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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">zldm</journal-id><journal-title-group><journal-title xml:lang="ru">Заводская лаборатория. Диагностика материалов</journal-title><trans-title-group xml:lang="en"><trans-title>Industrial laboratory. Diagnostics of materials</trans-title></trans-title-group></journal-title-group><issn pub-type="ppub">1028-6861</issn><issn pub-type="epub">2588-0187</issn><publisher><publisher-name>ООО «Издательство «ТЕСТ-ЗЛ»</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="doi">10.26896/1028-6861-2017-83-12-61-70</article-id><article-id custom-type="elpub" pub-id-type="custom">zldm-605</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>ОЦЕНКА СООТВЕТСТВИЯ. АККРЕДИТАЦИЯ ЛАБОРАТОРИЙ</subject></subj-group><subj-group subj-group-type="section-heading" xml:lang="en"><subject>COMPLIANCE VERIFICATION. LABORATORY ACCREDITATION</subject></subj-group></article-categories><title-group><article-title>ОЦЕНКА СООТВЕТСТВИЯ ЗАЯВЛЯЕМЫМ ХАРАКТЕРИСТИКАМ ДИФРАКТОМЕТРОВ ДЛЯ ОПРЕДЕЛЕНИЯ ФАЗОВОГО СОСТАВА ВЕЩЕСТВ И МАТЕРИАЛОВ</article-title><trans-title-group xml:lang="en"><trans-title>CONFORMITY ASSESSMENT OF THE CLAIMED CHARACTERISTICS OF DIFRACTOMETERS FOR PHASE ANALYSIS OF 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>Кодесс</surname><given-names>Б. Н.</given-names></name><name name-style="western" xml:lang="en"><surname>Kodess</surname><given-names>B. N.</given-names></name></name-alternatives><email xlink:type="simple">kodess@mail.ru</email><xref ref-type="aff" rid="aff-1"/></contrib><contrib contrib-type="author" corresp="yes"><name-alternatives><name name-style="eastern" xml:lang="ru"><surname>Кузин</surname><given-names>А. Ю.</given-names></name><name name-style="western" xml:lang="en"><surname>Kuzin</surname><given-names>A. Yu.</given-names></name></name-alternatives><email xlink:type="simple">kodess@mail.ru</email><xref ref-type="aff" rid="aff-1"/></contrib></contrib-group><aff-alternatives id="aff-1"><aff xml:lang="ru"><institution>ФГУП «ВНИИМС», Москва</institution><country>Россия</country></aff><aff xml:lang="en"><institution>All-Russian Research Institute of Metrological Service, Moscow</institution><country>Russian Federation</country></aff></aff-alternatives><pub-date pub-type="collection"><year>2017</year></pub-date><pub-date pub-type="epub"><day>01</day><month>12</month><year>2017</year></pub-date><volume>83</volume><issue>12</issue><fpage>61</fpage><lpage>70</lpage><permissions><copyright-statement>Copyright &amp;#x00A9; Кодесс Б.Н., Кузин А.Ю., 2017</copyright-statement><copyright-year>2017</copyright-year><copyright-holder xml:lang="ru">Кодесс Б.Н., Кузин А.Ю.</copyright-holder><copyright-holder xml:lang="en">Kodess B.N., Kuzin A.Y.</copyright-holder><license xml:lang="ru" license-type="creative-commons-attribution" xlink:href="https://creativecommons.org/licenses/by/4.0/" xlink:type="simple"><license-p>Данная работа распространяется под лицензией Creative Commons Attribution 4.0.</license-p></license><license xml:lang="en" 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.zldm.ru/jour/article/view/605">https://www.zldm.ru/jour/article/view/605</self-uri><abstract><p>Представлен обзор особенностей сертификации дифрактометрических измерительных систем с применением коротковолнового излучения, предназначенных для фазового анализа веществ и материалов. Точность результатов фазового анализа в основном определяется методическими погрешностями, а не инструментальными характеристиками дифрактометров. Для идентификационного (качественного и полукачественного) анализа используют базы структурных данных и отношения интегральных интенсивностей брегговских отражений. Для оценки достоверности результатов количественного фазового анализа необходимо провести испытания измерительной системы в целом, включая программное обеспечение, с применением аттестованных СО параметров решетки (размеров элементарной ячейки), СО с аттестованным соотношением интенсивностей брегговских отражений и/или СО для методов Ритвельда, позволяющих определить содержание каждой фазы. Использование адекватных СО обеспечивает повышение достоверности результатов фазового анализа.