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<article article-type="research-article" dtd-version="1.3" xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns:xsi="http://www.w3.org/2001/XMLSchema-instance" xml:lang="ru"><front><journal-meta><journal-id journal-id-type="publisher-id">rmjournal</journal-id><journal-title-group><journal-title xml:lang="ru">Эталоны. Стандартные  образцы</journal-title><trans-title-group xml:lang="en"><trans-title>Measurement Standards. Reference Materials</trans-title></trans-title-group></journal-title-group><issn pub-type="ppub">2687-0886</issn><publisher><publisher-name>D. I. Mendeleyev Institute for Metrology</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="doi">10.20915/2077-1177-2018-14-1-2-9-23</article-id><article-id custom-type="elpub" pub-id-type="custom">rmjournal-171</article-id><article-categories><subj-group subj-group-type="heading"><subject>Research Article</subject></subj-group><subj-group subj-group-type="section-heading" xml:lang="ru"><subject>Эталоны</subject></subj-group><subj-group subj-group-type="section-heading" xml:lang="en"><subject>Standards</subject></subj-group></article-categories><title-group><article-title>Совершенствование эталонного комплекса для метрологического обеспечения порометрии твердых веществ и материалов</article-title><trans-title-group xml:lang="en"><trans-title>Improving the measurement standard for the metrological support of the porometry of solid substances and materials</trans-title></trans-title-group></title-group><contrib-group><contrib contrib-type="author" corresp="yes"><name-alternatives><name name-style="eastern" xml:lang="ru"><surname>Собина</surname><given-names>Е. П.</given-names></name><name name-style="western" xml:lang="en"><surname>Sobina</surname><given-names>E. P.</given-names></name></name-alternatives><bio xml:lang="ru"><p>Собина Егор Павлович – канд. хим. наук, заместитель директора по инновациям, заведующий лабораторией метрологического обеспечения и наноиндустрии, член-корреспондент Метрологической академии </p><p>620075, г. Екатеринбург, ул. Красноармейская, 4</p></bio><bio xml:lang="en"><p>Egor P. Sobina – Ph.D (Chem.), Deputy Director for Innovation, Head of laboratory of metrological assurance and nanoindustry UNIIM, corresponding member of the Russian Academy of Metrology </p><p>4 Krasnoarmeyskaya St., Ekaterinburg, 620075</p></bio><email xlink:type="simple">251@uniim.ru</email><xref ref-type="aff" rid="aff-1"/></contrib></contrib-group><aff-alternatives id="aff-1"><aff xml:lang="ru">ФГУП «Уральский научно-исследовательский институт метрологии»<country>Россия</country></aff><aff xml:lang="en">Ural Research Institute for Metrology (UNIIM)<country>Russian Federation</country></aff></aff-alternatives><pub-date pub-type="collection"><year>2018</year></pub-date><pub-date pub-type="epub"><day>11</day><month>02</month><year>2019</year></pub-date><volume>14</volume><issue>1-2</issue><fpage>9</fpage><lpage>23</lpage><permissions><copyright-statement>Copyright &amp;#x00A9; Собина Е.П., 2019</copyright-statement><copyright-year>2019</copyright-year><copyright-holder xml:lang="ru">Собина Е.П.</copyright-holder><copyright-holder xml:lang="en">Sobina E.P.</copyright-holder><license license-type="creative-commons-attribution" xlink:href="https://creativecommons.org/licenses/by/4.0/" xlink:type="simple"><license-p>This work is licensed under a Creative Commons Attribution 4.0 License.</license-p></license></permissions><self-uri xlink:href="https://www.rmjournal.ru/jour/article/view/171">https://www.rmjournal.ru/jour/article/view/171</self-uri><abstract><p>В настоящее время в Уральском научно-исследовательском институте метрологии функционирует Государственный первичный эталон единиц удельной адсорбции газов, удельной поверхности, удельного объема и размера пор твердых веществ и материалов (ГЭТ 210 –2014), который имеет измерительные и калибровочные возможности размера пор в диапазоне от 2 до100 нм, при этом на практике возникает необходимость контроля размера пор твердых веществ и материалов в диапазоне от 100 до10 000 нм. Для расширения измерительных и калибровочных возможностей ГЭТ 