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Titrimetric and Spectrophotometric Determination of Some Thiadiazole Derivatives by Using Amplification Reactions

机译:用扩增反应滴定和分光光度法测定一些噻二唑衍生物的测定

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The principle of using amplification reactions of iodine was employed in this paper to estimate the thiadiazole derivatives on basis of their reactions with iodine I chloroform, removal of the excess iodine and determination of the resulting iodide, after oxidation to iodate. The overall reaction gave an amplification of the iodide that is (12) times larger for the compounds: 2-amino-5-mercapto-1,3,4-thiadiazole (I); 2,5-dimercapto-1,3,4-thiadiaole (II) and 2,5-diamino-1,3,4-thiadiazole (III) and (36) times for 2,5-dihydrazino-1,3,4-thiadiazole (IV) and (6) times for 5-mercapto-2[(3[5’-nitro-2-’furyl]·methylene)amino]-1,3,4-thiadiazole (V) and 5-mercapto-2[(3[5’-nitro-2-’furyl]-prop-2-enylidene)amino]-1,3,4-thiadiazole (VI). By titration, 1-mL of standard thiosulfate solution was found equivalent to 0.108 mg of (I); 0.126 mg of (II), 0.16 mg of (III), 0.041 mg of (IV), 0.40 mg of (V) and 0.435 mg of (VI). Using the spectrophotometric detection for the amplification reaction gave high absorbance values at 605 nm for the blue starch-iodine complex. Beer’s law was obeyed up to 4.0 ppm for compounds (I and II); 6.0 ppm for compounds (III, IV and VI) and 5.0 ppm for compound (V). The mechanism of the reactions was proposed and the analytical parameters were evaluated for both methods. The method was applied for synthetic samples of industrial importance. The recovery was comparable while the sensitivity and detection limits were better for the spectrophotometric detection.
机译:本文采用碘的扩增反应的原理,以根据碘I氯仿,除去过量的碘和测定所得碘化物的反应来估计噻二唑衍生物,并在氧化到碘酸碘后。总反应对化合物的碘化物放大,即化合物的(12)倍:2-氨基-5-巯基-1,3,4-噻二唑(I); 2,5-二羟基-1,3,4-噻二唑(III)和2,5-二羟基-1,3,4的2,5-二硫基-1,3,4-噻二唑(III)和(36)次 - 5-巯基-2 [(3 [5'-硝基-2-'糠]·亚甲基)氨基] -1,3,4-噻二唑(V)和5-巯基(3)次(3)次。 -2 [(3 [5'-硝基-2-'糠] -2-烯基)氨基] -1,3,4-噻二唑(VI)。通过滴定,发现1-mL标准硫代硫酸盐溶液相当于0.108mg(i); 0.126mg(II),0.16mg(III),0.041mg(IV),0.40mg(V)和0.435mg(VI)。使用分光光度检测进行扩增反应,对蓝淀粉 - 碘配合物进行605nm的高吸光度值。啤酒的法律适合高达4.0 ppm的化合物(I和II);用于化合物(III,IV和VI)和5.0ppm的化合物(V)的6.0ppm。提出了反应的机制,并对两种方法评估分析参数。该方法适用于工业重要性的合成样本。恢复可比较,而灵敏度和检测限优于分光光度检测。

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