Sciencemadness Discussion Board

Haloform with Calcium Hypochlorite (70%)

NEMO-Chemistry - 16-12-2017 at 12:59

I have read the erowid and SM posts about this, but the scales are much larger. The other problem i have is I dont fully understand where the figures used came from.

I want to use IPA (i find it better than Acetone) and calcium hypochlorite tablets, the ones i have say 70% available chlorine, i am not sure what this means regarding bleach.

70% seems really high considering the bleach i normally use is 15%. I dont have any normal bleach, so how much CH do i use per X amount of IPA?

Any help appreciated.

This is for the caffeine extractions I am doing, i wasnt going to use Chloroform but something I have read has made me decide to give it a go.

Aqua-regia - 17-12-2017 at 02:04

I produced chloroform a couple year before with calcium hypochlorite. I tryed several ways out, and the best methode was following:

Dissolved 3 mol common Ca-hypochlorite granular bleach + 600 ml water + 200 ml 10% NaOH.

between 40- 60 degrees celsius dropped acetone (34 g) into the flask with stirring. Exothermic reaction! If the reaction was done, distilled the chloroform off. Purification with shaking twice water and H2SO4 . Yield was quite good : 85%

Acetone is better starting material than IPA. Nail polish remover is good for it. Just calculate it for pure acetone contain.

IPA need more bleach for haloform, because the first step to oxidising it to acetone and the yield was in my exprerience worster compare with acetone.

NEMO-Chemistry - 17-12-2017 at 02:19

Thx for that, i use IPA because I have alot more of it, plus with IPA i only get a tiny rise in temperature. Normally it tops out around 25C starting from 10-15C.

The NaOH info is good so thx alot. I only need 200ml of Chloroform, its cheaper to make (my IPA was cheap) than buy it.

Aqua-regia - 17-12-2017 at 02:33

The swimming pool granular calcium hypochlorite has appr. 65-70% pure Ca(OCl)2. I checked it by iodometric titration before.

NEMO-Chemistry - 17-12-2017 at 02:42

Quote: Originally posted by Aqua-regia  
The swimming pool granular calcium hypochlorite has appr. 65-70% pure Ca(OCl)2. I checked it by iodometric titration before.

Ok great, so active chlorine in this case, simply means the purity of the chemical! It confused me, you dont often see bleach being sold as 5% active!

So its a simple (not for me lol) case of adding up the numbers and deducting 30 ish %. The rest is the same as normal.
Apart from the bits i have read that make it sound a bit of a mare to work with.

If needed i will distill straight off the main solution. Handy way to keep bleach though.

XeonTheMGPony - 17-12-2017 at 07:04

I've had very consistent results just following the erowid method. Bit tedious but very good conversion rate, very easy to manage.

Slight modification I use is to warn up the bleach solution befor adding the acetone so it kicks off the first drop and then allowing the exotherm to maintain reaction temp, I use an Allihn reflux condenser with good cold water 1 to 2c

It is the delay between addition and kick off that can cause issues, so preheating helps to reduce that lag so you don't inadvertently add to much, like wise had a bowl of cold water handy if it does get to vigorous.

Next run I will use MEK via Nurderages method with the powder modification to get propionic acid.

NEMO-Chemistry - 18-12-2017 at 22:33

First run didn't go well. My IPA. might be wet by now though. I will dry some out and give it another shot

JJay - 19-12-2017 at 00:36

I did a writeup on that a while back with acetone... it's in Everyday Chemistry I think. IIRC it takes 3 parts bleaching powder to one part acetone. The amount of water you use is somewhat arbitrary, but more is better to a point. You want strong stirring to make sure everything reacts, and if you don't have it then don't make chloroform from bleaching powder on a big scale because it is no fun manually shaking a big flask full of hot bleach, chloroform, and acetone with a condenser attached. Also, the suggestion to have some cold water nearby to dunk the flask is a good one.

[Edited on 19-12-2017 by JJay]

NEMO-Chemistry - 19-12-2017 at 03:55

My problem was getting anything to react. I will use less water and stir overhead until it gets going. I think i prefer the 15% bleach method :D.

NEMO-Chemistry - 19-12-2017 at 11:18

I am going to try and order Chloroform instead, looking into it the solubility is 21% @ 25C. No idea what it is at lower temps. Also it seems most stable PH 3.5 - 5.5, which probably isnt great for Chloroform. Also i note its prone to form Chlorates at a pH above 9.

Atom Scientific sell it cheaply, but the shipping is expensive (really expensive), the other brand they operate is ACP Pure, they dont sell Chloroform, but the shipping would be free if they did. This is annoying as I have a APC pure order ready, i called them and despite the chemicals being in the same place, and being dispatched at the same time and carried by the same people, they wont let me combine the order!

So I am looking for somewhere else to buy it

JJay - 19-12-2017 at 12:06

Chloroform's solubility in water is only about 1%.

NEMO-Chemistry - 19-12-2017 at 12:30

Quote: Originally posted by JJay  
Chloroform's solubility in water is only about 1%.

Sorry I have badly written the above! I was referring to calcium Hypochlorite having a solubility of 21%.

Seems like a bad choice for Chloroform production, but then again it isnt the easiest solvent to get hold of. But it looks like its a great solvent for coffee exaction.

[Edited on 19-12-2017 by NEMO-Chemistry]

JJay - 19-12-2017 at 12:34

Oh right... you actually don't have to dissolve all of the bleaching powder (though why wouldn't you?), but I completely agree that bleaching powder is not ideal for producing chloroform.