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caesee
03-26-2006, 04:42 PM
Seen this question before, thought this was interesting and could be of use to some

With that said, enjoy purifying your opiates. If only SWIM knew where to get chloroform or ether.......................... *sigh*

Pictorial - cleaning opioids.

The following pictorial was done using things like water, sugar, cacao
(for color), milk-powder. No illegal substances were used.

Needed:

- distilled water
- ether (or any other NP)
- Hydrochloroc acid (HCl), 25%
- ammonia (=ammonium hydroxide), 25%
- pipette 10ml, pipettes 1ml to add liquids dropwise
- magnetic stirrer with stirbar
- 2 small test tubes
- 1 glass
- evaporation dish (petri dish)
- sodium bicarbonate (or tricarbonate)

Time: about 1 hour


1. The opioid, for example street heroin, is put into a small test
tube together with some drops of 25% HCl, 10ml of water and
dissolved.
http://i35.photobucket.com/albums/d166/poppyjohnny/start.jpg

2. The solution is poured into a small vessel and placed on a
magnetic stirrer. Stirbar is dropped in. Diluted Ammonia
(1 drop ammonia on 1ml dH2O) is now added dropwise.
[The liquid is normally clear before ammonia is added, the
pic was taken after the ammonia step because I had to retake
the pic.]
http://i35.photobucket.com/albums/d166/poppyjohnny/000_0057.jpg

3. After a certain amount of ammonia has been added drop by
drop the liquid will look like this from one drop to the other.
http://i35.photobucket.com/albums/d166/poppyjohnny/prec.jpg

4. The solution is transferred into a testube again and ether is
poured on it, about 1/3 of the amount of liquid. You can see the
two layers.
http://i35.photobucket.com/albums/d166/poppyjohnny/testtube1.jpg

You can see how something white is settling down on the bottom
within the bottom layer. This is the spirit of the substance that
we had bought on the street. The clear layer on top is the ether.
If we had used chloroform, the NP layer would be on the bottom.
http://i35.photobucket.com/albums/d166/poppyjohnny/testtube2.jpg

5. After it was shaken for 3 minutes, two new layers form. You can
see the top layer now contains something, while the lower layer is
almost clear. In between them you see brownish stuff. We call this
a gross shit a** emulsion, that we want to get rid off. So we wait.
http://i35.photobucket.com/albums/d166/poppyjohnny/emulsion.jpg

6. After a while we pipette off the top layer an put it into another test
tube. We pour the solution, which is now clear again, from tube 1 into
the little vessel, place it on the stirrer, add ammonia and see if
precipitate forms again.
http://i35.photobucket.com/albums/d166/poppyjohnny/secondrun.jpg
If yes, then we shake it with ether again. If not, we can discard
it or shake another two times with ether to make sure everything
is collected. So on the above pic we have: tube 1, which contained
the solution which was shaken with ether. Tube 2, which contains
the ether layer and to which we add any ether from further NP
washes on the mother solution that we had pipetted off. And we
see the glass with the mother solution, in which we repeat the
adding of ammonia.

8. We then make up a little diluted HCl with 15ml dH2O and 15
drops of HCl 25%.
http://i35.photobucket.com/albums/d166/poppyjohnny/15mlhcl.jpg

We add 5ml of that to the ether in tube 2 and shake it.

9. We pipette off the water layer on the bottom of the test tube
and our it on something flat to evaporate it down.

10. But before we evaporate it, we add Bicarb to neutralize
any acid that is not bound to product. This happens:
HCl + Na2CO3 -> NaCl (Table Salt)+ H2O (water) + CO2
(Carbondioxide).
http://i35.photobucket.com/albums/d166/poppyjohnny/bicarb.jpg

It will bubble. The bubbles are the CO2 that is freed. The volume
of the liquid will raise cause of water and Table salt beeing
formed.
http://i35.photobucket.com/albums/d166/poppyjohnny/bubble.jpg
__________________

11. After the bubbling stops, it is dried in the oven for 30 minutes
at 40 - 50C.
http://i35.photobucket.com/albums/d166/poppyjohnny/drying.jpg

The final product.
http://i35.photobucket.com/albums/d166/poppyjohnny/finish.jpg

illchemist
03-26-2006, 07:12 PM
Looks good... There is most likely NaCl contaminating your product from doing the neutralization. Excess HCl will just evaporate off and will not harm anything. It also looks like you do a lot of transferring which can lead to a greater loss of product.

Keep it simple:

-Dissolve crude material in Acidic H2O
-filter (optional) and wash acidic layer with NP to remove contaminants
-basify with ammonium hydroxide and collect precipitate (extranct with NP or filter)
-acidify by dissolving in minimum amount of HCl solution and evaporate

respect...

illchemist

bogumil
03-30-2006, 05:47 PM
Here are just some ideas of someone who has never done this ....

Syringe filters would make it a little easier maybe, as a clearer solution probably gives a better precipitation.

SWIM prefers syringe filters cause they are easier to handle, faster and the loss is smaller (you can press an aditional ml water through it and get the stuff out that stays in the filter. They hold bck only very tiny amounts.

You also could skip step 5 (no transferring into an NP a second time) when you use the micron filters. Just let it rest a little longer and pipette off the top layer, then collect the precipitate adjust the pH and dry it.

And yeah, it might really save some material if one could leave it in one vessel, the test tube for example.

Just an idea ... good work.