</p><p> </p></abstract><trans-abstract xml:lang="en"><p>A review of the features of test performances for the purpose of certification of difractometric measuring systems using short-wave radiation (x-ray and neutron radiation) which are intended for diagnostics of phase composition of substances and materials is presented. The main contribution to the uncertainty of the results of phase analyses is made by methodological errors, much more significant than instrumental characteristics of difractometers. The problems of conformity assessment to the claimed characteristics of the corresponding difractometric systems intended for various types of phase analysis are considered. For the identification (referenced as «qualitative» or «semi-qualitative») analysis, various structural databases and sometimes the values of the integral intensity ratios of Bragg reflections of certified standard reference materials (CSRMs) are used. To achieve high accuracy and reliability of quantitative phase analysis calculations of the angular positions of reflections should be performed on the basis on standardized (certified) reference (evaluated) data of crystallographic databases. To assess the reliability of the results, the equipment (difractometric measuring systems) should be tested together with the software and CSRMs sets should be also used. The sets of CSRMs include certified characteristics, i.e. the lattice constants (unit cell dimension), the intensity ratio of Bragg reflections, and/or the mass fraction of the composition of each phase, determined by Rietveld methods, which provide rapid achievement of higher accuracy and reliability. The sets of CSRMs used for testing and especially during operation of difractometers enable specialists and metrologists to ensure high quality and legitimacy of measurement results, which allows further refining of materials engineering technology and ensure the reliability and safety of products.</p></trans-abstract><kwd-group xml:lang="ru"><kwd>фазовый анализ</kwd><kwd>заявляемые характеристики дифрактометров</kwd><kwd>оценка соответствия</kwd><kwd>испытания и периодическая поверка</kwd><kwd>базы стандартных справочных данных</kwd><kwd>стандартные образцы дифракционных свойств</kwd></kwd-group><kwd-group xml:lang="en"><kwd>accuracy and reliability of phase analysis</kwd><kwd>claimed characteristics of difractometers</kwd><kwd>conformity assessment</kwd><kwd>standard reference database</kwd><kwd>certified standard reference materials (CSRMs) of diffraction properties</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">Кодесс Б. Н., Нечаева Е. Н. Модель описания эволюции кристаллического вещества / Труды Первого Российского кристаллографического конгресса (от конвергенции наук к природоподобным технологиям). — М.: НП-Принт, 2016. С. 300.</mixed-citation><mixed-citation xml:lang="en">Kodess B. N., Nechaeva E. N. The model for evolution description of crystalline substance / Proc. Russian Crystallography Society (from convergence of sciences to nature-similar technologies). — Moscow: NP-Print, 2016. P. 300 [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit2"><label>2</label><citation-alternatives><mixed-citation xml:lang="ru">Kodess B. N., Kommel L. A., Teterin, G. P., Ovcharov V. K. Microstructure Evolution in Ti-Alloys During Severe Deformation by Electric Upsetting and Impact Fused-Forging Modeling / T. Lowe and R. Z. Valiev, eds. Investigations and Applications of Severe Plastic Deformation. Vol. 80. — Springer Science &amp; Business Media, 2000. P. 211 – 218.</mixed-citation><mixed-citation xml:lang="en">Kodess B. N., Kommel L. A., Teterin, G. P., Ovcharov V. K. Microstructure Evolution in Ti-Alloys During Severe Deformation by Electric Upsetting and Impact Fused-Forging Modeling / T. Lowe and R. Z. Valiev, eds. Investigations and Applications of Severe Plastic Deformation. Vol. 80. — Springer Science &amp; Business Media, 2000. P. 211 – 218.