В статье представлены первые результаты апробации макета светодиодного минифотометра, предназначенного для быстрого и чувствительного определения элементов в форме окрашенных комплексов с аналитическими реагентами в лаборатории и во внелабораторных условиях, например, для анализа природной воды на месте отбора проб. Новый прибор состоит из двух фотометрических устройств, объединенных общей системой управления, регистрации и представления результатов. Одно из устройств обеспечивает измерение коэффициента пропускания, другое -измерение коэффициента диффузного отражения. Сигнал регистрируется в видимой области излучения. Метрологические параметры прибора определены на примере двух систем: цветных комплексов марганца(II) с органическими аналитическими реагентами 1-(2-пиридилазо)-2-нафтолом (ПАН) и 2-(2-хинолиназо)-5-диэтиламинофенолом (ХАДАФ), известная реакция и новая, соответственно, а также по собственной окраске. Проведено сравнение спектров, полученных на минифотометре и серийных спектрофотометрах. Результаты проиллюстрированы на примере анализа образцов чая. Разработан компьютерный алгоритм обработки результатов измерений, учитывающий различия интенсивностей излучения светодиодов в разных спектральных интервалах. Показана возможность определения ионов металлов на уровне ≤1 мкг/см 3 .Ключевые слова: определение марганца(II), комплексные соединения, органические аналитические реагенты, анализ чая, светодиодный минифотометр, спектроскопия диффузного отражения. Results of testing a prototype light-emitting diod miniphotometer for rapid and sensitive elements determination both in laboratory and in field conditions are presented. The new photometer consists of two devices providing measurements of absorbance and diffuse reflectance, having aТонкие химические технологии / Fine Chemical Technologies 2017 том 12 № 5Определение марганца(II) методом спектроскопии диффузного отражения joint system of data management, registration and presentation of the results. The measurements of absorbance were registered in the visible spectrum. The explored reaction of Mn(II) with 1-(2-pyridylazo)-2-naphthol and the new reaction with 2-(2-quinolinazo)-5-diethylaminophenol were used to verify the device's metrological parameters. Spectra obtained by means of the proposed photometer were compared to those for commercial photometers. A computer algorithm considering the difference in light-emitting intensity between diods was developed. The possibility of determination down to 1 mkg/ml metal ions in liquid samples was shown.
A method for copper(II) determination based on copper(II) ions interaction with the organic reagent picramine-ε, concentrating the formed complex on a solid-phase matrix and recording diffuse reflectance spectroscopy spectra by a portable combined LED miniphotometer was developed. Poly-ε-caproamide membranes were investigated as solid-phase matrixes. It was found that the diffuse reflectance coefficient of the studied membranes in the visible spectrum region does not depend on wavelength. So, the signal from membranes does not distort the results of the analysis. Factors controlling the process of sorption of the copper(II) complex with picramine-ε were studied. It was shown that the poly-ε-caproamide membranes are effective sorbents which provide the possibility of concentrating the analyte at a level higher than 105. The dependences of analytical signal on the acidity of the solution, the time of keeping the complex in the solution and the initial volume of the solution passed through the membrane were studied. Based on the obtained data, the optimal conditions of the analysis were found. Calibration dependence of the analytical signal on the concentration of copper(II) in model solutions was estimated. The method was tested for the determination of copper(II) ions in white wine. The method of additives was used for the analysis. It was found that the concentration of copper(II) ions in “Vagrus” wine is 0.0016 mkg/ml.
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