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Author: Subject: Garage Experiments With Trichloromethane.
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[*] posted on 27-1-2007 at 05:28


Today I made a few mililiters of CHCl3. It smells very good.



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[*] posted on 7-3-2007 at 18:44


Has anyone done a "one-pot" oxidation and haloform reaction straight from isopropanol? I realize that yields would go down a bit since the alcohol:hypochlorite molar ratio would have to be 1:4 instead of 1:3 when acetone is used in place of the alcohol and you end up with more water for the chloroform to dissolve in.

Any idea what kind of "home-made" stopper I can use for this stuff? I have brown glass, but only some rubber stoppers for them. Someone said earlier that it will attack cork, and I imagine it can dissolve most plastics, not to mention reacting with metals. I don't have any teflon other than the white tape, which I know is probably too porous, no?

[Edited on 8-3-2007 by GhostofUnintentionalChaos]
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[*] posted on 8-3-2007 at 00:20


I don't think chloroform attacks cork. If corks get attacked, then only from the bleach and not from the chloroform.

It should work with isopropanol and adjusted ratios.
And you should of course always distill the chloroform out of the mix to get good yields, no matter which process you use.




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[*] posted on 13-4-2007 at 08:14


Hm, I just noticed that the wikipedia article for chloroform claims that it can be produced with bleach and MEK. Is this even possible, or just wrong?
"Sodium hypochlorite solution (bleach) and methyl ethyl ketone (nail-varnish remover) produces chloroform."
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[*] posted on 13-4-2007 at 08:59


That should work just fine. The resulting reaction products should be sodium propionate, sodium hydroxide, and chloroform. Look up "haloform reaction" which gives you the criteria for the reaction to occur.



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[*] posted on 13-4-2007 at 11:11


The haloform reaction is a general one for any compound having a methyl group alpha to a carbonyl.

Acetaldehyde, acetone, MEK, MIBK. And so on.
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[*] posted on 17-4-2007 at 23:34


Just how well does PTFE stand up to chloroform? I have recently acquired some heavy duty gas line PTFE tape (can handle Natural Gas under 100PSIG, propane, butane, naptha, benzene, kerosene, gasoline, and petroleum oils) and have a glass bottle to hold @250ml of CHCl3. It looks just like a miniature wine bottle (green glass) and has a standard soda bottle screwtop. I took out the little insert in the cap, gave it a triple layer of the tape, crushed the insert in a vice between wood blocks to bond the tape to itself, and jammed it back into the plastic screwtop. There is a very obvious dark yellow line where the glass rim compresses the light yellow PTFE tap after being screwed onto the bottle firmly. What kind of shelf life can I expect before I have to make a new insert, or is PTFE relatively immune to corossion by CHCl3? I have brown screwtop glass bottles as well, but without PTFE sheeting, I can't make a cap insert.



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[*] posted on 18-4-2007 at 00:58


So long as there isn't a hairline leak it should keep well. Even most halogenated hydrocarbons have little to no effect on PTFE


http://www.kimble-kontes.com/pdfs/solvent_compatibility_2.pd...
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[*] posted on 18-4-2007 at 12:50


Try mixing your trichloromethane with silver nitrate and see if you get an ungodly explosive. CHCl3 + 3 AgNO3 -> CH(NO3)3 + 3AgCl The silver chloride is insoluble and will sink to the bottom.
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[*] posted on 18-4-2007 at 13:30


The chlorinated brake cleaner we have locally contains tetrachloroethane. Can this be used in the same way as trichloroethane or does the extra chlorine render it useless.
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sad.gif posted on 2-5-2007 at 21:20
Perk -> CHCl3


I have never seen that mentioned. But it may be possible as C2Cl4 + 2 Cl2 <--> 2 CCl4 (this reaction is reversible). Therefore, maybe hydrochlorination of tetrachloroethylene under the right conditions may yeild a 1:1 mix of carbon tet and chloroform. Although this would be a vapor phase reaction and probably a tricky one to control at that as industrially neither carbon tet or chloroform are made from ethylene. Although CCl4 is a byproduct from the manufacture of tetrachloroethylene from 1,2 Dichloroethane.


