РАЗРАБОТКА МЕТОДИКИ РЕНТГЕНОФЛУОРЕСЦЕНТНОГО ОПРЕДЕЛЕНИЯ СОДЕРЖАНИЙ GA, HF И TA В РЕДКОЗЕМЕЛЬНЫХ РУДАХ
Аннотация
Представлены результаты исследований по разработке методики определения содержаний Ga, Hf и Ta применительно к образцам редкоземельных руд Катугинского месторождения (Забайкалье) с использованием кристалл-дифракционного спектрометра S8 TIGER. В качестве аналитической линии для Ta целесообразно использовать TaLβ1-линию, для измерения Ga и Hf выбраны GaKα1 (0.1340 нм) и HfLβ1 (0.1374 нм) спектральные линии. Произведена экспериментальная оценка вклада в интенсивности используемых аналитических линий излучения Dy, Ho, Er, Tm, Yb и Lu. Для количественного определения содержаний Ga необходимо учитывать влияние наложения на интенсивность GaKα1-линииизлучения следующих спектральных линий: ZnKb1,3, NbKβ1II, ErLγ1, HfLβ1, TaLβ1; для TaLβ1-линии: ZnKb1,3,GaKα1, NbKβ1II, ErLγ1, HfLβ1, WLβ1- линий; для HfLβ1-линии: CuKβ1, GaKa1, ZrKβ1II,DyLγ4, ErLγ1 и TaLβ1. Выбраны условия для возбуждения и регистрации излучения характеристических линий и фонового излучения Ga, Hf и Ta. Время измерения интенсивностей излучения аналитических линий и фона Ga, Hf и Ta: 100 и 80, 200 и 150, 300 и 200 с соответственно. Рассчитаны пределы обнаружения для Ga, Hf и Ta соответственно (в ppm): 1.6, 4.3, 2.6. Для построения градуировочных кривых использовали набор стандартных образцов и приготовленных синтетических смесей. Диапазоны определяемых содержаний составили для Ga, Hf и Ta соответственно (в ppm): 1.6 – 212, 4.3 – 960, 2.6 – 5200. С помощью разработанной методики выполнено количественное определение концентраций Ga, Hf и Ta в 120 образцах редкоземельных руд; диапазон содержаний определяемых элементов составил соответственно (в ppm): 1.6 – 174, 4 – 1950, 2 – 1900.
Ключевые слова: рентгенофлуоресцентный анализ, редкоземельные руды, количественное определение содержаний Ga, Hf, Ta, редкоземельные элементы (РЗЭ), наложение линий, способ эмпирических поправок
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