fraction imitators of typical fatty acids in the oil of oil crops (sunflower, linseed, and rapeseed)
Сотрудничество в области производства стандартных образцов, финансируемого государством
Get PDFEmteborg 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. Первоисточник статьи: Accred Qual Assur (2018) 23:371. https://doi.org/10.1007/s00769-018-1349-
Проблема тождественности характеристик стандартных образцов состава газовых смесей одного вида, выпускаемых разными предприятиями
No full textCurrently, in the Russian Federation, the metrological traceability of certified reference materials of the composition of gas mixtures in cylinders under pressure produced by manufacturers of certified reference materials is carried out in accordance with GOST 8.578-2014. Considering that certified reference materials of the composition of gas mixtures in cylinders under pressure are used for testing to approye the type of measuring instruments, verification, calibration, and graduation of gas-analytical measuring instruments used to control explosive gases and vapors, harmful components in the atmospheric air and the air of the working area, emissions from vehicles and enterprises, to control technological processes, the quality of hydrocarbon products, etc., the issue of ensuring the quality of seriously produced certified reference materials (about 100.000 cylinders with gas mixtures per year) is important. To ensure the quality of certified reference materials of gas mixtures in cylinders under pressure, mass-produced by manufacturers of certified reference materials, we offer the following actions:– manufacturers of certified reference materials’ passing of mandatory accreditation for compliance with the requirements of GOST ISO Guide 34–2014 and GOST ISO Guide 35–2015;– manufacturers of certified reference materials’ constant participation in the proficiency testing programs through interlaboratory tests;– actualizing and refining the existing set of standards defining the requirements for the entire life cycle of a certified reference material of a gas mixture in a cylinder under pressure;– improving the method of certification of a reference material by calculating the value of the expanded uncertainty of the reference material and the introducting a new coefficient «technological reserve»