胺共存时次亚磷酸根和亚磷酸根耗铈(Ⅳ)总量的测定

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本项研究是有关含胺体系中次亚磷酸根和亚磷酸根耗铈(Ⅳ)总量的测定,以便迅速获得混合物中亚磷酸根浓度。根据不同酸度的实验结果发现,反应混合物酸度的增加不仅能有效地抑制胺氧化,而且还能强烈地提高Ce(Ⅳ)与H2PO2或HPO间的反应速度。此外,在同一酸度下,上述反应速度极大地随Ag(I)催化剂的加入量而变化。在酸度[H+]=10mol/L,5%Ag2SO42.5ml,水浴沸腾温度,硫酸饰(Ⅳ)铵微过量和反匝物总体积50ml的条件下,只要5分钟反应时间即可使次亚磷酸根和亚磷酸根定量地氧化为磷酸根而无胺氧化干扰,并且耗铈(Ⅳ)总量的测定误差小于1%。 This study is concerned with the determination of the total amount of phosphinite and phosphite cerium (IV) in amine-containing systems in order to quickly obtain the phosphite concentration in the mixture. According to the experimental results of different acidity, it is found that the increase of the acidity of the reaction mixture can not only effectively inhibit the amine oxidation, but also strongly enhance the reaction rate between Ce (Ⅳ) and H2PO2 or HPO. In addition, at the same acidity, the above reaction rate greatly varies with the amount of Ag (I) catalyst added. Under the conditions of acidity [H +] = 10mol / L, 5% Ag2SO42.5ml, boiling temperature of water bath, ammonium triflurate (Ⅳ) and the total volume of anti-turns, 50ml reaction time, hypophosphorous acid Root and phosphite were quantitatively oxidized to phosphate without amine oxidation interference, and the determination of total cerium (IV) consumption was less than 1%.
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