210-2014 было предложено включение в состав эталона двух установок, реализующих методы ртутной порометрии и стационарной фильтрации, что позволит значительно расширить возможности нового эталона. В настоящей работе рассмотрено состояние метрологии порометрии и представлены первые результаты исследований метрологических характеристик эталонных установок, реализующих методы ртутной порометрии и стационарной фильтрации. Разработаны и опробованы алгоритмы расчета неопределенности воспроизводимых на эталонных установках величин, характеризующих пористость твердых веществ. Адекватность разработанных алгоритмов подтверждена результатами участия в 4 международных сличениях, измерений стандартных образцов зарубежного производства, а также итогами участия в6 раундах межлабораторных сличительных испытаниях. Совершенствование эталона позволит обеспечить метрологическое обеспечение СИ и методик измерений сорбционных свойств, пористости, газопроницаемости твердых веществ и материалов в различных отраслях промышленности. При этом обеспечивается метрологическая независимость Российской Федерации и осуществляется импортозамещение дорогостоящих зарубежных стандартных образцов.</p></abstract><trans-abstract xml:lang="en"><p>The State Primary Measurement Standard for units of specific gas adsorption, specific surface area, specific volume and pore size of solid substances and materials (GET 210–2014) is currently in operation at UNIIM. The GET 210-2014 has calibration and measurement capabilities for pore size in a range from 2 to 100 nm, while in practice there is a need to control the pore size of solid substances and materials in a range from 100 to 10,000 nm. In order to enhance the calibration and measurement capabilities of the GET 210-2014, it was proposed to include two reference systems implementing the methods of mercury porometry and stationary filtration into the measurement standard. This work considers the state of the metrology of porometry and presents the first results of studies on the metrological characteristics of reference systems implementing the methods of mercury porometry and stationary filtration. Algorithms for calculating the uncertainty of quantities being reproduced via the methods of mercury porometry and stationary filtration and characterizing the porosity of solids have been developed and tested. The reliability of the developed algorithms is confirmed by: the results of participation in 4 international comparisons, the measurements of foreign-made reference materials, along with the results of participation in 6 rounds of interlaboratory comparisons. The measurement standard improvement will provide metrological support to measuring instruments and measurement procedures for sorption properties, porosity and gas permeability of solid substances and materials in various industrial sectors. Thus, the metrological independence of the Russian Federation will be ensured and import substitution of expensive foreign reference materials carried out.</p></trans-abstract><kwd-group xml:lang="ru"><kwd>пористость</kwd><kwd>газопроницаемость</kwd><kwd>удельная поверхность</kwd><kwd>размер пор</kwd><kwd>стандартный образец</kwd><kwd>государственный первичный эталон</kwd></kwd-group><kwd-group xml:lang="en"><kwd>porosity</kwd><kwd>gas permeability</kwd><kwd>specific surface area</kwd><kwd>pore size</kwd><kwd>reference material</kwd><kwd>State Primary Measurement  Standard</kwd></kwd-group></article-meta></front><back><ref-list><title>References</title><ref id="cit1"><label>1</label><citation-alternatives><mixed-citation xml:lang="ru">Карнаухов А. П. Адсорбция. Текстура дисперсных и пористых материалов. Новосибирск: Наука. Сиб. предприятие РАН, 1999. 470 с.</mixed-citation><mixed-citation xml:lang="en">Karnaukhov A. P. Adsorption. Texture of Dispersed and Porous Materials. Nauka, Siberian Branch, Novosibirsk, 1999, 470 p. (In Russ.).</mixed-citation></citation-alternatives></ref><ref id="cit2"><label>2</label><citation-alternatives><mixed-citation xml:lang="ru">Paul A. Webb and Orr C. Clyde Analytical Methods in Fine Particle Technology. 1997. Micromeritics corporation, 301 p.