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[求助] 0.1 N高氯酸与 0.1 N高氯酸in醋酸一样吗？

请问各位高手
USP36里面有用
0.1 N perchloric acid VS滴定的实验
这里的0.1 N perchloric acid VS是怎么配的？
这个0.1 N perchloric acid VS和下面这个是一个东西吗？
Perchloric acid ( 0.1 N高氯酸在醋酸标准液 )
in anhydrous acetic acid, for titrations in non-aqueous media c(HClO4) = 0.1 mol/l (0.1 N) TitriPUR®

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1楼 2013-06-05 13:57:24

已阅回复此楼关注TA 给TA发消息送TA红花 TA的回帖

yugijiang

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【答案】应助回帖

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感谢参与，应助指数 +1
climbnail: 金币+5, 谢谢！但等进一步告诉我这个资料的出处吗？ 2013-06-05 15:21:54

Perchloric Acid, Tenth-Normal (0.1 N) in Glacial Acetic Acid
HClO4, 100.46
10.05 g in 1000 mL
[NOTE—Where called for in the tests and assays, this volumetric solution is specified as “0.1 N perchloric acid.” Thus, where 0.1 N or other strength of this volumetric solution is specified, the solution in glacial acetic acid is to be used, unless the words “in dioxane” are stated. [See also Perchloric Acid, Tenth-Normal (0.1 N) in Dioxane.] ]
Mix 8.5 mL of perchloric acid with 500 mL of glacial acetic acid and 21 mL of acetic anhydride, cool, and add glacial acetic acid to make 1000 mL. Alternatively, the solution may be prepared as follows. Mix 11 mL of 60 percent perchloric acid with 500 mL of glacial acetic acid and 30 mL of acetic anhydride, cool, and add glacial acetic acid to make 1000 mL.
Allow the prepared solution to stand for 1 day for the excess acetic anhydride to be combined, and determine the water content by Method I (see Water Determination 921), except to use a test specimen of about 5 g of the 0.1 N perchloric acid that is expected to contain approximately 1 mg of water and the Reagent (see Reagent under Method Ia in Water Determination 921) diluted such that 1 mL is equivalent to about 1 to 2 mg of water. If the water content exceeds 0.5%, add more acetic anhydride. If the solution contains no titratable water, add sufficient water to obtain a content of between 0.02% and 0.5% of water. Allow the solution to stand for 1 day, and again titrate the water content. The solution so obtained contains between 0.02% and 0.5% of water, indicating freedom from acetic anhydride.
Standardize the solution as follows.
Accurately weigh about 700 mg of potassium biphthalate, previously crushed lightly and dried at 120 for 2 hours, and dissolve it in 50 mL of glacial acetic acid in a 250-mL flask. Add 2 drops of crystal violet TS, and titrate with the perchloric acid solution until the violet color changes to blue-green. Deduct the volume of the perchloric acid consumed by 50 mL of the glacial acetic acid. Each 20.423 mg of potassium biphthalate is equivalent to 1 mL of 0.1 N perchloric acid.