Author Topic: European pill extraction Writeup (preliminary)  (Read 6890 times)

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jammin

  • Guest
European pill extraction Writeup (preliminary)
« on: May 30, 2004, 08:37:00 PM »
Ok, there are some others on the board with similar european non-supergaked pills and no access
to all the solvents used in the extraction procedures here.
(EDIT: someof the solvents are illegal where swim lives due to cancer related issues, and some are just not avail OTC, like xylene and MeOH. Belive me, he has tried. He even got LG RP and LG I2 and whatever he wanted, but some things readily avail in the US just isnt here)

I thougth i'd make a semi-writeup with exact volumes of solvents.
Thanks to geez, wareami and all the others that helped this confused euro-trash out.

(I was thinking about using this volume: 1000 tabs * 30 mg = 60g pillmass)

Correct me where im wrong here, and somebody please fill out the _?_ and replace them with a number! ;)
That way the euro bees can have their "own" writeup on the non supergaked pills.

(Obviousely they were more gaked than i thougth, thats why i wrote this down)



Anyway:


01 Distil tolly, then it should be dry.

02 Soak in _?_ ml toulene for 6 hours.
   How much toulene should i use?
   People just say let it cover about an inch etc.
   But that really depends on the shape of the container,
   and can thus vary a great deal. An amount in ml would be great!

03 Nuke in microwave for three minutes (on lowest setting?), take out and stir.
   Repeat until pillmass is hot enough to heat toulene (toulene wont heat by itself in a microwave)
   When toulene is close to boiling take it out and stir for about five minutes.
   Nuke one more time and let it sit and settle.
   Decant toulene into thrash container and repeat twice.

04 Repeat step 4 with _?_ ml dry VM&P Naptha or equivalent

05 Add _?_ ml dry acetone to pillmass and bring it slowly to a steady
   boil while stiring. Decant acetone into trash container

06 Let toulene, naptha and acetone cool in trash container and observe
   all the trash that crashes out when it cools

07 Dry pillmass

08 Add _?_ ml IPA, bring to boiling and filter trough prewetted filter.
   Add one drop of acid (HCl) for each theoretical gram of e.hcl to guarantee acidic conditions (only for ephedring, does not apply for psuedoephedrine)

   Repeat twice, joining extracts into new container.

10 Evaporate on pyrex dish on low heat with fan blowing over.
   When IPA has almost evaporated, do an acetone crash (

Post 238802 (missing)

(geezmeister: "Re: Acetone Crashing", Stimulants)



place

  • Guest
A/B
« Reply #1 on: May 31, 2004, 07:16:00 AM »
I would still do a A/B extraction or key plunk at the end.

jammin

  • Guest
ok, place
« Reply #2 on: May 31, 2004, 07:20:00 AM »
can you edit the wripteup to reflect that?


place

  • Guest
Ker plunk
« Reply #3 on: June 01, 2004, 03:38:00 AM »
Well, about the ammount of IPA, I don't have a glue. IPA and E is a bitch! ;)

After your extraction is finish, take your raw crystals, dissolve them in DH2O and do the Ker plunk. Wash the final product once in acetone and your should be ready to GO!

jammin

  • Guest
IPA Volume
« Reply #4 on: June 01, 2004, 04:29:00 AM »
I use 50ml IPA for 6g pillmass.

I guess i'll just use the same amount on all the solvents.
Seems like noone has excact amounts anyway. Most extraction procedures i've seen just state "cover the pill mass with about 2 inches.." etc, but this really depends on the container volume...

::)


wareami

  • Guest
Just for phun...
« Reply #5 on: June 01, 2004, 06:22:00 AM »
Jammin...most extraction methods won't list exact liquid volume measurement because all pills are different sizes.
Usually you're likely to see recommended volumes in the form of 3 times the amount of pillmass where alky extracts are concerned.


place

  • Guest
About IPA and E
« Reply #6 on: June 01, 2004, 03:24:00 PM »
To quote Newton from [url=

Post 501322 (missing)

(place: "Fucked up recrystallization?", Stimulants)
:


20g of l-ephed.hcl will not completely dissolve in 1/2 litre of warm IPA.




There must be a more efficient alcohol than IPA when playing with l-E.


jammin

  • Guest
EtOH as a replacement?
« Reply #7 on: June 02, 2004, 09:11:00 AM »
From various posts i've read that EtOH was reported to give better results than MeOH and IPA.
Both yieldwise and in respect of pulling out less gak/fillers. As MeOH is hard to get and and e.hcl
is less solluble in IPA, perhaps denaturated is the way to go. In swims location denaturated is pure ethanol
with denaturating and color agants. I.e. No MeOH.


