kaviaari
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Registered: 21-12-2005
Location: Finland
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Mood: Going green
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Got my first good ground joint setup
I am so so so exited  My christmas came a little bit late, but that doesn't
really matter.
This is what I got:
Stainless steel buncher funnel
Ion exchange colony
A steam tube from rot.vap.
100 ml RB flask with side tube
20ml dropping funnel with adapter
Distillation bridge
Coil condenser
500ml pear-shaped RB flask
100ml RB flask
Allihn condenser
Reciever apparatus for distillation
2ml Syringe
And I am so so so over-excited now 
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bereal511
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Very nice, how much did it all cost and where did you procure it?
As an adolescent I aspired to lasting fame, I craved factual certainty, and I thirsted for a meaningful vision of human life -- so I became a
scientist. This is like becoming an archbishop so you can meet girls.
-- Matt Cartmill
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kaviaari
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Registered: 21-12-2005
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It was totally free for me. All this stuff was going to be recycled. Luckly my friend happened to save them. He kept most of his findings and gave me
what you see in picture. The stuff is quite rare like those 7mm joints. And the 7mm stuff is also made here in Finland.
I have been fooling around with them whole evening. Now I have finished the refluxing part of chloroacetone synthesis. I really hope that I would have
a fumehood, my eyes hurt quite a bit because of the acetone fumes 
And here is a picture of a distillation setup:
[Edited on 30-12-2006 by kaviaari]
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Organikum
resurrected
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Mood: frustrated
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Refluxing for chloroacetone? For monochloroacetone mostly low temperatures are asked for to avoid overchlorination I thought...
The hotplate looks to me like one of those with a bimetal-temperature switch. Those are big shit and caused me lots of problems because they provide
almost no temperature control at all, even with a water or oilbath the temperature fluctuates over a terrible wide range.
Nice glassware though.
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kaviaari
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Registered: 21-12-2005
Location: Finland
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Mood: Going green
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| Quote: | Originally posted by Organikum
Refluxing for chloroacetone? For monochloroacetone mostly low temperatures are asked for to avoid overchlorination I thought...
The hotplate looks to me like one of those with a bimetal-temperature switch. Those are big shit and caused me lots of problems because they provide
almost no temperature control at all, even with a water or oilbath the temperature fluctuates over a terrible wide range. |
| Quote: | Originally posted by Mendeleev
Chloroacetone [1]
Good method of preperation 150 ml acetone 50 ml water 12 g Cupric chloride 6 g lithium chloride. Reflux till reaction completes. Literature states 24
hours but the reaction has a half-life of about 24 minutes at 20°C (same article half of marker in 24 minutes, the marker being oxygen consumption in
a slightly different reaction), therefore 5 hours is probably sufficient at reflux.
After reacting, distill everything below 123°C. The still bottoms can be reprocessed to recover cuprous chloride and lithium chloride. Both can be
recovered by disolving with minimum water. The mix is easily converted to cupric chloride-lithium chloride by boiling with 20-35% hydrochloric acid.
Redistill slowly through a packed column to remove acetone. This leaves two fractions one distilling at 89C which is water and chloroacetone and the
second distilling at 121°C which is ?pure? chloroacetone. The second fraction may contain unsymetrical dichloroacetone I haven't had a sample
analysed. Calcium Chloride will crash the water-chloroacetone mix which tends to form a colloidal solution.
Chloroacetone must be stabalized with 1% calcium carbonate or 0.1% water if it is stored or it forms an explosive sludge. Distillation of a
water-chloroacetone mix at 89°C is the most efficient way of separating unsym-dichloroacetone from commercial products.
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in http://www.sciencemadness.org/talk/viewthread.php?tid=2713
It looked fine for me. Well I am just starting with organics so what looks ok to me might not be as it seems.
The hotplate .. yes. It is old, rusty and it smells very odd. I have been dreaming of a hotplate with magnetic stirrer but I am so mingy that I just
can't buy one.
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Ephoton
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Mood: trying to figure out why I need a dark room retreat when I live in a forest of wattle.
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depends on the route you use. becarefull when you wash your flask hehe. id be goen the aqua route i posted it looks like a good way and that is at
reflux for 5 hours very good yield. I would not be maken chlorinated ketones with a setup that has a reciver open to the air. Dont use water to wash
up what ever you do use another ketone.
[Edited on 31-12-2006 by Ephoton]
[Edited on 31-12-2006 by Ephoton]
e3500 console login: root
bash-2.05#
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