fang zhi xue xi chong bing yao wu de yan jiu . wei liang ti de bi se ce ding fa
Author(s): SHEN MAI-LING CHANG HUI-MIN TING KUANG-SHENG
Pages: 127-132
Year: 1957 Issue: 2
Journal: Acta Physiologica Sinica
Keyword: 比色测定法; 微量锑; 醋酸; 硫酸纳; 干涉; 毫升; 生物样品; 血吸虫病; 亚硫酸钠; 提取液;
Abstract: A procedure for colorimetric microdetermination of Sb in biological materials by means of rhodamine B and amyl acetate is established:To the sample add 3 ml of concen- trated H_2SO_4,and digest with concentrated HNO_3.Following the complete destruction of organic matter add 3 ml of 1% Na_2SO_3 and heat until fumes of SO_3 evolve,thus the Sb is reduced to trivalent.On cooling,add 4 ml of 6 N HCl and 2% Ce(SO_4)_2 to slight excess, so the Sb is oxidized to pentavalent.Dilute to 24 ml with H_2O.Extract the Sb with 5 ml of amyl acetate.After complete removal of the aqueous layer,add 9 ml of 2.5 N HCl and 1 ml of 0.2% rhodamine B and shake.If the aqueous layer becomes colorless or only faintly colored, add more rhodamine B.Then centrifuge and take the acetate phase for color measurement, using yellow-green filter.If the color is too intense that does not obey Beer-Lambert law, dilute the extract with amyl acetate previously shaken with 2.25 N HCI. The advantages of this procedure are:(a)high sensitivity;(b)no interference from iron or ceric sulfate;(c)color stable;(d)high extracting power of amyl acetate which is less volatile; (e)easily to be mastered and(f)high duplicability. The influences of amounts,concentrations and order of adding reagents are studied and discussed.
Pages: 127-132
Year: 1957 Issue: 2
Journal: Acta Physiologica Sinica
Keyword: 比色测定法; 微量锑; 醋酸; 硫酸纳; 干涉; 毫升; 生物样品; 血吸虫病; 亚硫酸钠; 提取液;
Abstract: A procedure for colorimetric microdetermination of Sb in biological materials by means of rhodamine B and amyl acetate is established:To the sample add 3 ml of concen- trated H_2SO_4,and digest with concentrated HNO_3.Following the complete destruction of organic matter add 3 ml of 1% Na_2SO_3 and heat until fumes of SO_3 evolve,thus the Sb is reduced to trivalent.On cooling,add 4 ml of 6 N HCl and 2% Ce(SO_4)_2 to slight excess, so the Sb is oxidized to pentavalent.Dilute to 24 ml with H_2O.Extract the Sb with 5 ml of amyl acetate.After complete removal of the aqueous layer,add 9 ml of 2.5 N HCl and 1 ml of 0.2% rhodamine B and shake.If the aqueous layer becomes colorless or only faintly colored, add more rhodamine B.Then centrifuge and take the acetate phase for color measurement, using yellow-green filter.If the color is too intense that does not obey Beer-Lambert law, dilute the extract with amyl acetate previously shaken with 2.25 N HCI. The advantages of this procedure are:(a)high sensitivity;(b)no interference from iron or ceric sulfate;(c)color stable;(d)high extracting power of amyl acetate which is less volatile; (e)easily to be mastered and(f)high duplicability. The influences of amounts,concentrations and order of adding reagents are studied and discussed.
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