</mixed-citation></citation-alternatives></ref><ref id="cit3"><label>3</label><citation-alternatives><mixed-citation xml:lang="ru">Kodess B. N., Teterin G. P., Kommel L. A., Ovcharov V. K. Structure and mechanical properties of the engine valves with intermetallic disk / MRS Proceedings. 1998. Vol. 552. P. KK8.37.1.</mixed-citation><mixed-citation xml:lang="en">Kodess B. N., Teterin G. P., Kommel L. A., Ovcharov V. K. Structure and mechanical properties of the engine valves with intermetallic disk / MRS Proceedings. 1998. Vol. 552. P. KK8.37.1.</mixed-citation></citation-alternatives></ref><ref id="cit4"><label>4</label><citation-alternatives><mixed-citation xml:lang="ru">Кодесс Б. Н., Сарин В. А. Нейтронный дифрактометр для определения структурных характеристик монокристаллов / Измерительная техника. 2014. № 11. С. 51 – 54.</mixed-citation><mixed-citation xml:lang="en">Kodess B., Sarin V. A. Neutron diffractometer for determining the structural characteristics of single crystals / Measur. Tech. 2015. Vol. 57. N 11. P. 1299 – 1303.</mixed-citation></citation-alternatives></ref><ref id="cit5"><label>5</label><citation-alternatives><mixed-citation xml:lang="ru">Cline J. P., Mendenhall M. H., Black D., et al. The Optics and Alignment of the Divergent Beam Laboratory X-ray Powder Diffractometer and its Calibration Using NIST Standard Reference Materials / J. Res. NIST. 2015. Vol. 120. P. 173 – 222.</mixed-citation><mixed-citation xml:lang="en">Cline J. P., Mendenhall M. H., Black D., et al. The Optics and Alignment of the Divergent Beam Laboratory X-ray Powder Diffractometer and its Calibration Using NIST Standard Reference Materials / J. Res. NIST. 2015. Vol. 120. P. 173 – 222.</mixed-citation></citation-alternatives></ref><ref id="cit6"><label>6</label><citation-alternatives><mixed-citation xml:lang="ru">Mendenhall M. H., Henins A., Windover D., Cline J. P. Characterization of a self-calibrating, high-precision, stacked-stage, vertical dual-axis goniometer / Metrologia. 2016. Vol. 53. N 3. P. 933 – 944.</mixed-citation><mixed-citation xml:lang="en">Mendenhall M. H., Henins A., Windover D., Cline J. P. Characterization of a self-calibrating, high-precision, stacked-stage, vertical dual-axis goniometer / Metrologia. 2016. Vol. 53. N 3. P. 933 – 944.</mixed-citation></citation-alternatives></ref><ref id="cit7"><label>7</label><citation-alternatives><mixed-citation xml:lang="ru">Kodess B. N. Structure of multi-component super-alloy systems / Proceedings of «Intermetallics 2013» conf. — Bad Staffelstein, Germany, 2013. P. 7.</mixed-citation><mixed-citation xml:lang="en">Kodess B. N. Structure of multi-component super-alloy systems / Proceedings of «Intermetallics 2013» conf. — Bad Staffelstein, Germany, 2013. P. 7.</mixed-citation></citation-alternatives></ref><ref id="cit8"><label>8</label><citation-alternatives><mixed-citation xml:lang="ru">Золотухин П. А., Кодесс Б. Н. Метрологическое обеспечение качества монокристаллических пленок / Труды Первого Российского кристаллографического конгресса (от конвергенции наук к природоподобным технологиям). — М.: НП-Принт, 2016. С. 315.</mixed-citation><mixed-citation xml:lang="en">Zolotukhin P. A., Kodess B. N. The metrological assuring of the quality of single-crystal films / Proc. Russian Crystallography Society (from convergence of sciences to nature-similar technologies). — Moscow: NP-Print, 2016. P. 315 [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit9"><label>9</label><citation-alternatives><mixed-citation xml:lang="ru">Mighell A. D., Karen V. L. NIST crystallographic databases for research and analysis / J. Res. NIST. 1996. Vol. 101. N 3. P. 273 – 280.</mixed-citation><mixed-citation xml:lang="en">Mighell A. D., Karen V. L. NIST crystallographic databases for research and analysis / J. Res. NIST. 1996. Vol. 101. N 3. P. 273 – 280.