The Vespiary

The Hive => Stimulants => Topic started by: Bandil on February 18, 2004, 12:24:00 AM

Title: DCM for post RP/I2 extraction
Post by: Bandil on February 18, 2004, 12:24:00 AM

Hi!

This is the first post in the stimulant forum, so bear with me  8) .

Usually DCM is my preferred solvent for extracting basically everything, but meth seems to be swims nemesis. After filtering and washing the post reaction liquid, the stuff is basified and extracted with DCM. I Think 2 X 100 mL's was used for a 20 g's batch. The yield coming out of the DCM was however less than 10%... And this is the case in every meth extraction that has been tried out. It always ends up with a tedious steam distillation of the meth out of the basified water phase etcetc...

Any reason why DCM perform so horribly on this particular molecule? Any other amines has never given any troubles with this solvent... And what would be a better choice, ether or something similar?

Regards
Bandil

Title: A different NP
Post by: kris_1108 on February 18, 2004, 12:38:00 AM

Hi how are ya
I don't know much about DCM but I do know that you could replace it with Toluene or Xylene. As for doing two pulls, well some would say do three and leave the last one over night.
Remember that DCM is the bottom layer in your sep funnel! However, Toluene or Xylene will be ontop. That may bee where the problem is.
DCM is more effective than Xylene/Toluene so you dont have to use as much.
Remember to base the reaction BEFORE adding DCM, Xylene/Toluene - add first, and then base.
You should bee gassing when using DCM, as it does not titrate well.

I will take no credit for any of this information cos I stole it all from here -

Post 428410 (https://www.thevespiary.org/talk/index.php?topic=8697.msg42841000#msg42841000)

(geezmeister: "The post-reaction workup: a cook's summary", Stimulants)(thanks Geez ;D )

Title: I can't guarantee whether this info is 100%...
Post by: mr_pyrex on February 18, 2004, 01:32:00 AM

I can't guarantee whether this info is 100% correct or not, but I do seem to remember that DCM reacts somewhat unpredictable when it comes into contact with either bases or acidic solutions.  But as was stated above...toluene would be a more preferable extraction solvent for meth.   Good Luck and Bee safe.  Pyrex out of extraction techniques

Title: Never heard that DCM should be unstable in...
Post by: Bandil on February 18, 2004, 01:36:00 AM

Never heard that DCM should be unstable in acidic/basic solutions. But the odd thing here is that DCM works wonders for everything else but meth... Very strange indeed. Maybe the tweaker gods don't like me  :)

Title: other solvents
Post by: geezmeister on February 18, 2004, 06:43:00 AM

Other, less expensive solvents, work quite well. Extracting twenty grams of meth with 200 ml of solvent? I haven't looked it up, but I would think using more solvent would likely improve your yield. Tolulene, xylene, and even hot naptha work very well for this extraction. If you want a bottom puller, TCE works well,but you will need to wash it well with water to remove the base before gassing.

Title: Ether?
Post by: place on February 18, 2004, 06:56:00 AM

First post, yep hey  :)

What about Ether? Would that work better than eg. DCM or chloroform?

rgs, place.

Title: Please use the search engine!
Post by: JUMPER on February 18, 2004, 07:13:00 AM

Follow Geez's advice above. Much easier to acquire for most and work great. Otherwise hit that search engine again for ether.

Bandil just said first post here in stimulants. If he wasn't a dinasour at the hive he might have gotten flamed to UTFSE (no offense bandil). But then I was polite and didn't flame you. You will find your answers there.

Title: I have the problem that I cant get DCM where I
Post by: shulginwannabe on February 18, 2004, 09:17:00 AM

I have the problem that I cant get DCM where I live, so I need an replacement. Which is the best? If I use say Xylen, how much more (than DCM) will I need?

kris_1108: Do you mean that when using xylene or toluene you have to base the meth after you add the solvent? Why?

Title: I think you misunderstood the sentence swik
Post by: gluecifer69 on February 18, 2004, 12:12:00 PM

---

Remember to base the reaction BEFORE adding DCM, Xylene/Toluene - add first, and then base

---

I think what kris meant by add first is the base.  This is usually done with a diluted Sodium Hydroxide solution, to  making the basing not as exothermic as opposed to adding the dry soium hydroxide to water.

