how can i prepare water saturated butyl chloride?

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i want to prepare water saturated butyl chloride for assay determination of Hydrocortisone Acetate. the mobile phase: Butyl chloride : water saturated Butyl chloride : Tetrahydrofuran : Glacial acetic acd : Methanol (475:475: 60:30:35) . how can i prepare water saturated BC.
Put butyl chloride and water in the same flask, shake, and let stand overnight then pour off the butyl chloride.
-- Tom Jupille
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
Please maintain a consistent room temperature if you want reproducible results.

Rod
tom jupille wrote:
Put butyl chloride and water in the same flask, shake, and let stand overnight then pour off the butyl chloride.


In your answer, there is no proper direction for composition. Please tell me the composition of water and butyl chloride for water saturated butyl chloride.
There is no set saturation point as it is a moving target, which will vary with the temperature of the water. Tom's directions are quite appropriate.

If you want a reproducible answer then follow his instructions and weigh the amount of butyl chloride added to the known amount of water and after overnight equilibration, remove and weigh the butyl chloride that did not dissolve into the water. Of course, degas the water before adding the butyl chloride and measure the temperature of the saturated water for your records.

Good luck.

Rod
I just did a quick Google search for n-butyl chloride and water solubility.

http://macro.lsu.edu/HowTo/solvents/n-B ... loride.htm

Solubility in water 0.11% at 20°C

Solubility of water in n-butyl chloride 0.08% at 20°C

So obviously you need to exceed that concentration bearing in mind the previous very helpful comments.

10mls of water added to every 90mls of butyl chloride would allow more than enough to saturate the butyl chloride.

Regards

Ralph
Regards

Ralph
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