It has also been brought to my attension that the EU pills are infact gaked in the same manner as US pills.
This was not the case a couple of years ago he said.
This statement comes from someone with hands on experience with EU pills.

I also talked to another bee that did a water pull and A/B it. Hoping for a writeup from him.

Here are some refs for ephedrine.hcl (it varies from psuedo as you probably know):

Post 509365

(Rhodium: "No exact answer, but a lower solubility limit...", Stimulants)



geezmeister

  • Guest
not quite
« Reply #8 on: June 02, 2004, 01:02:00 PM »
"EtOH was reported to give better results than MeOH and IPA.
Both yieldwise and in respect of pulling out less gak/fillers"

I disagree. Don't confuse yield with purity. High yields often indicate lower purity. EtOH and MeOH are both more agressive solvents than IPA. They dissolve more substances, and do it faster than IPA. That might not be what you want to happen.
 
"perhaps denaturated is the way to go. In swims location denaturated is pure ethanol with denaturating and color agants. I.e. No MeOH."

Where SWIG lives the principal denaturant IS MeOH, which is poisonous. Do NOT assume denatured alcohol does not contain MeOH. DO assume it that it is about 5% water. I do not imply on cannot use EtOH in extraction, and in fact many people do. Do not assume that because EtOH or MeOH is a more agressive solvent is it a better solvent for pseudo or E extraction than IPA. They may be better at doing some things you don't want done than they are at doing the things you do want done.


jsorex

  • Guest
EU solvent bottles are required by law to list
« Reply #9 on: June 02, 2004, 01:15:00 PM »
EU solvent bottles are required by law to list what they contain. Thus, if MeOH were present it would be esasy to check. But I haven't seen MeOH denaturated alcohol here  for years anymore. I guess it is just considered a toxicological risk. They use some nasty tasting amines and shit like that.


methyl_ethyl

  • Guest
denatured
« Reply #10 on: June 02, 2004, 02:23:00 PM »
In swims location denaturated is pure ethanol
with denaturating and color agants. I.e. No MeOH.


The denaturing agents in the US are more than likely IPA or Methanol or both.

EDIT Or in the EU there are hundreds of different formulations used to denature ethanol.  ::)


place

  • Guest
It has also been brought to my attension that...
« Reply #11 on: June 02, 2004, 03:48:00 PM »
It has also been brought to my attension that the EU pills are infact gaked in the same manner as US pills.


I don't agree. In US, the government use gakk to make it harder for meth cooks. I don’t think that’s the case with many EU-pills because using E to make meth isn’t that known in EU, at least not compared to the US. I don’t think the gakk you find in most EU pills is there to annoy meth-cooks, but for other reasons. Or am I to naive?   ;)

jammin

  • Guest
Gak in the EU
« Reply #12 on: June 03, 2004, 03:55:00 AM »
I dont know about the amount of gak personally, but i was under the same impression as you place...

anyway i got this in a PM:
---------------------------
SWIM has pratical experience with all types of european pills, it´s a urban myth that our pills are not supergakked, in the last 2years many pharma companies changed their mixtures.

Some pillz are extractable with a few MeOH pulls and others need US style pill cures to get rid of the gaak, depends on the brand used.
-----------------


When i extracted with only hot 50% IPA i got about 3g from 6g pillmass. That would be about high 90% return.

If it was a large amount of gak following the alky i find it strange that IPA would not extract e.hcl + fillers thus giving a 100%++ return.

I dont know if im way off here, but...

Anyone else with practical experience who can enligthen us?


Newton

  • Guest
EDIT Or in the EU there are hundreds of ...
« Reply #13 on: June 03, 2004, 06:06:00 AM »
EDIT Or in the EU there are hundreds of different formulations used to denature ethanol.

I remember having read that there are 5 different denaturants for ethanol approved in the EU (one of them was pyridine). Methanol was not on that list. Methanol is not a likely denaturant for household ethanol in my humble opinion, as it would pose a considerable health risk. People use that stuff for cleaning surfaces in the kitchen area, or even lighting the barbecue coal (not recommended for other reasons).

Emde states in his classic papers on ephedrine that l-ephedrine.Hcl is more soluble in ethanol than in IPA, and I would assume that it is even more soluble in methanol, but I don't have data on that.