However from trichloroethylene (electronics cleaner and some degreasers, although it is being phased out) one can make chloroform in 2 steps:

First trichloroethylene is oxidized and rearranged by HClO forming chloral. Chloral can then enter the haloform reaction in the presence of NaOH yielding chloroform. It is possible that bleach and trichloroethylene will yeild chloroform and sodium formate, although I have never seen both of these reactions run together.
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[*] posted on 28-8-2007 at 15:59


Tetrachloroethane is a halogenated solvent, same as chloroform, trichloroethane, etc. However, if I remember correctly it is much more hazardous to your health. It's classified as very toxic.
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[*] posted on 24-9-2007 at 12:20


[Edited on 24-9-2007 by Slimz]



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[*] posted on 27-9-2007 at 14:50
Cloroform


Ok so following a procedure ifound here, i tried to make this.

I used the same 6% bleach and 100% acetone (denatured)

500ml 6% bleach in a beaker
added 20ml of acetone over about 5 minutes time
stirred for about 10 min
cooled during process in a cool water bath (kept cool with pieces of ice periodicaly)

let stand for about 10-15 min (sorry for the approx times)

when it was all over i had a milky wight to and about 7ml of something on the bottom

i sucked it out with an eyedropper after removing much of the top liquid

the smell of this substance is similar to acetone but sweeter and warmer... was i successful??

[Edited on 27-9-2007 by Slimz]




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[*] posted on 27-9-2007 at 14:53


OK slimz don't sniff it because it obviously killed the brain cells that you use to spell words correctly.:P



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[*] posted on 27-9-2007 at 14:56


Yes odds are you were successful.

This should have been a clear oil on the bottom.

This process I have done several times successfully, you can probably get away with this in a simpler manner by adding the acetone all at once and not worrying too much about cooling the reaction.

-ssdd




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[*] posted on 27-9-2007 at 15:03


You knew there was a thread on this already, and posted a new thread on the same topic? The other one is perfectly fine, and this is being merged with it.



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[*] posted on 27-9-2007 at 15:25


sorry about the thread.. different forums have different expectations... ill know better next time\



i just did it again with 1000ml bleach and about 40ml acetone (added all at once) it bubbled like crazy .. i added a little more acetone after a while (just to see if i could continue the reaction) about 20ml .. its sitting outside now, but i have not seen separation yet...

No problem. Unlike some forums, we don't mind old threads being resurected, it helps keep valuable information all in one spot -Davster




[Edited on 27-9-2007 by The_Davster]




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[*] posted on 27-9-2007 at 15:39


Quote:
Originally posted by bob000555
Try mixing your trichloromethane with silver nitrate and see if you get an ungodly explosive. CHCl3 + 3 AgNO3 -> CH(NO3)3 + 3AgCl The silver chloride is insoluble and will sink to the bottom.


Ungodly tell me more?

How safe is this what sort of reaction conditons are needed, time, temp, mixing, chloroform in excess, gravity feed filtration of AgCl, washing of product?

The product CH(NO3)3, what are the propities of this, shock sensitve, cap sensitive etc. Storage criteria; dissolved in solvent, safe handling advice, safe amouunts for first time reaction?

Uses?
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[*] posted on 27-9-2007 at 15:53


Do a search for trinitromethane (also called nitroform). And you should get plenty of information.
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[*] posted on 27-9-2007 at 15:54


ok this stuff is still not separating... but its still warm.. the last reaction was smaller, do you think this one could just be taking a long time, or do you think its botched??



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[*] posted on 27-9-2007 at 16:01


You may have added too much acetone, usually 20-30 ml is enough for 900ml to react to near completion. I am not sure if this would have any effect.

** Found it chloroform is soluble in acetone so adding too much acetone would cause the small amount of product to dissolve.

Try tipping the reaction vessel to the side a bit to see if the oil sloshes over to the corner, sometimes in large quantities this is needed.

-ssdd




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[*] posted on 27-9-2007 at 16:48


no i botched it... too much acetone... i winder if i could add mure bleach to react out the rest of the acetone... ???



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[*] posted on 27-9-2007 at 17:14


well added bleach and im getting product now... that was definitely an interesting experiment...



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[*] posted on 27-9-2007 at 18:04


Quote:
Originally posted by stygian
Do a search for trinitromethane (also called nitroform). And you should get plenty of information.


Chloroform and silver nitrate dosent look like it will make nitroform

Was that fact or guess work
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