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Lithium
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[*] posted on 2-3-2012 at 19:24
What is this?


hello

1 to 2 months ago i attempted to make chloroform with calcium hypochlorite, but i could not recover any as there was too much calcium hydroxide ppt, so i poured in excess hypochlorite and poured that into a large porcelain bowl and blew through a tube into the 4 or 5 litres of solution because i read somewhere that carbon dioxide destroys hypochlorite, turning it into Cl2O. after a few days of me blowing into the solution on and off, it stopped precipitating calcium hydroxide/ carbonate, so i left it till present day. it occasionally bubbled feebly, and the gas flamed when lit with a match. fast forward to today and i thought i might have a look at it. there was a little purple stuff around the rim of the dish. i blew into the solution and it caused the ppt to rise to the surface. the ppt is now a strong purple colour, and i have no idea what it is. the sol. no longer smells of chlorine

is this substance harmful?

does any one no what this is, i am starting to get a bit worried:(

Li

[Edited on 3-3-2012 by Lithium]
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ThatchemistKid
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[*] posted on 2-3-2012 at 19:29


Could you describe this in a bit more detail how much acetone or ketone did you use? I am thinking that what ignited was probably a mixture of acetone and chloroform (chloroform is not flammable but will burn if mixed with another flammable substance, also the by-products of burning chloroform are quite nasty.) What did your reaction mixture smell like? Did you cool the reaction flask in ice prior to mixing of the reactants?
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[*] posted on 2-3-2012 at 20:10


I think the ignited gas is acetone as well, as there are no other explanations (Cl2 or Cl2O is not flammable; they're oxidizers) I suggest you to be careful with it burning, as chloroform reacts with oxygen under sunlight or when heated to a high temperature, like the fire to phosgene, which is a cumulative poison gas that will kill you in about few to few tens of ppms! Do not burn that again. Also, you can just filter out the excess Ca(ClO)2 and Ca(OH)2 with a paper towel and a funnel, you don't need to blow CO2 in. As for the purple precipate, that might be some substance formed by HOCl, the hydrated form of Cl2O and a very reactive oxidizer. Keep this purple stuff and do some tests on it.

Edit: The feeble bubbling is caused by: 2HOCl====>2HCl+O2, both which escapes as a gas or HCl+HOCl<=====>Cl2+H2O, in which the Cl escapes as a gas.

[Edited on 3-3-2012 by weiming1998]
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Lithium
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[*] posted on 2-3-2012 at 21:39


yes, i understand chloroform oxidises to phosgene, which is exactly why i am worried.

i added 220g 70%Ca(ClO)2 and 2.5L of water in a 3L container and waited until most had dissolved. i then added, drip by drip in a bucket of cold water, 40g of acetone. this produced a layer of chloroform, but as the excess hypochlorite dissolved, it went away. it bubbled alot. i filtered the sol. and added another 220g hypochlorite and 20ml acetone, in an icebath. the ppt smelled strongly of CHCl3. i left it for a day, gave up and poured it into the bowl with a few more litres of water, blew into it heaps, and that's it!:D

i so don't want to filter 5L of solution, my largest funnel holds 100ml:(

do you think the purple ppt is some derivative of HOCl?

Li

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[*] posted on 2-3-2012 at 22:02


dont blow into chloroform and acetone solutions. you stated you are getting migraines I bet this is the cause.

chloroform in the air gives me migraines as well as liver problems (ahh the curse of alcoholism)

I would next time use sodium hypochlorite for the reaction as I think it is easier to seperate due to there
being no percipitate.

I would say at a glance of what you have done that you did indeed make chloroform but it got trapped in the
calcium salts (yep you already stated that)

as stated above do not burn unknown compound mixtures and even if you know what they are only do so
if you know what the outcome will be.

best you throw an unknown like this away and next time do your tests on a much smaller scale so you dont
hurt the enviroment your self and your loved ones when things dont go right.

try again brother :) just try it on a smaller scale and maby try with a high conc sodium hypochlorite instead of
the calcium.

Calcium for me at least is one of those salts that is a real pain in the arse. I try to stear clear of it as much as
possible as it complexes with quite a few organics and always gives a nasty precipitate that is hard to filter
and gobbles up a lot of the goodies.

maby try making sodium hypochlorite from your calcium hypochlorite and sodium bicarb solution.

there is a writeup on here that explains how to do this. (I believe that it is somewere in the hydrazine thread)

use the procedure that has been corrected by chromic (OTC god of the hive)
http://www.erowid.org/archive/rhodium/chemistry/chloroform.h...


[Edited on 3-3-2012 by Ephoton]




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[*] posted on 2-3-2012 at 22:20


thanks for the directions, i will remember them for next time:)

calcium salts piss me off too, but i have 2kg of the hypochlorite, so why let it go to waste?

i tried the haloform reaction with some 2L of bleach i "borrowed" from the laundry room. i did it all correctly and left the CHCl3 layer to settle for a day. when i came back, the bottle had filled with so much gas that if if hadn't come back at that time, it would have exploded. my yield was 6g, the theoretic being 36g:o.
the CHCl3 has been stabilized with 5% ethanol.

we live on 6 acres and have a bonfire every year, would it be wise to add this to it:D

Li
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[*] posted on 2-3-2012 at 22:42


calcium salts should not be a serious problem if there in small amounts to the enviroment.

this sounds like another hole job :) just make sure your next one is smaller then when you are getting
close to the yeilds you expect slowly step up the size if you need more.

turn your caclium hypochlorite into 10 - 15 % sodium hypochlorite at least then your not waisting it.

dont burn chemicals if you can avoid it imagine you dump the chems (which should be not a prob to be honest
after some time) on the fire pile. then after 12 months of putting experiments on there you go to light it.

dambed if I could remember exactly what I threw on there under the circumstances. you would be burning
a mixture of unknown reactions.

still calcium nitrate and hydroxide and other ions are used for ag and farming so it wont do to much damage to
the environment. if you dump it on grass expect it to wilt after a week and then after a few rains come back :)

with what you have I would be more worried about animals so put it a few feet under so they cant get there noses in it and if you have a bore for water be carefull that you dont place any chems anywere near it or
you will be drinking your reactions.

