shady shady biz

[fightingfires]

@BIGMESC I tried something similar with methanol and water, only I heated them to just under the boiling point of methanol to get higher solubility, and (stupidly) I mixed the test raws in the water then added methanol until the test dissolved (the solution turned clear). I now have a nice solution of water, methanol and 20g of test-e raws. It doesn't recrystallize even in the freezer. I did get some sediment out that's definitely not test and not water soluble.

I tried similar @flenser. I took 10g of raw test E and dissolve it in methanol. Too much methanol (maybe 120-150ml) then slowly dripped frozen distilled water into it through a funnel over a period of a whole day. I probably added 1 liter of water during that time.
Nothing I could do would make the test precipitate out of the methanol.
I have no idea why but I could not make it work

 

[flenser]

I tried similar @flenser. I took 10g of raw test E and dissolve it in methanol. Too much methanol (maybe 120-150ml) then slowly dripped frozen distilled water into it through a funnel over a period of a whole day. I probably added 1 liter of water during that time.
Nothing I could do would make the test precipitate out of the methanol.
I have no idea why but I could not make it work

Right, with too much solvent you won't get anything. It's better to bring the methanol to near boiling then add it to the powder until it just barely dissolves (turns clear). Then let it cool to room temp undisturbed and then add the ice water slowly as BM described.

The other method I tried (mixing the water first) was from a testosterone synthesis patent that supposedly produced bigger cleaner crystals. Maybe they filed the patent before they tried it : )

 

[dredd09]

I found an interesting paper on extraction methods but dont know whether ibshould post it or surmise it. But it seems to give list of preffered solvents to each steroid, cortico, anabolic or otherwise.

 

[flenser]

I found an interesting paper on extraction methods but dont know whether ibshould post it or surmise it. But it seems to give list of preffered solvents to each steroid, cortico, anabolic or otherwise.

Post away! Or summarize it and include a link : )

 

[devildog93]

That would be super useful information.

 

[dredd09]

Sorry for the delay, it was my birthday, so got busy. I see from reading the other forums that at least one source is now experimenting with info gleaned from this thread, and I think that's a great thing. Ill either post up the study or summarize in a few minutes.

 

[dredd09]

This is a study involving pre purification of steroid samples before mass spec or chromatography. The info, of course , has a wider range of interest than that for those who can use it to there own end. Or for the good of others.

Steroids are hydrophobic compounds and do not dissolve
significantly in aqueous media and are thus added to the matrix dissolved in
ethanol, methanol, or other polar solvent which is miscible with water. The volume
of such a solvent should be as small as possible in comparison with the volume of
fluid used for analysis to prevent denaturation of any protein. Sometimes, the
steroid is added to a glass container, the solvent evaporated off and the fluid for
analysis added. This practice is not to be recommended since steroids, when added
in this way, can be adsorbed to the surface of the glass and may not subsequently
be dissolved in the matrix, even when the glass has been inactivated by prior
treatment with dimethyldichlorosilane. In addition, some steroids can be destroyed
when evaporated to dryness on glass surfaces, particularly when the glass has
previously been cleaned by treatment with chromic acid, a practice which used to
be common but is now no longer so.

Methods for purification vary and its good to know more than one type. Therefore...

The main drawback of
liquid–liquid extraction is emulsion formation, though centrifugation will often
overcome this situation but is time-consuming. Standing extraction tubes in dry ice
to freeze the aqueous phase is a useful way of decanting an upper organic layer.
While the modern trend has been to move away from such extractions because of
the need to restrict use of toxic and/or flammable solvents and the problems of disposal, such extractions should not be completely discarded and there may well
be situations where such procedures can still be useful.

Indeed, a recent publication
(Hill et al., 2007), describing the measurement of pregnanolones in third trimester
pregnancy plasma, used ether for extraction, freezing the aqueous phase in solid
CO2
/ethanol, and pouring off the ether layer. After evaporation to dryness, the residue
was further purified by partitioning between n-pentane: 80% methanol in water
(1:1)
Tbc later..

