It is well known that cadmium and zinc at high concentrations adversely affect the environment. Cadmium and its compounds exhibit carcinogenic properties and damage bones [1,2]. Therefore, the determination of heavy-metal ions at a trace level in different environmental and industrial samples is an intricate and important analytical problem. The main procedures of the spectrometric determination of heavy-metal ions do not always meet modern requirements for the detection limit and require their separation from concomitant elements. To increase the determination sensitivity, combined methods that involve preconcentration appear promising.The use of chelating polymer sorbents (PCSs) allows one to perform individual or group preconcentration of microelements from large volumes of solutions of complex composition, to decrease the detection limit, and to eliminate or significantly reduce the influence of macrocomponents, which improves the reliability and accuracy of analysis [3-6].As a rule, chemically modified, complexing sorbents based on cellulose, polystyrene, silica, porous glass, polyurethane foam, and acrylic fiber; ionexchangers chemically modified with complexing reagents highly selective for the recovered elements; aluminum oxide; and, less commonly, commercial anion and cation exchangers are used for element preconcentration [10][11][12][13][14]. However, we have found no data on the analytical application of polybutadienebased sorbents. Therefore, an investigation of the adsorption properties of novel polybutadiene-based sorbents and their analytical application are topical problems.In the present paper, conditions are investigated for cadmium and zinc preconcentration on a new chelating polybutadiene-based sorbent followed by the determination of these elements by flame atomic absorption spectrometry (FAAS). The effects of the sample solution pH, the flow rate of the sample and eluent solutions, the eluent composition, the sample volume, and other parameters have been studied. The developed method has been employed for the determination of trace cadmium and zinc in water obtained after oil pumping and in seawater.
EXPERIMENTAL
Reagents and solutions.Reagents of analytical or chemically pure grade and distilled water were used. Stock solutions of metal ions (1 mg/mL) were prepared by dissolving accurately weighed portions of their salts in water followed by dilution to 1 L volume. Working solutions were made by properly diluting stock solutions with distilled water. Ammonium acetate buffer solutions (pH 3-10) were prepared by mixing corresponding volumes of 0.1 M CH 3 COOH and 0.1 M NH 3 solutions; a commercial volumetric concentrate of HCl (Fixanal) was also used (pH 1-2).In our study, a new chelating polymer sorbent modified with fragments of 2-amino-4-nitro-phenol-6-sulphonic acid was used. To obtain this sorbent, polybutadiene was phosphochlorinated and fragments of 2-amino-4-nitro-phenol-6-sulphonic acid were inserted in the macromolecule using the procedure described in [7]. The obtained sorbent was...
Синтезирован сорбент на основе сополимера малеинового ангидрида со стиролом, содержащий фрагменты м-фенилендиамина. Идентификацию полученного сорбента, высушенного при 50-60 °С, проводили методом инфракрасной спектроскопии. Был исследован процесс сорбции свинца синтезированным сорбентом. С этой целью было определено влияние рН среды, времени, ионной силы, концентрации металла на сорбцию. Эксперимент показал, что максимальная сорбция происходит при рН = 6. Полная сорбция свинца(II) происходит после 3 ч контакта металла с сорбентом. Результаты анализа влияния ионной силы на сорбцию показали, что увеличение ионной силы до 0,6 моль/л на сорбцию влияет незаметно, последующее же увеличение приводит к значительному уменьшению сорбции. Построена изотерма сорбции свинца синтезированным сорбентом и исследованы оптимальные условия концентрирования. Результаты анализа показали, что с увеличением концентрации ионов свинца(II) в растворе увеличивается количество сорбированного металла, а при концентрации 6•10 -3 моль/л оно становится максимальным (pH = 6, СPb +2 = 6•10 -3 моль/л, Vоб. = 20 мл, mсорб. = 0,05 г, СЕ = 405 мг/г). Степень извлечения ионов свинца(II) при оптимальных условиях превышает 95 %. Исследование сорбции проводилось в статических и динамических условиях. Изучено влияние разных минеральных кислот (HClО4, H2SО4, HNО3, HCl) с одинаковой концентрацией на десорбцию свинца(II) из сорбента. Эксперимент показал, что максимальная десорбция свинца(II) происходит в серной кислоте. Таким образом, предлагаемая новая комплексная экспрессная методика, включающая предварительное концентрирование свинца(II) синтезированным сорбентом, позволяет количественно выделять свинец(II) из большого объема пробы со сложным фоновым составом.
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