The reason naptha is often preferred is because it is not as an aggressive solvent as Xylene or tolly and won't pull back as much garbage. Remember that naptha must be warm to perform well as it is lazy at room temperature.  Swim read once where Wareami said that a 50/50 mix of ether and naptha would be the ideal NP.

On the other hand swim wouldn't wash his post reaction fluid without including xylene, tolly or some other "aggresive" solvent.  TCE(tetrachlorethylene) is also a great post rxn fluid washer.

Title: About twice as much
Post by: kris_1108 on February 18, 2004, 12:17:00 PM

Hi shulginwannabe,
I think you hve to use about twice as much xylene/toluene as DCM.
I dont actually know why the NP should be added before basing.

Title: what about mineral spirits
Post by: Buckshot on February 18, 2004, 12:17:00 PM

what aqbout plain old, cheap, and non-flamable mineral spirits? Why doesn't anyone cept me, seem to use this stuff?

Title: Buckshot you are not alone
Post by: gluecifer69 on February 18, 2004, 12:31:00 PM

Swim has used oderless mineral spirits more times than any other NP, only recently has he finally tried Naptha. Their main advantage is their availibilty and cheap price. 8)

Swim doesn't know why they are hardly mentioned here. Are there any disadvantages that any bees have encounted using oderless mineral spirits?

Title: disadvantages
Post by: geezmeister on February 18, 2004, 12:52:00 PM

well, yes. And no.

I never found it to be as effective a meth solvent as hot naptha or xylene, and we are playing a game where a gram of product is worth many times more than the value of the solvent. I find naptha gives a clean extraction if one titrates for the meth HCl. Xylene seems to be very effective if one gasses, and I prefer its dryness and lack of affinity for absorbing water.

I also had occasions where I used odorless mineral spirits as a pre-extraction wash of the reaction fluid and for some reason is was miscible with the reaction fluid. I never obtained any response to my post asking if anyone had similar experiences. I stopped using it post-reaction after that experience. Regardless of its low price, if there are conditions in which it becomes miscible with the reaction fluid, I will use something else.

Title: I can't see any reason it would bee miscible...
Post by: foxy2 on February 18, 2004, 05:54:00 PM

I can't see any reason it would bee miscible with the post reaction fluids.  If it was then a little bit of water should have taken care of the problem.

Title: Got a Grudge with Naphtha?
Post by: ChemoSabe on February 18, 2004, 08:03:00 PM

Are you somehow opposed to the usage of Naphtha for this as it seems to be the #1 favorite of most for this particular application.

edit - just experienced a strange time warp where there were no reponses to this right when I started the post but about 10 more had been addeed once I'd submitted it so sorry if the info's now redundant

Title: me too
Post by: elfspice on February 18, 2004, 08:11:00 PM

I've tried using turps a few times, and i found the same thing, some kind of water soluble residue also comes across on the other side... I decided it was only useful as a defatting solvent, and only if one washes afterwards a couple of times with naptha or something else less crappy. Whatever this residue is, it also smells bad, somewhat remeniscient of the main smells in regular mineral turps.

Title: I can see there is diffents opinions on this...
Post by: place on February 27, 2004, 09:27:00 AM

I can see there is diffents opinions on this subejct, but most of you think hot naptha is the best to use?

Placebos methode, the last A/B ekstraction of the honey, what would be best, chloroform, N-Heptan or hot naptha?

Title: NONPOLARS
Post by: Ganzas2003 on March 15, 2004, 08:01:00 AM

hi

hey ive extracted meth using the following:

1. TURPENTINE - CAS Nº8006-64-2
  
Well it didnt worked. Left residue and the smell was there after the water evaped. Only used once for the very first reaction, a straight curbs nano.

2. XYLENE/TOLUENE - NO CAS No.

Directly from the can which states "Contains Xylene/Toluene" and its sold as paint thinner("celuloso"). Extracts well in my opinion. Room temperature. Extracting garbage...well that leaves room to think about it now that this is mentioned...yes maybe i agree but still ceptic at the same time.

3. NAPHTA

Directly from the can which states "Contains naphta from pretroleum(petroleum).medium alifatic" and its sold as paint thinner(sintectic).
Using currently and allways the same.recicling.not measuring anymore.just dump the whole.
Heated in microwave maximum power for 2:30 minutes. i guess thats hot enough!:)
I like the naphta for extracting. cant seriouly notice a serious improve in yields but i like the naphta.


