Устранение эффекта памяти для корректного определения ртути методом масс-спектрометрии с индуктивно-связанной плазмой

При определении ртути методом масс-спектрометрии с индуктивно-связанной плазмой (ИСП-МС) происходит адсорбция этого элемента на поверхности системы ввода проб прибора: эффект памяти искажает результаты определения следовых количеств ртути. Проведено экспериментальное сравнение эффективности предлагаемых в литературе способов удаления следовых количеств ртути для ее корректного определения методом ИСП-МС и выбран оптимальный отмывающий агент. В качестве отмывающих агентов для очистки системы ввода проб масс-спектрометра Agilent 7900 использовали разбавленные растворы азотной и соляной кислот, растворы хлорида золота, дихромата калия, тиомочевины, L-цистеина, бромида калия, бромата калия различных концентраций в воде, 1 %-ных азотной и соляной кислотах, а также водный раствор аммония пирролидиндитиокарбамата. Установлено, что фонового уровня содержания ртути удается достичь при использовании растворов хлорида золота (5 %), тиомочевины (0,01, 0,1 и 0,5 %), L-цистеина (2 %), бромида и бромата калия (0,5 ммоль/л) в 1,0 %-ной соляной кислоте. Фон понижается при использовании 3- и 5 %-ной HCl, растворов дихромата калия (60 мг/л), бромида и бромата калия (0,01 и 0,05 моль/л) в 1 %-ной соляной кислоте. Применение водного раствора аммония пирролидиндитиокарбамата вызывает резкую деградацию пластиковых трубок системы ввода проб. Эффективность отмывающих агентов на основе соляной кислоты выше, чем на основе азотной кислоты и воды. Наиболее перспективными отмывающими агентами являются бромсодержащие растворы и раствор бихромата калия в соляной кислоте. Оптимальным способом очистки прибора представляется его промывка 0,5 мМ раствором бромида калия в 1,0 %-ной соляной кислоте, что позволяет снизить интенсивность фонового сигнала изотопа ²⁰²Hg и не затрудняет определение других элементов.

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