Abstract

A new and sensitive preconcentration procedure was developed for the determination of trace amount of Mn(II) in environmental water samples. Amberlite XAD-4 resin was functionalized with N,N-bis(salicylidene)cyclohexanediamine (SCHD) to preconcentrate and separate Mn(II) at the trace level concentrations. Mn(II) ion in environmental water samples was determined by the formaldoxime spectrophotometric method. The influences of analytical parameters including pH and volume of sample, type and concentration of elution solution, flow rate of sample and elution solution, etc. were investigated on the recoveries of Mn(II) ion. The adsorption was achieved quantitatively for Mn(II) on XAD-4-SCHD resin at the pH range of 3–10 and 3 mL min^–1 sample flow rate. Elution was performed with 0.5 mol L^–1 nitric acid solution. Under the optimized conditions, calibration curve was found to be linear in the concentration range of 0.1–5 mg L^–1 with a limit of detection of 0.65 μg L^–1. The effect of foreign ions on the perconcentration and determination of Mn(II) was studied and no adversely affecting ion was observed even at high ionic media. The recovery value was above 90%, with an enrichment factor of 100. The per cent relative standard deviation (%) value was found to be 1.8 for twenty repetitive measurements containing 1 mg L^–1 of Mn(II). Sorption capacity of the Mn(II) ion on the XAD-4-SCHD resin was found to be 29.217 μg. The accuracy of the presented preconcentration and determination method was checked by the analysis of TMDA-70.2 Ontario lake Water certified reference material and synthetic water sample. The method was applied for the analyses of tap water and industrial wastewater samples for Mn(II). Almost the similar results were observed for the Mn(II) determination in different environmental water samples using both the proposed and ICP-MS methods.

中文翻译：

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N，N-双（水杨基）环己二胺官能化Amberlite XAD-4树脂上环境水样品中Mn（II）的预浓缩和分光光度评估

摘要

建立了一种新的灵敏的预浓缩程序，用于测定环境水样品中的痕量Mn（II）。将Amberlite XAD-4树脂用N，N-双（水杨基）环己二胺（SCHD）官能化，以痕量浓度预浓缩和分离Mn（II）。用福尔多肟分光光度法测定环境水样中的Mn（II）离子。考察了pH，样品体积，洗脱液的种类和浓度，样品和洗脱液的流速等分析参数对Mn（II）离子回收率的影响。在3–10和3 mL min ^–1的pH范围内，XAD-4-SCHD树脂上的Mn（II）定量吸附样品流速。用0.5 mol L ^–1硝酸溶液进行洗脱。在最佳条件下，发现浓度范围为0.1–5 mg L ^–1时校准曲线呈线性，检出限为0.65μgL ^–1。研究了外来离子对Mn（II）的浓度和测定的影响，即使在高离子介质下也未观察到不利的离子影响。回收率值超过90％，富集系数为100。发现20次包含1 mg L ^–1的重复测量，相对标准偏差（％）的百分比值为1.8。Mn（II）。发现Mn（II）离子在XAD-4-SCHD树脂上的吸附容量为29.217μg。通过分析TMDA-70.2安大略湖水认证标准物质和合成水样品，验证了所提出的预浓缩和测定方法的准确性。该方法用于自来水和工业废水中的Mn（II）样品分析。使用提议的方法和ICP-MS方法在不同环境水样中测定Mn（II）几乎观察到了相似的结果。