4.2% bleach is not always the best for haloform reactions 10 + is way better also bleach over time looses its
potency maby this explains your low yeild.

what you should be left with when turning your calcium hypochlorite into sodium hypochlorite will be calcium
carbonate. This can go in the same hole as the failed extraction (I think your reaction worked just the extraction
didont)

I dont know how this place thinks of this but back on the hive we used to reasearch then post a dream (procedure someone wished to follow) it would then get shot down or excepted.

This makes for a much easier time when doing reactions as you get the advice before the aftermath.

of course the dream should be posted in beginings as your about to begin a synthesis and are not realy
talking about theoretic chemistry and are not sharring results.

oh be warned chloroform in OZ needs a license to be legal so be carefull who you talk to about your hobby
I would hate to see some one take your love for chemistry the wrong way.

best of luck brother and dont worry to much so long as the reaction didont get too hot there is probably no
phosgene (though the burning is a worry) get rid of it and work on a smaller scale.

when stepping up you will find that cooling is one of the hurdels you will have to overcome. its much easier
to cool a small solution than a large one.

stirring makes a massive difference when cooling larger solutions also never put a reaction like this into a bowl.

your asking to breath it in if you do this try and keep reaction and products that come from reactions contained
as much as possible.
This can be harder than it sounds especially for a new reaction set. but by trying to always think that it is better
to keep chemicals contained and away from your nose eyes and skin you will always get better yeilds and
have a much safer and enjoyable time.

I am a little upset with some of our brothers/sisters here for not telling you that blowing into reactions with your
mouth and putting reaction mixtures like this into open containers like bowls is dangerous.

well done in making chloroform lithium dont give up or get disinheartend just be a little more carefull :)




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[*] posted on 2-3-2012 at 23:01


thanks ephoton.

i was going to use the CHCl3 to make a safe 12% sol. of NCl3. i have barely any chloroform, so i think if they turn up thinking i am trying to extract alkaloids, i think i will be safe.

blowing into a CHCl3 containing solution sounds pretty bad now that i look back on it:)

eventhough i live out of town, i cannot find a ag farming warehouse anywhere. nitrates are the bane of my existence!:)

but this still brings me to the question, what is the purple ppt?

Li

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[*] posted on 2-3-2012 at 23:08


I would say that it is not one compound but a mixture of a few.

as to what they are I am not sure but calcium carbide (which this is not) is black purple.

aldol condensations of acetone can go red and stain other salts this color.

in the end it may be like paint you have had a few side reactions and it has stained your precipitate.
Free chlorine in the reaction may be responsible as you left it for such a long time.

Still I am not sure lithium what the precipitate is nor can I find any leads from a quick search online.

Too add to this you used the word safe for NCl3.

dont think this way always believe that what you make is not
safe so make sure (especially for what your planning) that you
do this on a very very small scale and try and take as many
precautions as possible.

I have not worked with NCl3 but NI3 which I have played with
was more than scary enough.

just remember unknown precipitate from making solvent.

dont know what impurities are in the solvent that may react
with the NCl3 :)

tiny volumes very tiny if I was you.

good luck dude play it safe and if your realy interested in this
follow it up as a carrer path so you dont end up outside the law.

Chemists get paid pritty well and can travel the world working on
wonderfull jobs.

Some times they can even change society itself it is a carrer and
passion well worth following.

[Edited on 3-3-2012 by Ephoton]




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[*] posted on 2-3-2012 at 23:14


that was a quick reply!

i don't think it is a calcium salt as i read somewhere that most/all Ca salts are white.

i have 1kg of calcium carbide, and i can tell you that it is not purple/black, though more of a cream colour.

i should run some tests on it, but i have 10+ assignments due next week, and i have yet to start them:o

oh well

and yes, i once made nitrogen trichloride by accident in a test tube. i immediately poured it into heaps of ammonia sol. that was very scary.

i was running by a synth plante1999 had posted on youtube, which makes extremely small amounts.

i dont even know what to use NCl3 for yet, any ideas?
Li

[Edited on 3-3-2012 by Lithium]

[Edited on 3-3-2012 by Lithium]
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[*] posted on 2-3-2012 at 23:17


I edited my post just so you know :)

here is a link to a purple calcium salt.
http://factory.dhgate.com/other-chemicals/black-purple-gray-...

remember when salts are wet there colors can be different or more vibrant as well.

At a guess I would sat its a chlorinated organo salt of calcium.
which one though I have no idea.




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[*] posted on 2-3-2012 at 23:25


i guess i just got owned! though mine is a cream colour nonetheless:D

you beat me too it, but i was just about to say that the amount of chlorine and organic material in there is enough to produce many different chlorinated organic materials, and the Ca ions don't help much.

Li

[Edited on 3-3-2012 by Lithium]
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