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[交流] 十六烷基氯化吡啶的分析方法

请教十六烷基氯化吡啶的分析方法,谢谢。
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lwl913(金币+1,VIP+0):呵呵,谢谢,不过感觉很乱,比如用高效液相色谱测,具体的条件有没有?
Cetylpyridinium Chloride

C21H38ClN · H2O     358.00

Pyridinium, 1-hexadecyl-, chloride, monohydrate.
1-Hexadecylpyridinium chloride monohydrate   [6004-24-6].

Anhydrous 339.99   [123-03-5].
» Cetylpyridinium Chloride contains not less than 99.0 percent and not more than 102.0 percent of C21H38ClN, calculated on the anhydrous basis.
Packaging and storage— Preserve in well-closed containers.
USP Reference standards 11 — USP Cetylpyridinium Chloride RS.
Identification—
A: Infrared Absorption 197K .
B: Ultraviolet Absorption 197U —
Solution: 40 µg per mL.
Medium: water.
C: Dissolve 100 mg in 50 mL of water: a 10-mL portion of the solution responds to the tests for Chloride 191 , except that a turbidity is produced, rather than a curdy white precipitate, when the silver nitrate TS is added.
Melting range, Class I 741 : between 80 and 84, the preliminary drying treatment being omitted.
Acidity— Dissolve 500 mg, accurately weighed, in 50 mL of water, add phenolphthalein TS, and titrate with 0.020 N sodium hydroxide: not more than 2.5 mL is required for neutralization.
Water, Method I 921 : between 4.5% and 5.5%.
Residue on ignition 281 : not more than 0.2%, calculated on the anhydrous basis.
Heavy metals, Method II 231 : 0.002%.
Pyridine— Dissolve 1 g in 10 mL of sodium hydroxide solution (1 in 10) without heating: the odor of pyridine is not immediately perceptible.
Organic volatile impurities, Method V 467 : meets the requirements.
Residual solvents 467 : meets the requirements.
(Official January 1, 2007)
Assay— Transfer about 200 mg of Cetylpyridinium Chloride, accurately weighed, to a glass-stoppered, 250-mL graduated cylinder containing 75 mL of water. Add 10 mL of chloroform, 0.4 mL of bromophenol blue solution (1 in 2000), and 5 mL of a freshly prepared solution of sodium bicarbonate (4.2 in 1000), and titrate with 0.02 M sodium tetraphenylboron VS until the blue color disappears from the chloroform layer. Add the last portions of the sodium tetraphenylboron solution dropwise, agitating vigorously after each addition. Each mL of 0.02 M sodium tetraphenylboron is equivalent to 6.800 mg of C21H38ClN.
平平淡淡才是真
2楼2008-12-17 15:38:28
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lwl913

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呵呵,谢谢,不过感觉很乱,比如用高效液相色谱测,具体的条件有没有?
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3楼2008-12-18 10:56:09
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