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liuxuanyan

金虫 (小有名气)

[求助] 怎么除去环己烷中的芳烃

做紫外时需要环己烷作溶剂,我们实验室只有分析纯的,通过紫外扫描发现在250nm左右有吸收,请问在怎么除去环己烷中的芳烃,消除此段吸收?

   我用硫酸洗过后,吸收有减弱,但是再经过蒸馏,无水硫酸钠干燥后,在300-260nm间出现了强吸收,请问这是为什么??

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jianmei97

捐助贵宾 (著名写手)


liuxuanyan(金币+1):谢谢你,我去试试!
Cyclohexane [110-82-71 M 84.2, f 6.6O, b 80.7O, d24 0.77410, n 1.42623, n25 1.42354.
    Commonly, washed with conc H2SO4 until the washings are colourless, followed by water, aq Na2C03 or 5%
NaOH, and again water until neutral. It is next dried with P2O5, Linde type 4A molecular sieves, CaC12, or
MgS04 then Na and distd. Cyclohexane has been refluxed with, and distd from Na, CaH2, LiAl& (which also
removes peroxides), sodiudpotassium alloy, or P2O5. Traces of *benzene can be removed by passage through
a column of silica gel that has been freshly heated: this gives material suitable for ultraviolet and infrared
spectroscopy. If there is much *benzene in the cyclohexane, most of it can be removed by a preliminary
treatment with nitrating acid (a cold mixture of 3OmL conc HNO3 and 70mL of conc H2SO4) which converts
*benzene into nitrobenzene.
The impure cyclohexane and the nitrating acid are placed in an ice bath and stirred
vigorously for 15min, after which the mixture is allowed to warm to 25O during lh. The cyclohexane is
decanted, washed several times with 25% NaOH, then water dried with CaC12, and distd from sodium.
Carbonyl-containing impurities can be removed as described for chloroform. Other purification procedures
include passage through columns of activated alumina and repeated crystn by partial freezing. Small quantities
may be purified by chromatography on a Dowex 710-Chromosorb W gas-liquid chromatographic column.
Rapid purification: Distil, discarding the forerun. Stand distillate over Grade I alumina (5% w/v) or 4A
molecular sieves.

[ Last edited by jianmei97 on 2007-6-13 at 12:24 ]
4楼2007-06-13 12:23:34
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abcdelm

木虫 (著名写手)

月落之后,不说爱你*abcdelm


liuxuanyan(金币+1):谢谢光临!
暂时没有想到环己烷中的芳烃的方法,不过想提醒一句,不一定非得去除。你要做的物质的最大吸收波长在250nm吗?如果历此较远,是不是可以不考虑。
另在300-260nm间出现强吸收有可能还是芳烃衍生物的吸收,比较特征。
是不是可以用溶剂法去除环己烷中的芳烃,你考虑一下。其实就多花些钱买个较纯的吗
我的生命中走过许多女人, 她们来了, 又走了; 你要知道, 你不是第一个, 也不会是最后一个.....
2楼2007-06-07 20:18:32
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liuxuanyan

金虫 (小有名气)

谢谢!
买较纯的,老板舍不得和花钱啊。
我做的是吡啶,用环己烷作溶剂。吡啶最大吸收波长是251nm,所以想除去环己烷中芳烃的干扰。
3楼2007-06-08 22:47:29
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