SILICA GEL WITH COVALENTLY IMMOBILIZED THIOSEMICARBAZIDE FOR SOLID-PHASE CONCENTRATION OF MERCURY

Autor: Konshina, Dzh. N., Open'ko, V. V., Temerdashev, Z. A., Konshin, V. V., Romanovskii, K. A.
Jazyk: ruština
Rok vydání: 2014
Zdroj: Analitika i kontrol` (Analytics and control); Том 18, № 4 (2014); P. 451-457
Аналитика и контроль; Том 18, № 4 (2014); P. 451-457
ISSN: 2073-1442
2073-1450
1542-2119
Popis: А new thiosemicarbazide modified silica gel sorbent was prepared and applied for preconcentration of trace mercury(II) prior to the measurement by spectrophotometry and atomic absorption spectroscopy. The optimization of some analytical parameters affecting the adsorption of the analyte such as acidity, shaking time, sample flow rate and volume, eluent condition, and interfering substances were investigated. At pH 2, the maximum static adsorption capacity of Hg(II) onto the thiosemicarbazide modified silica gel was 0.49 мМ∙g-1 . The sorbent was used to remove mercury in a dynamic mode. Changing the speed of pumping the solution (0.5 ml / min (0.25 cm / min) to 6 ml / min (3.2 cm / min)) as an increase in volume from 50 ml to 2000 ml to levels of concentrations (0.0125 mM / l, 0.0375mM / l, 0.075mM / l) did not affect the recovery of mercury. The quantitative recovery (>95 %) of Hg(II) could be obtained using 5 mL of 6 mol L−1 HCl solution as eluent. Common coexisting substances did not interfere with the separation of mercury(II) under optimal conditions. The detection limit of sorption-spectrophotometric method definition of mercury was 0.07 µg L−1, and the relative standard deviation (RSD) was lower than 5.0 % . The prepared sorbent was successfully applied for the preconcentration of trace Hg(II) in mineralizate sample fish.Keywords: silica gel, thiosemicarbazide, sorption, mercury, spectrophotometry(Russian)DOI: http://dx.doi.org/10.15826/analitika.2014.18.4.012Dzh. N. Konshina, V.V. Open'ko, Z.A. Temerdashev, V.V. Konshin, K.A. Romanovskii Federal State Educational Institution of Higher Professional Education «Kuban State University», Krasnodar, Russian FederationREFERENCES1. Vlasova N.N, Oborina E.N, Grigor`eva O.Yu., Voronkov M.G. [Organosilicon ion-exchange and complexing adsorbents]. Russian Chemical Reviews, 2013, vol. 82, no. 5, pp. 449-465. doi:10.1070/RC2013v082n05ABEH004301 (in Russian).2. Kara D., Fisher A. 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Осуществлен синтез силикагеля с химически иммобилизованным тиосемикарбазидом (степень функционализации 0.49 мМ/г). Изучены некоторые параметры, влияющие на адсорбционную способность полученного материала по отношению к ртути, такие как рН, время контакта фаз, объем раствора и элюента, а также селективность сорбции в присутствии посторонних ионов. Максимальная сорбционная емкость полученного силикагеля по отношению к ионам ртути при рН = 2 составила 0.48 ± 0.04 мМ/г. Изменение скорости пропускания (от 0.5 мл/мин (0.25 см/мин) до 6 мл/мин (3.2 см/мин)) как и увеличение объема пропускаемого раствора от 50 мл до 2000 мл для уровней концентраций 0.0125, 0.0375 и 0.075мМ/л не влияет на степень извлечения ртути. Количественной десорбции ртути можно добиться при использовании 5 мл 6 МНСl. В выбранных условиях концентрирования ртути присутствие в растворе Fe3+, Zn2+ Cu2+, Pb2+, Co2+, Ni2+ и Cd2+ в n∙102 мольных избытках не влияет на степень её извлечения. Полученный сорбционный материал был применен для сорбционно-спектрофотометрического определения ртути в минерализате, полученном после СВЧ автоклавного разложения образца рыбы.Ключевые слова: силикагель, тиосемикарбазид, сорбция, ртуть, спектрофотометрия DOI: http://dx.doi.org/10.15826/analitika.2014.18.4.012 ЛИТЕРАТУРА1. Кремнийорганические ионообменные и комплексообразующие сорбенты / Н.Н. Власова [и др.] // Успехи химии. 2013. T. 82, №5. C. 449-464.2. Kara D., Fisher A. Modified silica gel and their use for the preconcentration of trace elements // Separation and purification reviews. 2012. V. 41. P. 267-317.3. Sigma-aldrich // [электронный ресурс]: http://www.sigmaaldrich.com/catalog/ search?interface=All&term=silica&N=0&mode=match%20partialmax&focus=product&lang=en®ion=RU (дата обращения 01.08. 2014).4. Silicycle // [электронный ресурс]: http://www.silicycle.com/ (дата обращения 01.08. 2014).5. Химия привитых поверхностных соединений / Г.В. Лисичкин [и др.]. 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