But Geezmeister is right, methanol and ethanol might solve alot more unwanted stuff as well, making it less useful for recrystallisation. Has anyone tried a H20 extraction of the l-ephedrine.HCl? It is very soluble in water, and that particular solvent is as OTC as it gets  ;) .

jammin

  • Guest
Yep, water extraction has been talked about...
« Reply #14 on: June 03, 2004, 07:23:00 AM »
Im planning to test water, IPA and ethanol extactions on the same amount of pillmass to see what works best.

Problem is that i've read that many gaks/fillers love water and will go with the pull. How to get rid of them? Evap and disolve in another solvent?


Some bee proposed a 24 hour water soak and an IPA recryst before an AB... Perhaps this makes sense?


KidCurry

  • Guest
Just a small note: Where I live (in the EU of...
« Reply #15 on: June 03, 2004, 07:27:00 AM »
Just a small note: Where I live (in the EU of course), OTC ethanol (not from lab supplier but supermarkets/gas stations etc)is almost always denatured with methanol along with some colouring and MEK if I remember it correctly.

jammin

  • Guest
Well...
« Reply #16 on: June 03, 2004, 09:14:00 AM »
I guess these issues could easily be overcomed by means of simple distillation. The coloragents vanishes like a breeeze. (not fun to stain the e )  :P


methyl_ethyl

  • Guest
EU Ethanol Denaturation
« Reply #17 on: June 03, 2004, 07:11:00 PM »
I remember having read that there are 5 different denaturants for ethanol approved in the EU (one of them was pyridine). Methanol was not on that list. Methanol is not a likely denaturant for household ethanol

I realize you specified household ethanol, I am not familiar  as to what denatured household ethanol is, however the following information may be useful.

Ethanol when used as an industrial solvent, has to contain one or more denaturants (Commission Regulation (EC) No 3199/93 of 22 November 1993 on the mutual recognition of procedures for the complete denaturing of alcohol for the purposes of exemption from excise duty).  Permitted  denaturants vary according to the end use and national practice, resulting in many different denatured ethanol formulations  (hundreds across all EU member states). The denaturants do not of course change the basic chemical properties of the ethanol as a solvent, merely render it difficult or impossible to divert to beverage applications. 

     As the  proposals stand, denatured ethanol suppliers would have to prepare chemical safety reports for each individual formulation,  and each end user  and supply chain actor would in turn need to maintain individual assessments for each formulation used and the components. This would create an explosion of bureaucracy and paperwork associated with denatured  ethanol formulation and use with no associated benefit for health or the environment.  Such bureacracy may well discourage continued use of what is a benign solvent (well known and controlled).  Whilst it would not be appropriate to exempt denatured ethanols from the rigours of REACH, we would propose  that a simplified system is adopted which enables grouped assessments to be used and a single assessment prepared for the denatured formulation.  Provided it can be demonstrated by the ethanol producer that the denaturant package does not increase the hazard of the ethanol itself, a system based on the hazard classification of the denatured preparation would be workable for industry; individual chemical safety assessments would only then be required for denatured preparations by classification category  e.g.  'non hazardous, 'irritant' etc.

Source: REACH Regulation (Ethyl Alcohol Group "EAG")


Related:

Alcohol Specifications
European Union

Ethanol Denaturants
22 November 1993

Please note: The text below is copied directly from the original, without correcting what appears to be factual and typographical errors.

The denaturants which are employed in each Member State for the purposes of completely denaturing alcohol in accordance with Article 27 (1) (a) of Directive 92/83/EEC are as described below:

Belgium

Five litres of methylene per 100 litres of ethyl alcohol irrespective of the alcoholic strength and sufficient colourant to produce a good markable blue or purple (violet) colour.

The following are included within the meaning of "methylene":

    * actual methylene, that is to say raw methyl alcohol produced from the dry distillation of wood and containing at least 10 % by weight of acetone,
    * a mixture of methylene and methanol containing at least 60 % by weight of actual methylene and 10 % by weight of acetone,
    * a mixture of methanol, acetone and pyrogenetic impurities with a strong empyreumatic colour, containing at least 10 % by weight of acetone.

Denmark

Per hectolitre pure alcohol:

    *  2 litres methylethylketone, and
    *  3 litres methylisobutylketone.

