zldmЗаводская лаборатория. Диагностика материаловIndustrial laboratory. Diagnostics of materials1028-68612588-0187ООО «Издательство «ТЕСТ-ЗЛ»10.26896/1028-6861-2024-90-12-16-26zldm-2359Research ArticleАНАЛИЗ ВЕЩЕСТВАSUBSTANCES ANALYSISРасширение области применения и оценка метрологических характеристик методики определения органического углерода в отходах добычи, переработки и сжигания углейExpanding the scope of application and evaluating the metrological characteristics of the method of determination of organic carbon in wastes of mining, processing and combustion of coalГолынецО. С.GolynetsO. S.

Ольга Станиславовна Голынец,

620075, г. Екатеринбург, ул. Красноармейская, д. 4; 

119049, Москва, Ленинский проспект, д. 4.

Olga S. Golynets,

4, Krasnoarmeiskaya ul., Yekaterinburg, 620075;

4, Leninskii prosp., Moscow, 119049.

golynets_olga@uniim.ruМедведевскихМ. Ю.MedvedevskikhM. Yu.

Мария Юрьевна Медведевских,

119049, Москва, Ленинский проспект, д. 4.

Maria Yu. Medvedevskikh,

4, Leninskii prosp., Moscow, 119049

ЭпштейнС. А.EpshteinSvetlana A.

Светлана Абрамовна Эпштейн,

119049, Москва, Ленинский проспект, д. 4.

 

Svetlana A. Epshtein,

4, Leninskii prosp., Moscow, 119049.

ШохинаО. С.ShokhinaO. S.

Ольга Сергеевна Шохина,

620075, г. Екатеринбург, ул. Красноармейская, д. 4.

Olga S. Shokhina,

4, Krasnoarmeiskaya ul., Yekaterinburg, 620075.

СергееваА. С.SergeevaA. S.

Анна Сергеевна Сергеева

620075, г. Екатеринбург, ул. Красноармейская, д. 4.

Anna S. Sergeeva,

4, Krasnoarmeiskaya ul., Yekaterinburg, 620075.

УНИИМ — филиал ФГУП «ВНИИМ им. Д. И. Менделеева»; Национальный исследовательский технологический университет «МИСИС»РоссияUNIIM — Affiliated Branch of the D. I. Mendeleyev Institute for Metrology; National University of Science and Technology «MISIS»Russian FederationНациональный исследовательский технологический университет «МИСИС»РоссияNational University of Science and Technology «MISIS»Russian FederationУНИИМ — филиал ФГУП «ВНИИМ им. Д. И. Менделеева»РоссияUNIIM — Affiliated Branch of the D. I. Mendeleyev Institute for MetrologyRussian Federation20242312202490121626Copyright © Голынец О.С., Медведевских М.Ю., Эпштейн С.А., Шохина О.С., Сергеева А.С., 20242024Голынец О.С., Медведевских М.Ю., Эпштейн С.А., Шохина О.С., Сергеева А.С.Golynets O.S., Medvedevskikh M.Y., Epshtein S.A., Shokhina O.S., Sergeeva A.S.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.zldm.ru/jour/article/view/2359

Проведены дополнительные исследования в целях расширения области применения и оценки метрологических характеристик ранее разработанной авторами методики гравиметрического определения органического углерода в отходах добычи, переработки и сжигания углей. С использованием метода термогравиметрического анализа с масс-спектрометрическим детектированием (ТГА/МС) показано отсутствие влияния пирита, часто сопутствующего углям, на результаты определения углерода и установлена полнота его извлечения при условиях реализации методики (815 °C). Проанализировали реальные пробы отходов добычи, переработки и сжигания углей, образцы известного состава, приготовленные методами добавок и разбавления, и модельные вещества — образцы последовательного озоления углей различной степени метаморфизма (бурый, каменный и антрацит) с разным содержанием углерода во всем заявленном диапазоне определяемых содержаний (от 0,5 до 60 %). Установлено отсутствие систематической погрешности результатов определения углерода по разработанной методике, оценены показатели точности, повторяемости и воспроизводимости для каждого из четырех поддиапазонов определяемых содержаний. Методика аттестована с присвоением регистрационного номера ФР.1.31.2023.46507 в Федеральном информационном фонде по обеспечению единства измерений. Рассмотрена возможность применения методики для характеризации стандартных образцов, используемых для построения градуировочных характеристик экспрессных инфракрасных анализаторов углерода.

The organic carbon content is one of the marker indicators for wastes of mining, processing and combustion of coal, which reflect the quality of drilling and blasting operations carried out at the deposit, enrichment and safety of gold and slag waste and fly ash. The article presents the results of studies on establishing the scope of application and evaluating the metrological characteristics of a developed analytical procedure for determination of organic carbon in samples of wastes of mining, processing and combustion of solid mineral fuel using the gravimetric method. The applicability of the procedure for rock samples containing pyrites, as well as the completeness of carbon extraction for coal samples of different degrees of metamorphism (brown, hard and anthracite) were tested using thermogravimetric analysis with mass spectroscopic detection (TGA/MS), which allows conducting a qualitative analysis of volatile substances (water, oxides of sulfur and carbon) released from the analyzed samples under the influence of high temperature. The scope of application and measurement range of the measurement procedure were confirmed by studying real samples of wastes of mining, processing and combustion of coal and specially prepared samples based on sequential ashing of coal samples. The absence of systematic bias in the measurement results according to the measurement procedure was established by analyzing attested samples based on rock samples, a standard sample of rock composition (mudstone) GSO 7223–96 (containing no carbon) and a standard sample of coal composition GSO 10877–2017 (with a specified carbon content) prepared by the addition method and the dilution method. The measurement procedure was certified and assigned registration number FR.1.31.2023.46507 in the Federal Information Fund for Ensuring the Uniformity of Measurements. The prospects for using the measurement procedure to characterize matrix reference materials required for constructing calibration characteristics of express infrared carbon analyzers are considered.

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The authors declare that there are no conflicts of interest present.