</mixed-citation></citation-alternatives></ref><ref id="cit10"><label>10</label><citation-alternatives><mixed-citation xml:lang="ru">Hart H. V. ZONES: a search/match database for single-crystal electron diffraction / J. Appl. Cryst. 2002. Vol. 35. N 5. P. 552 – 555.</mixed-citation><mixed-citation xml:lang="en">Hart H. V. ZONES: a search/match database for single-crystal electron diffraction / J. Appl. Cryst. 2002. Vol. 35. N 5. P. 552 – 555.</mixed-citation></citation-alternatives></ref><ref id="cit11"><label>11</label><citation-alternatives><mixed-citation xml:lang="ru">Bish D. L., Howard S. A. Quantitative phase analysis using the Rietveld method / J. Appl. Cryst. 1988. Vol. 21. N 2. P. 86 – 91.</mixed-citation><mixed-citation xml:lang="en">Bish D. L., Howard S. A. Quantitative phase analysis using the Rietveld method / J. Appl. Cryst. 1988. Vol. 21. N 2. P. 86 – 91.</mixed-citation></citation-alternatives></ref><ref id="cit12"><label>12</label><citation-alternatives><mixed-citation xml:lang="ru">Winburn R. S. et al. Rietveld quantitative X-ray diffraction analysis of NIST fly ash standard reference materials / Powder Diffraction. 2000. Vol. 15. N 03. P. 163 – 172.</mixed-citation><mixed-citation xml:lang="en">Winburn R. S. et al. Rietveld quantitative X-ray diffraction analysis of NIST fly ash standard reference materials / Powder Diffraction. 2000. Vol. 15. N 03. P. 163 – 172.</mixed-citation></citation-alternatives></ref><ref id="cit13"><label>13</label><citation-alternatives><mixed-citation xml:lang="ru">Kodess B., Kommel I., Shabalin D. Standard reference materials for validation crystal software / Acta Crystallogr. A. 2010. Vol. 66. P. 314.</mixed-citation><mixed-citation xml:lang="en">Kodess B., Kommel I., Shabalin D. Standard reference materials for validation crystal software / Acta Crystallogr. A. 2010. Vol. 66. P. 314.</mixed-citation></citation-alternatives></ref><ref id="cit14"><label>14</label><citation-alternatives><mixed-citation xml:lang="ru">Кодесс Б. Н., Норе Н., Бескровный А. И. и др. Стандартные образцы для анализа структурных характеристик веществ с водородным типом химической связи / Труды Первого Российского кристаллографического конгресса (от конвергенции наук к природоподобным технологиям. — М.: НП-Принт, 2016. С. 239.</mixed-citation><mixed-citation xml:lang="en">Kodess B. N., Nore N., Beskrovnyi A. I., et al. Standard reference materials for analysis of structural characteristics of substance with hydrogen chemical bond / Proc. Russian Crystallography Society (from convergence of sciences to nature-similar technologies). — Moscow: NP-Print, 2016. P. 239.</mixed-citation></citation-alternatives></ref><ref id="cit15"><label>15</label><citation-alternatives><mixed-citation xml:lang="ru">Кодесс Б. Н. Метрологическое обеспечение высокоточных измерений характеристик ключевых материалов современных технологий и их стандартные образцы состава и свойств / История науки и техники. 2010. № 9. С. 29 – 36.</mixed-citation><mixed-citation xml:lang="en">Kodess B. N. Metrological assurance of high accuracy measurements of key materials characteristics for modern technology and their certified reference materials of composition and properties / Istor. Nauki Tekhn. 2010. N 9. P. 29 – 36 [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit16"><label>16</label><citation-alternatives><mixed-citation xml:lang="ru">Кузин А., Лахов В., Новиков Ю. и др. Российские стандарты для измерения линейных размеров в нанотехнологиях / Наноиндустрия. 2009. № 3. С. 1 – 5.</mixed-citation><mixed-citation xml:lang="en">Kuzin A., Lakhov V., Novikov Yu., et al. Russian standards for measurements of linear sizes in nanotechnologies / Nanoindustriya. 2009. N 3. P. 1 – 5 [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit17"><label>17</label><citation-alternatives><mixed-citation xml:lang="ru">Gadayev A., Kodess B. By-product materials in cement clinker manufacturing / Cement and Concrete Res. 1999. Vol. 29. N 2. P. 187 – 191.