zldmЗаводская лаборатория. Диагностика материаловIndustrial laboratory. Diagnostics of materials1028-68612588-0187ООО «Издательство «ТЕСТ-ЗЛ»10.26896/1028-6861-2023-89-5-5-13zldm-1927Research ArticleАНАЛИЗ ВЕЩЕСТВАSUBSTANCES ANALYSISСопоставление методических подходов к определению органического углерода в отходах добычи, переработки и сжигания углейComparison of methodological approaches to the determination of organic carbon in wastes of mining, processing and combustion of coalСергееваА. С.SergeevaA. S.

Анна Сергеевна Сергеева

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

Anna S. Sergeeva

4, Krasnoarmeiskaya ul., Yekaterinburg, 620075

golynets_olga@uniim.ruГолынецО. С.GolynetsO. S.

Ольга Станиславовна Голынец

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

Olga S. Golynets

4, Krasnoarmeiskaya ul., Yekaterinburg, 620075

МедведевскихМ. Ю.MedvedevskikhM. Yu.

Мария Юрьевна Медведевских

119049, Москва, Ленинский просп., д. 4.

Maria Yu. Medvedevskikh

 4, Leninskii prosp., Moscow, 119049

КочетковаЕ. М.KochetkovaE. M.

Елизавета Максимовна Кочеткова

119049, Москва, Ленинский просп., д. 4.

Elizaveta M. Kochetkova

 4, Leninskii prosp., Moscow, 119049

ЭпштейнС. А.EpsteinS. A.

Светлана Абрамовна Эпштейн

119049, Москва, Ленинский просп., д. 4.

Svetlana A. Epstein

 4, Leninskii prosp., Moscow, 119049

УНИИМ — филиал ФГУП «ВНИИМ им. Д. И. Менделеева»РоссияUNIIM — Affiliated Branch of the D. I. Mendeleyev Institute for MetrologyRussian FederationНациональный исследовательский технологический университет «МИСиС»РоссияNational University of Science and Technology «MISiS»Russian Federation202326052023895513Copyright © Сергеева А.С., Голынец О.С., Медведевских М.Ю., Кочеткова Е.М., Эпштейн С.А., 20232023Сергеева А.С., Голынец О.С., Медведевских М.Ю., Кочеткова Е.М., Эпштейн С.А.Sergeeva A.S., Golynets O.S., Medvedevskikh M.Y., Kochetkova E.M., Epstein S.A.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/1927

Содержание органического углерода является одним из ключевых показателей при определении сфер использования отходов добычи, переработки и сжигания углей. Результаты его определения различными методами анализа во многих случаях несопоставимы друг с другом, что не позволяет получать достоверную информацию о составе отходов. Цель настоящего исследования заключалась в обобщении существующих методических подходов и выборе наиболее эффективного из них для определения органического углерода в пробах отходов добычи, переработки и сжигания углей. На основании проведенного обзора способов его определения в различных природных и техногенных объектах выбраны три наиболее подходящих метода. Первый основан на расчете содержания органического углерода по разности содержаний общего и карбонатного углерода, определяемых с использованием CHN-анализатора и гравиметрически соответственно; второй — на определении зольности, влаги и карбонатного углерода; третий метод включает деминерализацию пробы соляной кислотой, высушивание и прокаливание полученного остатка. В качестве объектов исследования служили пробы отходов добычи, переработки и сжигания углей с массовой долей органического углерода от 0 до 60 %. На основе полученных экспериментальных данных и с учетом возможных ограничений выбрана методика определения содержания несгоревшего углерода в золе и шлаках ТЭЦ, основанная на методе № 3. Проверена применимость разработанной методики для анализа более широкого круга объектов, включающего помимо отходов сжигания углей также отходы их добычи и переработки, продемонстрирована сопоставимость результатов с полученными другими методами, выполнена предварительная оценка метрологических характеристик. Методика может быть использована для анализа образцов сравнения, применяемых при построении градуировочных характеристик для определения органического углерода инструментальными методами, а также для установления метрологических характеристик стандартных образцов состава отходов добычи, переработки и сжигания углей.

The content of organic carbon is one of the key indicators in determining the areas of using waste of mining, processing and combustion of coal. The measurement results obtained by existing measurement methods are often incomparable to each other, which does not allow obtaining a reliable information about the waste composition. The goal of this study is to generalize current methodological approaches and choose the most effective one for determining the content of organic carbon in samples of waste of mining, processing and combustion of coal. Three most appropriate methods were selected proceeding from the analysis of the methods used for determining organic carbon in various natural and technogenic objects. Method No. 1 is based on the calculation of organic carbon content as the difference between total carbon measured by a CHN analyzer and carbonate carbon determined by the gravimetric method. In method No. 2, the determination of organic carbon content is carried out through the determination of the ash, moisture and carbonate carbon content. Method No. 3 includes demineralization of the sample with hydrochloric acid, drying, and calcination of the resulting residue. The samples of waste of mining, processing and combustion of coal with mass fraction of organic carbon from 0 to 60% were used as objects of the research. According to the results of experimental studies and taking into account possible limitations, measurement procedure based on method No. 3 for determining the content of unburned carbon in ash and slag from a thermal power plant was chosen. The applicability of the newly developed measurement procedure was verified for an extended area of objects, which includes, in addition to the samples of coal combustion waste, the samples of waste of their mining and processing. The comparability of the results obtained by other methods was demonstrated, and a preliminary assessment of the metrological characteristics was performed. The measurement procedure can be used in analysis of the reference samples used for construction of the calibration characteristics in the determination of organic carbon by instrumental methods, as well as in the determination of the metrological characteristics of the reference materials of the composition of waste of mining, processing and combustion of coal.

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