I just received some chloroform. I order it along with some other shit coz i read that it can be used to separate the meth from efedrine. 3 questions:

      - can anyone link me to a procedure for this   please?thx.
 
      - Can chloroform be used to extract meth freebase and tritated as per normal method?(water+4/6 drops HCL?)

      - what about using cloroform to wash the pills?

regarding DCM i have 2 cans there...I found it useless since its kinda of a thick paste...thicker then honey bee....i guess its mixed with some other shit. Its sold as paint remover but states "metilene chloride"...can i use a method to get the pure DCM from this thick shit?

in th emean time ill stick with the hot naphta.

Title: Choice of NP?
Post by: place on April 15, 2004, 01:10:00 PM

The name "Naptha" is not so "worldwide" knowen, so SWIM is not sure what the name covers. When he extracted meth FB, he can choose to use "white spirit" (is that naptha?) or Xylene? What work best? The NP is going to be washed (and not gassed) with H2O + HCL to extract and make meth.hcl crystals.

Title: naptha
Post by: elfspice on April 15, 2004, 05:25:00 PM

variations of the same basic solvent involving different blends of the various fractions boiling from about 40°C to a small amount up around 110ish basically contain pentane, hexane, heptane, benzene (these days usually very trace) toluene and various isomers of saturated hydrocarbons in that boiling range. It is not the most ideal solvent, vogels says one should try to use fractions with no more than 20 degrees (celsius) of boiling point difference as otherwise there can be solubility interactions and issues when distilling and whatnot. It is variously called 'white spirit', 'naptha', 'vm&p naptha' (varnish makers and polisers i think that stands for) shellite, fuelite, calite, mobilite, bla bla bla. pegasol...

Probably the biggest caveat of this solvent is that it's just not that good, and you can't always guarantee it hansn't got something problematic in it, for example i recall seeing shellite and other substances which have, for example, napthalene in trace amounts, enough to make the whole thing stink, and other things too, i think one bottle i saw one time had oil of wintergreen in it or something.

yuck

if one is using it to extract to a final salt product, toluene and xylene are about the best choice in terms of availability, cost and effectiveness... they are also a bit safer, by a fair degree, than naptha, as the pentanes and hexanes boil quite low and have quite a lot of vapour pressure, and ignite explosively. a lot less expensive than dcm and ether too

using the the fraction about 45-69 of the local naptha seemed to give the best results for extraction. A local supplier sells a solvent about this kind of consistency (maybe a little narrower) which is the same price as toluene and xylene, i would say it should be available elsewhere. the stated uses of this almost n-hexane are in extracting plant oils, things which can't be steam distilled because of high bp, i think this includes its use to extract triglycerides (fats and oils) from nuts and seeds and other such things. It certainly seems to make a good defatting solvent.

that very good and useful fraction in naptha is frequently 1/4 to 1/5th of the volume, so it's cost is high if sourced this way.

Title: um...
Post by: auntyjack on April 19, 2004, 03:35:00 PM

my chemistry book says the naphtha layer is between 110 and 180 C (consider that toluene boils at 110 C and xylene at 140)....previous posts on naphtha give good info on the various types and their respective boiling point ranges....elfspice, where did you get your info from?

Title: er
Post by: elfspice on April 19, 2004, 06:11:00 PM

the terminology of various lower boiling petroleum distillates is perhaps deliberately confusing as it has manifested out of marketing strategies and not standardised nomenclatures etc etc...

I know 'naptha' as a chemical, a dual hexane ring thingy, that is not what i mean, i think it is 'vm&p naptha in some places' which fits the same ranges (40ish to 140ish)

bla bla

here's the local low bp solvent's msds

http://www.andrewindustrial.co.nz/content/images/docs/msds/chemicals/Fuelite%20MSDS.pdf (http://www.andrewindustrial.co.nz/content/images/docs/msds/chemicals/Fuelite%20MSDS.pdf)

here's there special purpose plant oil/extraction solvent, a nice hexane fraction

http://www.andrewindustrial.co.nz/content/images/docs/msds/chemicals/Solvent%20X4%20MSDS.pdf (http://www.andrewindustrial.co.nz/content/images/docs/msds/chemicals/Solvent%20X4%20MSDS.pdf)

the data stated in the fuelite msds seems to be incorrect from its behaviour in distillation, it started distilling a fraction at about 38 degrees C