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北京石油化工学院2026年研究生招生接收调剂公告
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abacus988

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[交流] 【求助】PVP K-30的检测方法。

如何检测PVP,k-30的含量呢,要求简单点,仪器检测在小公司很难执行。
最好有滴定分析。谢谢各位达人。
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xiaozhu629

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Mike


clkk216(金币+1,VIP+0):3Q~~! 辛苦了~~!
ASSAY for Povidone K30 from BP
  
Place 100.0 mg of the substance to be examined (m mg) in a combustion flask, add  5 g of a mixture of 1 g of copper sulphate R, 1 g of titanium dioxide R and 33 g of  dipotassium sulphate R, and 3 glass beads. Wash any adhering particles from the  neck into the flask with a small quantity of water R. Add 7 ml of sulphuric acid R,  allowing it to run down the sides of the flask, and mix the contents by rotation. Close  the mouth of the flask loosely, for example by means of a glass bulb with a short  stem, to avoid excessive loss of sulphuric acid. Heat gradually at first, then increase  the temperature until there is vigorous boiling with condensation of sulphuric acid in  the neck of the flask; precautions are to be taken to prevent the upper part of the  flask from becoming overheated. Continue the heating for 45 min. Cool, dissolve the  solid material by cautiously adding to the mixture 70 ml of water R, cool again and  place in a steam-distillation apparatus. Add 30 ml of strong sodium hydroxide  solution R through the funnel, rinse cautiously the funnel with 10 ml of water R and  distil immediately by passing steam through the mixture. Collect about 80-100 ml of  distillate in a mixture of 30 ml of a 40 g/l solution of boric acid R and 3 drops of  bromocresol green-methyl red solution R and enough water R to cover the tip of the  condenser. Towards the end of the distillation lower the receiver so that the tip of the  condenser is above the surface of the acid solution and rinse the end part of the  condenser with a small quantity of water R. Titrate the distillate with 0.025 M  sulphuric acid until the colour of the solution changes from green through pale  greyish-blue to pale greyish-red-purple (n1 ml of 0.025 M sulphuric acid).
  
Repeat the test using about 100.0 mg of glucose R in place of the substance to be  examined (n2 ml of 0.025 M sulphuric acid).
  

是凯式定氮法,主要是玻璃仪器以及滴定,应该比较简单,另外也可参考ChP2005 921页 《聚维酮 K30》
2楼2008-12-25 12:19:21
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abacus988

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谢谢了.
3楼2008-12-25 16:44:42
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