zldmЗаводская лаборатория. Диагностика материаловIndustrial laboratory. Diagnostics of materials1028-68612588-0187ООО «Издательство «ТЕСТ-ЗЛ»10.26896/1028-6861-2021-87-8-19-22zldm-1466Research ArticleАНАЛИЗ ВЕЩЕСТВАSUBSTANCES ANALYSISСорбция As (III) и Se (IV) из водных растворов для определения методом рентгенофлуоресцентного анализа с полным внешним отражениемSorption of As (III) and Se (IV) from aqueous solutions for subsequent determination by total reflection X-ray fluorescenceФилатоваД. Г.FilatovaD. G.

Дарья Геннадьевна Филатова

Россия, 119991, Москва, ГСП-1, ул. Ленинские горы, д. 1

Darija G. Filatova

GSP-1, 1-3, Leninskiye Gory, Moscow, 119191 Russia

gak1.analyt@gmail.comАрхипенкоА. А.ArkhipenkoA. A.

Александра Александровна Архипенко

Россия, 119991, Москва, ГСП-1, ул. Ленинские горы, д. 1

Alexandra A. Arkhipenko

GSP-1, 1-3, Leninskiye Gory, Moscow, 119191 Russia

СтаткусМ. А.StatkusM. A.

Михаил Александрович Статкус

Россия, 119991, Москва, ГСП-1, ул. Ленинские горы, д. 1

Mikhail A. Statkus

GSP-1, 1-3, Leninskiye Gory, Moscow, 119191 Russia

МихеевИ. В.MikheevI. V.

Иван Владимирович Михеев

Россия, 119991, Москва, ГСП-1, ул. Ленинские горы, д. 1

Ivan V. Mikheev

GSP-1, 1-3, Leninskiye Gory, Moscow, 119191 Russia

БарановскаяВ. Б.BaranovskayaV. B.

Василиса Борисовна Барановская

Россия, 119991, Москва, Ленинский просп., д. 31

Vasilisa B. Baranovskaya

31, Leninsky prosp., Moscow, 119991, Russia

КарповЮ. А.KarpovYu. A.

Юрий Александрович Карпов

Россия, 119991, Москва, Ленинский просп., д. 31

Yury A. Karpov

31, Leninsky prosp., Moscow, 119991, Russia

Московский государственный университет имени М. В. ЛомоносоваРоссияDepartment of Chemistry, M. V. Lomonosov Moscow State UniversityRussian FederationИнститут общей и неорганической химии имени Н. С. Курнакова Российской академии наукРоссияN. S. Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of SciencesRussian Federation2021200820218781922Copyright © Филатова Д.Г., Архипенко А.А., Статкус М.А., Михеев И.В., Барановская В.Б., Карпов Ю.А., 20212021Филатова Д.Г., Архипенко А.А., Статкус М.А., Михеев И.В., Барановская В.Б., Карпов Ю.А.Filatova D.G., Arkhipenko A.A., Statkus M.A., Mikheev I.V., Baranovskaya V.B., Karpov Y.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/1466

Предложен подход к совместному выделению As (III) и Se (IV) из растворов на новом S,N-содержащем сорбенте с последующим определением аналита в фазе сорбента методом рентгенофлуоресцентного анализа с полным внешним отражением (РФА ПВО). Для этой цели синтезирован сорбент с разветвленной структурой на основе полиакриламида, модифицированный с помощью формальдегида и сероводорода. Это гетероатомный сополимер, содержащий в своей цепи сульфидные мостики и сшивку посредством третичного амина. Определены условия количественного совместного извлечения As (III) и Se (IV) — сорбция в 1 М растворах HNO3 в присутствии ионов кальция, нагревание до 60 °C, время контакта фаз — 1 час. Обсужден механизм сорбционного взаимодействия аналитов в данных условиях. Установлено, что 100-кратные избытки железа, цинка и меди не мешают извлечению аналитов, таким образом, возможно применение сорбента для выделения As (III) и Se (IV) из сырья различного типа и продуктов переработки. Разработана методика прямого рентгенофлуоресцентного определения мышьяка и селена с Sr 0,09 и 0,08 соответственно в фазе сорбента. Правильность результатов подтверждена методом ИСП-МС при анализе водных растворов сравнения после растворения сорбата в HNO3 (1:1).

An approach to the simultaneous isolation of As (III) and Se (IV) from solutions on a new S,N-containing sorbent followed by determination of the analyte in the sorbent phase using total reflection X-ray fluorescence (TXRF) has been proposed. To match the goal, a sorbent with a branched structure was synthesized on the base of polyacrylamide modified with formaldehyde and hydrogen sulfide. This is a heteroatomic copolymer containing sulfide bridges in the chain and crosslinking by a tertiary amine. Conditions for the quantitative co-extraction of As (III) and Se (IV), i.e., sorption in solutions of 1 M HNO3 with calcium ions present, heating to 60°C and phase contact time of 1 h were determined. The mechanism of sorption interaction of the analytes under specified conditions is discussed. It is shown that a 100-fold excess of iron, zinc and copper does not interfere with the extraction of analytes, thus providing the possibility of As (III) and Se (IV) isolation from different types of raw materials and processed products using the synthesized sorbent. A method for the direct XRF quantification of arsenic and selenium with sr 0.09 and 0.08, respectively, in the sorbent phase has been developed. The correctness of the results was confirmed by the ICP-MS method in analysis of aqueous reference solution after dissolution of the sorbate in HNO3 (1:1).

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