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Camroc37
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Mood: Must...Nitrate...EVERYTHING!
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Quote: Originally posted by j_sum1  | Well, you both did better than my first attempt. I reasoned that the bleach I have available is a bit lower in concentration but I had another
hypochlorite source that would work as well. So, being careful with my stoichiometry and the temperature and exothermic nature of the reaction I
proceeded. I was hoping to make 100mL of CHCl3 in one hit.
All I really got was an ugly slurry of chloroform and Ca(OH)2 that sunk to the bottom of my containers. For the record, calcium hypochlorite is not
an acceptable substitute. And it is really easy to think things through very thoroughly and overlook the obvious. |
I got less than 1ml on my first go...
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JJay
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| Quote: Originally posted by gdflp | | That sounds an awful lot like water, I would guess that you used insufficient drying agent. Cloudy distillates such as that typically clear after
sitting for a day or two, so if this happens I would dry and redistill. |
That is exactly what I was thinking... I used quite a bit of drying agent, but it was just tech grade CaCl2 without any special treatment, and I only
let it dry for about 20 minutes.
I let it stand overnight on CaCl2, and now I am going to distill again. If that doesn't work, I'll break out the 3A molecular sieves.
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JJay
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So far, the run has been crystal clear from the beginning.
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JJay
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The final yield was 136.7 mL of chloroform from 230.0 mL of acetone, a yield of 54.00%. The purity is probably very good, though the yield was pretty
crappy. I stabilized it with 1% ethanol and stored it in an amber glass bottle.
I'm not sure why the yield was so bad, but I definitely noticed a loss of product each time it was washed, and there was also a loss on each
distillation.
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Dr.Bob
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A yield of 54% for that prep sounds pretty good to me for such a reaction. You did likely loose some chloroform and acetone on each wash. And
distillations lose some each time, it is nearly inevitable, unless you have great equipment and perfect technique.
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