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Reductimetric Determination of Nitroso Compounds With Iron(II)

机译:铁(II)还原还原测定亚硝基化合物

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A simple accurate and convenient reductimetric titration method has been developed for the determination of two nitroso compounds namely: I -Nitroso 2 Napthol (α-Niraso β –Napthol) and 2-Nitraso 1-Napthol (β-Nitroso α- Napthol) using iron(II) as a reducing agent in a phosphoric acid medium. The method consists in titrating the solutions of these compounds against iron(II) in about 9 M (or above) phosphoric acid medium and in presence of a small amount of resorufin (RSF) which acts as a catalyst as well as redox indicator. The color transition of the indicator at the end- point (from red to bluish green) is sharp, reversible and no indicator correction need to be applied. The two nitroso compounds in the range 5 -20 mg have been determined with an accuracy of ± 0.06 %. The precision of the method is found by computing pooled standard deviation and 95% confidence limits. The two nitroso compounds are found to be reduced by iron(II) to their corresponding amino compounds each in a four electron reduction step. The indicator RSF is reduced to its bluish green semi quinone by iron(II) in one electron reduction step. The formal redox potentials of the two oxidant systems ( [nitroso compound]/[amino compound] couple) and the reductant system ( [ iron(III)] /[ iron(II)] couple ) and the transition potential of the indicator RSF have been measured in 9-12 M phosphoric acid medium. Based on these potentials data, the conditions needed in the titrations have been explained.
机译:已开发出一种简单,准确,方便的还原滴定法,用于测定两种亚硝基化合物:I-亚硝基2-萘(α-Nirasoβ-萘)和2-Nisoso 1-萘(β-亚硝基α-萘)。 (II)在磷酸介质中作为还原剂。该方法包括在约9M(或以上)的磷酸介质中,在少量的作为催化剂和氧化还原指示剂的试卤灵(RSF)存在下,滴定这些化合物对铁(II)的溶液。指标在端点处的颜色过渡(从红色到蓝绿色)清晰,可逆,无需进行指标校正。已测定5 -20 mg范围内的两种亚硝基化合物,准确度为±0.06%。该方法的精度可通过计算合并的标准偏差和95%的置信度来确定。发现两种亚硝基化合物在四电子还原步骤中被铁(II)还原为它们各自的氨基化合物。指示剂RSF在一个电子还原步骤中被铁(II)还原为蓝绿色半醌。两种氧化剂体系([亚硝基化合物] / [氨基化合物]对)和还原剂体系([铁(III)] / [铁(II)]对)的形式氧化还原电势和指示剂RSF的跃迁电势均具有在9-12 M磷酸介质中测量。基于这些电势数据,已经说明了滴定所需的条件。

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