</mixed-citation><mixed-citation xml:lang="en">Webb P. A. and Orr C. Analytical Methods in Fine Particle Technology. Micromeritics Corp.,1997, 301 p.</mixed-citation></citation-alternatives></ref><ref id="cit3"><label>3</label><citation-alternatives><mixed-citation xml:lang="ru">Фенелонов В. Б. Введение в основы адсорбции и текстурологии. Новосибирск: Изд-во СО РАН, 2004.</mixed-citation><mixed-citation xml:lang="en">Fenolonov V. B. Introduction to the Elements of Adsorption and Texturology, Izd. SO RAN, Novosibirsk, 2004. (In Russ.).</mixed-citation></citation-alternatives></ref><ref id="cit4"><label>4</label><citation-alternatives><mixed-citation xml:lang="ru">Грек С., Синг К. Адсорбция, удельная поверхность, пористость. Пер. с англ., 2-е изд. М.: Мир,1984. 306 с.</mixed-citation><mixed-citation xml:lang="en">Gregg S. and Sing K. Adsorption, specific surface, porosity, Mir, Moscow (1984). (In Russ.).</mixed-citation></citation-alternatives></ref><ref id="cit5"><label>5</label><citation-alternatives><mixed-citation xml:lang="ru">Sing K. S. W., Everett D. H., Haul R. A.W., Moscou L., Pierotti R. A., Rouquerol J., Siemieniewska T. Reporting physisorption data for gas/solid systems with special reference to the determination of surface area and porosity (Recommendations 1984) // Pure Appl. Chem. 1985. V. 57. No 4. P. 603–619.</mixed-citation><mixed-citation xml:lang="en">Sing K. S. W., Everett D. H., Haul R. A.W., Moscou L., Pierotti R. A., Rouquerol J., Siemieniewska T. Reporting physisorption data for gas/solid systems with special reference to the determination of surface area and porosity (Recommendations 1984). Pure Appl. Chem. 1985; 57(4): 603–619.</mixed-citation></citation-alternatives></ref><ref id="cit6"><label>6</label><citation-alternatives><mixed-citation xml:lang="ru">Федеральный информационный фонд по обеспечению единства измерений [Офиц. сайт]. http://www.fundmetrology.ru/default.aspx.</mixed-citation><mixed-citation xml:lang="en">Federal Information Foundation for the Support of Uniformity of Measurements. Available at: www.fundmetrology.ru/default.aspx. (In Russ.)</mixed-citation></citation-alternatives></ref><ref id="cit7"><label>7</label><citation-alternatives><mixed-citation xml:lang="ru">Об утверждении Государственного первичного эталона единиц удельной адсорбции газов, удельной поверхности, удельного объема и размера пор твердых веществ и материалов: Приказ Федерального агентства по техническому регулированию и метрологии от 29 января 2015 г. № 128.</mixed-citation><mixed-citation xml:lang="en">Decree of the Federal Agency for Technical Regulation and Metrology «On approval of the State Primary Measurement Standard for units of specific gas absorption, specific surface area, specific volume, and pore size of solid substances and materials» No. 128 of 29/01/2015.</mixed-citation></citation-alternatives></ref><ref id="cit8"><label>8</label><citation-alternatives><mixed-citation xml:lang="ru">ASTM D 4222–03(2008). Standard test method for determination of nitrogen adsorption and desorption isotherms of catalysts and catalyst carriers by static volumetric measurements.</mixed-citation><mixed-citation xml:lang="en">ASTM D 4222–03(2008). Standard test method for determination of nitrogen adsorption and desorption isotherms of catalysts and catalyst carriers by static volumetric measurements.</mixed-citation></citation-alternatives></ref><ref id="cit9"><label>9</label><citation-alternatives><mixed-citation xml:lang="ru">DIN 66131. Determination of specific surface area of solids by gas adsorption using the method of Brunauer, Emmett and Teller (BET).</mixed-citation><mixed-citation xml:lang="en">DIN 66131. Determination of specific surface area of solids by gas adsorption using the method of Brunauer, Emmett and Teller (BET).</mixed-citation></citation-alternatives></ref><ref id="cit10"><label>10</label><citation-alternatives><mixed-citation xml:lang="ru">ISO 15901–2:2006. Pore size distribution and porosity of solid materials by mercury porosimetry and gas adsorption – Part 2: Analysis of mesopores and macropores by gas adsorption.