Дуговое атомно-эмиссионное определение редкоземельных элементов после сорбционного извлечения из растворов, содержащих кальций и фосфор

Предложено использование аминотиоэфирного сорбента 2-(1,3,5-дитиазинан-5-ил)уксусной кислоты (ДТУК) для сорбционного извлечения и концентрирования редкоземельных элементов (РЗЭ) из водных растворов и растворов проб гидроксиапатитов (ГА) и трикальцийфосфатов (ТКФ), легированных РЗЭ. Последующее определение РЗЭ проводили непосредственно в фазе сорбционного концентрата методом атомно-эмиссионной спектрометрии с возбуждением спектра в дуге постоянного тока (ДАЭС). Установлено, что для полного извлечения РЗЭ из модельных солянокислых растворов необходимо добавление 10^–7 г/л HF. С использованием модельных растворов выбраны условия сорбционного извлечения РЗЭ (кислотность растворов, масса сорбента, температура и время сорбции). Способность сорбента ДТУК полностью извлекать РЗЭ в выбранных условиях подтверждена путем анализа растворов реальных образцов ГА и ТКФ методом атомно-эмиссионной спектрометрии с индуктивно-связанной плазмой (АЭС-ИСП). Выбраны условия определения примесей РЗЭ методом ДАЭС — режим работы генератора и сила тока, время экспозиции, форма электродов и расстояние между ними, масса навески пробы. Для уменьшения влияния матрицы пробу разбавляли графитовым порошком (1:1 по массе), для улучшения атомизации РЗЭ в дуговом разряде в пробу вводили носитель — NaCl. Правильность результатов определения РЗЭ в образцах ГА и ТКФ по предложенной сорбционно-атомно-эмиссионной методике подтверждена сравнением с результатами референтного метода АЭС-ИСП. Оценены пределы определения РЗЭ (5 · 10^–6 – 5 · 10^–5 % масс.), относительное стандартное отклонение не превышало 10 %.

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