치오씨안 錯化合物에 關한 硏究 = STUDY ON THE THIOCYANCOMPLEX COMPOUNDS
저자
崔宗仁 (成均館大學校 藥學大學 藥學科)
발행기관
학술지명
권호사항
발행연도
1970
작성언어
Korean
KDC
518.000
자료형태
학술저널
수록면
67-85(19쪽)
제공처
1. Study on the stability of ammonium cobalt thiocyanate solution and formation of perthiocyanuric acid;
The stability of cobaltous thiocyanate complex has been determined at various concentrations of mineral acids, and the rate of decomposition of this complex ion in the presence of acids as the time passes has also been studied. In this experiment, enough amount of ammonium thiocyanate solution was used so that dissociation of the complex by the shortage of thiocyanate ion can be neglected. The stability of the complex was calculated on the bases of spectrophotometric extinction measurements.
It was found that the complex was very stable in the presence of sulfuric acid, fairly stable in hydrochloric acid and unstable in nitric acid. Therefore it can be said that in the case of cobalt analysis by means of thiocyanate, excess amount of sulfuric acid does not cause any interferance and trouble and the color of the cobaltous thiocyanate ion is intensified. It is possible to determine the absorbance directly without removing the excess amount of sulfuric acid.
The effect of the excess amount of sulfuric acid on the absorbance is shown by figure 2.
An excess amount of nitric acid interferes very much with the formation of the cobaltous thiocyanate complex ion, but an excess amount of hydrochloric acid interferes only a little.
In a conclusion, attention should be paid to the fact that the color of cobaltous thiocyanate ion is not only intensified by the excess amount of sulfuric acid but also the color intensy is almost proportional to the amounts of sulfuric acid present.
It is considered that the stability of cobaltous thiocyanate ion is increased in the presence of the excess amounts of sulfuric acid.
2. The effect on the R.f. value by the number of thiocyanate radical in vaious thiocyanate ammine chromium complex salts;
Several thiocyanate ammine chromium complex salts are prapared by the known methods and the R.f. value of these complex salts are determined by four deveropers which were used in the paper chromatographical work of cobalt complex salts by Yamamoto in 1954. It was found that the R.f. value is increased with the number of thiocyanate radical by the descending development using developer A.
The reason of this curious results can be explained that the thiocyanate radical in the complex ion is more active for the organic solvent than ammine radical. Shifting of electrons to the central metal and charge of the complex ion can also effect to the R.f. value but much questions are remained for the explanation of the above curious phenomenon.
Separation of mixed samples is also studied for various mixtures of above complex salts. In the case of the mixture of hexammine and diammine complex salts, the clear separation is possible but in almost all other mixed samples, the results are not clear. Therefore it can be said that the results of this work can only be used in the qualitative analysis of the individual complex salts, except the mixed sample of hexammine and diammine complex salt.
3. Preparation of Potassium hexathiocyanato chromate;
Several preparation processes of this compound have been reported and in these processes KCNS and potassium chromium alum are used as the starting materials.
In this report, this compound is made from chloropentammine chromium chloride. The chloride 3g is suspended in a solution of KCNS 24g, glacial acetic acid 24ml and water 48ml.
The mixture is heated with stiring until it almost boils and boiled until it is completely dissolved. After cooling, the deposited orange-yellow thiocyanato pentammine chromium thiocyanate is filtered off. To the filtrate(65ml), 50g of KCNS is added and the mixture is warmed until a clear solution is obtained.
After cooling potassium hexathiocyanato chromate is crystallized as very beautiful red-violet crystals, the yield is 1.2g-1.3g.
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