</mixed-citation><mixed-citation xml:lang="en">Gadayev A., Kodess B. By-product materials in cement clinker manufacturing / Cement and Concrete Res. 1999. Vol. 29. N 2. P. 187 – 191.</mixed-citation></citation-alternatives></ref><ref id="cit18"><label>18</label><citation-alternatives><mixed-citation xml:lang="ru">Горелик С. С., Скаков Ю. А., Расторгуев Л. Н. Рентгенографический и электронно-оптический анализ. Учеб. пос. для вузов. — М.: МИСиС, 1994. — 328 с.</mixed-citation><mixed-citation xml:lang="en">Gorelik S. S., Skakov Yu. A., Rastorguev L. N. X-ray and electron-optical analysis. Textbook for high schools.. — Moscow: MISiS, 1994. — 328 p. [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit19"><label>19</label><citation-alternatives><mixed-citation xml:lang="ru">Нахмансон М. С., Фекличев В. Г. Диагностика состава материалов рентгенодифрак-ционными и спектральными методами. — Л.: Машиностроение, 1990. — 357 с.</mixed-citation><mixed-citation xml:lang="en">Nakhmanson M. S., Feklichev V. G. Diagnostic of material composition by x-ray and spectroscopic methods. — Leningrad: Mashinostroenie, 1990. — 357 p. [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit20"><label>20</label><citation-alternatives><mixed-citation xml:lang="ru">Зевин Л. С., Завьялова Л. Л. Количественный рентгенографический фазовый анализ. — М.: Недра, 1974. — 184 с.</mixed-citation><mixed-citation xml:lang="en">Zevin L. S., Zav’yalova L. L. Quantitative x-ray powder diffraction phase analysis. — Moscow: Nedra, 1974. — 184 p. [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit21"><label>21</label><citation-alternatives><mixed-citation xml:lang="ru">Kodess B. N., Kodess P. The study of nano-fragmentary materials for new x-ray standard Reference Materials / Advance of X-Ray Analysis. 2016. Vol. 59. P. 243 – 254.</mixed-citation><mixed-citation xml:lang="en">Kodess B. N., Kodess P. The study of nano-fragmentary materials for new X-ray standard Reference Materials / Advance of X-Ray Analysis. 2016. Vol. 59. P. 243 – 254.</mixed-citation></citation-alternatives></ref><ref id="cit22"><label>22</label><citation-alternatives><mixed-citation xml:lang="ru">Кодесс Б. Н., Лютцау А. В., Котелкин А. В. и др. Неразрушающий контроль многокомпонентных материалов методами портативной дифрактометрии / Поверхность. Рентгеновские, синхротронные и нейтронные исследования. 2002. № 9. С. 10 – 12.</mixed-citation><mixed-citation xml:lang="en">Kodess B. N., Lutzao A. V., Kotelkin A. V., et al. Non-destructive testing of multicomponent materials using portable diffractometry / Poverkhn. Rentgen. Sinkhrotr. Neitron. Issl. 2002. N 9. P. 10 – 12 [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit23"><label>23</label><citation-alternatives><mixed-citation xml:lang="ru">Богданов Г. П., Кузин А. Ю., Ржевский Д. А. Критерии отнесения методик выполнения измерений к методикам, подлежащим аттестации / Измерительная техника. 2001. № 1. С. 66 – 69.</mixed-citation><mixed-citation xml:lang="en">Bogdanov G. P., Kuzin A. Y., Rzhevskii D. A. Criteria for assigning measurement methods as requiring certification / Measur. Tech. 2001. Vol. 44. P. 1. P. 108 – 112.</mixed-citation></citation-alternatives></ref><ref id="cit24"><label>24</label><citation-alternatives><mixed-citation xml:lang="ru">Кодесс Б. Н., Исаев Л. К. Испытания дифрактометрических измерительных систем на основе системы стандартных образцов / Труды Первого Российского кристаллографического конгресса (от конвергенции наук к природоподобным технологиям). — М.: НП-Принт, 2016. С. 168.</mixed-citation><mixed-citation xml:lang="en">Kodess B. N., Isaev L. K. The testing of diffractometric measurement systems for type approve on basis of the system of Standard References Materials / Proc. Russian Crystallography Society (from convergence of sciences to nature-similar technologies). — Moscow: NP-Print, 2016. P. 168 [in Russian].</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>