 

[flenser]

Ordered what I thought was ethanol (200 proof) denatured only with methanol, but I had been looking on multiple sites and got confused. I actually ordered ethanol denatured with the following:

Methyl Alcohol: 67-56-1
Methyl Isobutyl Ketone: 108-10-1
Heptane: 142-82-5
Ethyl Acetate: 1141-76-6

I guess recrystallization is out. Any other uses for this crap?

-----------------------

I also did a few straight water washes of 5g each t-e. This was mixed in 250ml room temp water with a magnetic mixer for 15 minutes, then vacuum filtered through a coffee filter and rinsed several times. I recovered on average 4.85g. I'm guessing that means there's no filler added, at least no water soluble filler. Going to continue washing as a first step before any recrystallization, in case other raws do contain fillers.

 

[dredd09]

Nice. Ya , dont use that bottle for anything chem related. Too many selective solvents. Wouldnt do ya any good . Have you tried freezing the alcohol / water layer and decanting the solvent laden goodies ?

 

[flenser]

Nice. Ya , dont use that bottle for anything chem related. Too many selective solvents. Wouldnt do ya any good . Have you tried freezing the alcohol / water layer and decanting the solvent laden goodies ?

All those solvents a miscible, you can't extract them by boiling or freezing. Don't know if they are all polar, but probably. Otherwise I could use salt to extract.

 

[Bradly]

dude, why dont you just go down to the liqour store.you have distilling apparatus right?

 

[dredd09]

Freezing with a non polar on top to extract . The chosen one for each steroid is different. This is done in labs for pre analysis purification.

 

[dredd09]

Unless yourbtalking about the mixed bottle of solvent . Agree with bradly ..if your not using methanol or isopropyl , both of which are commonly bought pure, then shouldnt be an issue to get everclear..its maybe 5 percent water..distillation or freezing could remove the significant chunk of h2o

 

[flenser]

Nice. Ya , dont use that bottle for anything chem related. Too many selective solvents. Wouldnt do ya any good . Have you tried freezing the alcohol / water layer and decanting the solvent laden goodies ?

Err, miscible liquids don't layer, they freeze at a single temperature.

 

[flenser]

Unless yourbtalking about the mixed bottle of solvent . Agree with bradly ..if your not using methanol or isopropyl , both of which are commonly bought pure, then shouldnt be an issue to get everclear..its maybe 5 percent water..distillation or freezing could remove the significant chunk of h2o

Same with boiling. You need fractional distillation to separate it, and doing that with ethanol has it's won risks : )

And damn VA laws anyway. The closest I can get at the ABC store is 100 poof.

 

[dredd09]

I meant for extraction with a non polar, such as ether. Didnt mean your bottle of ethanol.

 

[dredd09]

Id toss that. Not worth it trying to fraction those compounds. I dont know where you are but might be worth it to make a drive for some everclear or consider using methanol or isopropyl..i think iso better used for recrystallizing though if i remember right.

 

[flenser]

Id toss that. Not worth it trying to fraction those compounds. I dont know where you are but might be worth it to make a drive for some everclear or consider using methanol or isopropyl..i think iso better used for recrystallizing though if i remember right.

I have plenty of purified methanol. I just wanted a comparison. Freaking laws require poisoning ethanol to "protect" drinkers. Sheer lunacy.

 

[dredd09]

Ya you can def blame that on the meth craze. Cant even assemble good reagents for a lab anymore without a big hassle.

 

[dredd09]

Everclear is bottled at 151-proof (75.5% ABV) and 190-proof (95% ABV). Sale of the latter is prohibited in many U.S. states (California, Florida, Hawaii, Iowa, Maine, Maryland, Michigan, Massachusetts, Minnesota, Nevada, New Hampshire, North Carolina, Ohio, New York, Virginia). Kentucky then maybe?