Germany

Per hectolitre pure alcohol:

1) 0.75 litres methylethylketone, consisting of

    * 95 to 96 % by weight of methylethylketone,
    * 2.5 to 3 % by weight of methylisopropylketone,
    * 1.5 to 2 % by weight of ethylisoamylketone (5-methyl-3-heptanon)
      together with 0.25 litres of pyridine bases;

2) One litre methylethylketone, consisting of

    * 95 to 96 % by weight of methylethylketone,
    * 2.5 to 3 % by weight of methylisopropylketone,
    * 1.5 to 2 % by weight of ethylisoamylketone (5-methyl-3-heptanon),
      together with one gram denatonium benzoate.

Greece

Five litres of methyl alcohol per hectolitre of impure ethyl alcohol, plus:

    * 0.5 % lamp oil,
    * 4 p.p.m methylene blue,
    * 1 % oil of turpentine.

Spain

Per hectolitre of pure alcohol:

    * 1 gram denatonium benzoate,
    * 2 litres methylethylketone (butanone), and
    * 0.2 grams methylene blue (CI basic blue 52015).

France

To one hectolitre ethyl alcohol at 90 % vol add:

    * 3.5 litres of methylene, and
    * 1 litre of isopropyl alcohol.

"Regie type" - methylene

Definition:

    * it must register 90 % vol at a temperature of 20°C, with a tolerance of 0.5,
    * it must contain at least 6 % pyrogenic impurities (disregarding products that can be saponified by soda and expressed as methyl acetate),
    * it must contain ketones and water to bring the methyl alcohol up to 100,
    * it must be obtained exclusively from the carbonization of wood, carried out under the supervision of the tax authorities.

The pyrogenic impurities are the real denaturants. They give the mixture an unpleasant taste, making the alcohol unfit for oral consumption.

Through its chemical properties, acetone makes it easier, in the laboratory, to isolate the denaturant in the alcohol.

Lastly, methyl alcohol indicates denaturation. Its boiling point is much the same as that of ethyl alcohol. It can therefore be separated only by using special techniques and apparatus.

In principal, its presence, above a certain percentage, which varies according to the different types of ethyl alcohol, indicates whether the alcohol analysed has been previously denatured by the general process.

Ireland

Mineralized methylated spirits:

    * 9.5 % wood naphtha,
    * 0.5 % crude pyridine,
    * 0.025 ounce methyl violet dye (per 100 gallons of pure ethyl alcohol),
    * 0.375 % petroleum oil.

NB: The wood naphtha and crude pyridine may be substituted with 10 % methyl alcohol.

Italy

Per hectolitre of pure alcohol:

    * 125 grams of tiofene,
    * 0.8 grams of denatonium benzoate,
    * 0.4 grams of CI acid red 51 (red colourant),
    * 2 litres of methylethylketone

Luxembourg

Five litres methylene per hectolitre of ethyl alcohol irrespective of the alcoholic strength and sufficient colourant to produce a good markable blue or purple (violet) colour.

The following are included within the meaning of "methylene":

    * actual methylene, that is to say raw methyl alcohol produced from the dry distillation of wood and containing at least 10 % by weight of acetone,
    * a mixture of methylene and methanol containing at least 60 % by weight of actual methylene and 10 % by weight of acetone,
    * a mixture of methanol, acetone and pyrogenetic impurities with a strong empyreumatic odour, containing at least 10 % by weight of acetone.

Netherlands

Per hectolitre of ethyl alcohol:

Five litres of a mixture consisting of:

    * 60 % by volume of methanol,
    * 11 % by volume of fusel oil (a concentrate of by-products of alcohol distillation),
    * 20 % by volume of acetone,
    * 8   % by volume of water,
    * 0.5 % by volume of butanol,
    * 0.5 % by volume of formalin (a watery solution of 37 % by weight of formaldehyde),

together with colouring the quantity and constituents of which meet the conditions laid down by the chemist of the Fiscal Service.

United Kingdom

Base:

    * 90 % vol ethanol,
    * 9.5 % vol "wood naphtha" (1), and
    * 0.5 % vol crude pyridine.

To each 1,000 litres of which is added:

    * 3.75 litres of mineral naphtha (petroleum oil) and
    * 1.5 p.p.m of methyl violet.

(1) Wood naphtha is a product which may be synthetic but must produce such properties as to render a mixture of 5 % wood naphtha with 95 % spirits unfit for use as a beverage. This is achieved by producing a relatively complex but stable "cocktail" of substances which cannot be easily removed from the spirits.

Composition of "wood naptha":
There is no prescriptive list of ingredients, but some or all of the following are found in approved synthetic wood naptha:

    * pyridine,
    * pyridine bases,
    * allyl alcohol,
    * crotenaldehyde,
    * picolene,
    * denatonium benzoate,
    * methyl alcohol