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Sequential spectrophotometric determination of methanol and iron in vinegar by a flow injection-pervaporation method

机译:流动注射-全蒸发光度法分光光度法测定食醋中的甲醇和铁

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摘要

An easily automatable sequential flow-injection-pervaporation method is proposed for the photometric determination of methanol and iron in vinegar. The method is based on separation of the methanol from the sample matrix by pervaporation followed by its oxidation to formaldehyde with permanganate, decolouration of the latter with S_2O_5~(2-), and subsequent reaction of formaldehyde with p-rosaniline to yield a violet reaction product with maximum absorption at 567 nm. Iron is determined by an existing method based on reaction with thiocyanate in acidic medium and monitoring at 508 nm. After optimisation by either the univariate or multivariate approaches, as required, the linear range was established for methanol (4-1000 mg L~(-1)) and iron (0.18-20 mg L~(-1)). The proposed method was then compared with reference methods for methanol and iron in terms of repeatability (2.452 mg L~(-1) and 0.245 mg L~(-1), respectively), reproducibility (4.435 mg L~(-1) and 0.356 mg L~(-1), respectively), detection limit (LOD = 82 and 0.234 mg L~(-1), respectively), and traceability. The throughput was nine samples per hour.
机译:提出了一种易于自动化的顺序流动注射-全蒸发方法,用于光度法测定醋中的甲醇和铁。该方法基于以下方法:通过蒸发将样品基质中的甲醇分离出来,然后用高锰酸盐将其氧化为甲醛,用S_2O_5〜(2-)对其进行脱色,然后甲醛与对罗萨林碱反应生成紫罗兰色反应。产品在567 nm处具有最大吸收。铁是根据现有方法在酸性介质中与硫氰酸盐反应并在508 nm处监测而确定的。通过单变量或多变量方法优化后,根据需要,确定了甲醇(4-1000 mg L〜(-1))和铁(0.18-20 mg L〜(-1))的线性范围。然后将拟议的方法与参考方法的甲醇和铁方法的重复性(分别为2.452 mg L〜(-1)和0.245 mg L〜(-1)),重现性(4.435 mg L〜(-1)和分别为0.356 mg L〜(-1)0.356 mg L〜(-1),检出限(LOD分别为82和0.234 mg L〜(-1))和可追溯性。吞吐量为每小时9个样本。

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