</mixed-citation><mixed-citation xml:lang="en">ISO 15901–2:2006. Pore size distribution and porosity of solid materials by mercury porosimetry and gas adsorption – Part 2: Analysis of mesopores and macropores by gas adsorption.</mixed-citation></citation-alternatives></ref><ref id="cit11"><label>11</label><citation-alternatives><mixed-citation xml:lang="ru">Badalyan A., Pendleton P. Analysis of uncertainties in manometric gas adsorption measurements. Propagation of Uncertainties in BET Analyses // Lanmiur. 2003. № 19. P. 7919–7928.</mixed-citation><mixed-citation xml:lang="en">Badalyan A., Pendleton P. Analysis of uncertainties in manometric gas adsorption measurements. Propagation of Uncertainties in BET Analyses. Lanmiur. 2003; (19): 7919–7928.</mixed-citation></citation-alternatives></ref><ref id="cit12"><label>12</label><citation-alternatives><mixed-citation xml:lang="ru">Stefanidou M. Methods for porosity measurement in lime-based mortars // Construction and Building Materials. 2010. V. 24. I. 12, pp. 2572–2578. Doi.org/10.1016/j.conbuildmat.2010.05.019</mixed-citation><mixed-citation xml:lang="en">Stefanidou M. Methods for porosity measurement in limebased mortars. Construction and Building Materials. 2010; 24 (12): 2572–2578. DOI: 10.1016/j.conbuildmat.2010.05.019</mixed-citation></citation-alternatives></ref><ref id="cit13"><label>13</label><citation-alternatives><mixed-citation xml:lang="ru">BIPM [Офиц. сайт]. http://www.bipm.org (дата обращения 09.04.2015)</mixed-citation><mixed-citation xml:lang="en">BIPM. Available at: www.bipm.org</mixed-citation></citation-alternatives></ref><ref id="cit14"><label>14</label><citation-alternatives><mixed-citation xml:lang="ru">Sobina E., Zimathis A., Prinz C., Emmerling F., Unger W., R. de Santis Neves, Galhardo C. E, E. De Robertis, Wang H., Mizuno K. and Kurokawa A. Final report of CCQM-K136 Measurement of porosity properties (specific adsorption, BET specific surface area, specific pore volume and pore diameter) of nanoporous Al2O3 // Metrologia, 2016, Vol.53, № 1а, С. 1–39. DOI: 10.1088/0026–1394/53/1A/08014</mixed-citation><mixed-citation xml:lang="en">Sobina E., Zimathis A., Prinz C., Emmerling F., Unger W., R. de Santis Neves, Galhardo C. E, E. De Robertis, Wang H., Mizuno K. and Kurokawa A. Final report of CCQM-K136 Measurement of porosity properties (specific adsorption, BET specific surface area, specific pore volume and pore diameter) of nanoporous Al2O3. Metrologia. 2016; 53(1а): 1–39. DOI: 10.1088/0026–1394/53/1A/08014.</mixed-citation></citation-alternatives></ref><ref id="cit15"><label>15</label><citation-alternatives><mixed-citation xml:lang="ru">Собина Е. П. Разработка аттестованного стандартного образца нанопористого оксида алюминия. // Измерительная техника. 2016. № 8. С. 68–72.</mixed-citation><mixed-citation xml:lang="en">Sobina E. P. Development of a certified standard reference sample of nanoporous aluminum oxide. Measurement Techniques. 2016; 59 (8): 892–898. (In Russ.).</mixed-citation></citation-alternatives></ref><ref id="cit16"><label>16</label><citation-alternatives><mixed-citation xml:lang="ru">ISO 9277:2010 Determination of the specific surface area of solids by gas adsorption – BET method // ISO [Электронный ресурс]. URL: www.iso.org/standard/44941.html</mixed-citation><mixed-citation xml:lang="en">ISO 9277:2010 Determination of the specific surface area of solids by gas adsorption – BET method. Available at: URL: www.iso.org/standard/44941.html</mixed-citation></citation-alternatives></ref><ref id="cit17"><label>17</label><citation-alternatives><mixed-citation xml:lang="ru">Собина Е. П. Разработка комплекта стандартных образцов открытой пористости твердых веществ, материалов (имитаторов) // Стандартные образцы, 2016, № 2. С. 36–43.</mixed-citation><mixed-citation xml:lang="en">Sobina E. P. Development of сertified reference materials set for opened porosity of solid substances and materials (imitators). Reference materials. 2016; (2): 36–43. (In Russ.). DOI: 10.20915/2077-1177-2016-0-2-36-43</mixed-citation></citation-alternatives></ref></ref-list><fn-group><fn fn-type="conflict"><p>The authors declare that there are no conflicts of interest present.</p></fn></fn-group></back></article>
