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OfflineDadeMurphy
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Registered: 01/29/03
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mesc extraction q, about possible impurities / safety
    #3675914 - 01/25/05 03:09 AM (12 years, 30 days ago)

Hey all,

SWIM is planning a mesc extraction in the next week or so, following nan's tek. They are starting out small to test the process and then will be doing a large amount of dried peruvianus. Reagent grade sulfuric acid has been obtained for this process, some xylene (this may have to be tested for purity, the container just says "XYLENE" but doesnt describe the purity), some good quality lye (~98% NaOH), RO water and all the right glassware etc.

SWIM is lacking ammonia and norite for the last steps and is not sure what to use. They are kind of hoping to avoid some of nan's work up because it seems cumbersome to work with that black acidic solution of oxidized pigments and stuff.

So my q's:
-Can a defat of the acidic solution in the beginning avoid nan's messy work up?
-Is NaOH safe when neutralizing the wash water or will this lead to toxic sodium bisulfate (i know it's acidic/unstable in presence of strong bases) or other contams in the precipitate.
-How can I avoid unwanted sulfur compounds in the final product?
-If ammonia must be used, can household ammonia be concentrated and used?
-What are the products of the acidic water and ammonia? No one wants anyone to be injesting toxic products of acid base reactions.

TIA, any input will be appreciated, I am in chemistry so I should be able to figure this stuff out but some outside opinions are invaluable.


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Edited by DadeMurphy (01/25/05 04:06 AM)


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Offlineneuro
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Re: mesc extraction q, about possible impurities / safety [Re: DadeMurphy]
    #3676605 - 01/25/05 10:03 AM (12 years, 30 days ago)

I generally don't follow teks, instead I work on A/B theory and use appropriate solvents.

I'd use Naptha instead of xylene, xylene I've found doesn't have the solvating power as naptha.

Excess unreacted H2SO4 + NaOH --> H2O + Na(SO4)2, this should be soluble and I wouldn't worry too much about it if you have good technique and can keep track of what's where in solution, it will stay in solution at all times, and will not precipitate.

You don't need ammonia.

>>What are the products of the acidic water and ammonia? No one wants anyone to be injesting toxic products of acid base reactions.

Acidic water H+ ions, from H2SO4 would be this

H2SO4 + NH3 --> NH4(SO4)2 [ammonium sulfate)


You don't have to worry about the Sodium Sulfate [Na(SO4)2] because it's always aqueous and as a result , after I recovered my alkaloid crystals (through crystallization/precipitation NOT evaporation or you will have Na(SO4)2 + your alkaloid), I'd recrystallize after recovering and washing the crystals to be sure it's devoid of residual Na(SO4)2,

That is pour your precipitate through a vaccuum filter, wash with cold deionized water, recover the crystals and recrystallize the alkaloid crystals.


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Offlineneuro
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Re: mesc extraction q, about possible impurities / safety [Re: neuro]
    #3676636 - 01/25/05 10:13 AM (12 years, 30 days ago)

instead of NH3 use saturated Sodium Bicarb.


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OfflineDadeMurphy
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Re: mesc extraction q, about possible impurities / safety [Re: neuro]
    #3678991 - 01/25/05 07:39 PM (12 years, 29 days ago)

thanks for the input.
yeah i think i've got my head around all the work up involved now. should be a cinch, stuff ive done in the chem lab many times. Wouldn't it be nice to have all the equip of the uni lab though? Sigh...my vac. filter apparatus is going to be so ghetto....
oh well i'll post the results!
peace


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Offlinetregar
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Re: mesc extraction q, about possible impurities / safety [Re: DadeMurphy]
    #3679484 - 01/25/05 09:30 PM (12 years, 29 days ago)

Head on over to www.thenook.org and begin reading in ion's chemistry forum, all the latest on mesc can be found there.

You may have to register to see all the forums.

me! and ion and others will be more than happy to answer all your questions.

Foaf's mesc extraction read over there requires only xylene, lots of sodium hydroxide, a glass tumbler like the kind used by beer making hobbyist, distilled water, some 31% hcl, and your set.

What neuro said is true--No ammonia needed. No toxic by-products are possible, at most maybe a little table salt in your final product if your not careful following the process, harmless.

checkout "foaf's simple mescaline extraction" in the archives over there.

If you insist on using sulfuric acid, then just follow ion's tek, it's in ion's chemistry forum. Foaf's tek or Ion's tek is your best bet. Nan has been away from the nook for quite some time, mesc extraction has come a long ways since Nan left. The newer teks are really worth the look, and also, Toluene can be used in place of xylene(not as stinky) but stick with either xylene or toluene.


Edited by tregar (01/25/05 10:03 PM)


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OfflineDadeMurphy
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Re: mesc extraction q, about possible impurities / safety [Re: tregar]
    #3682608 - 01/26/05 12:37 PM (12 years, 28 days ago)

Interessant I am registering on the forums now.

Yeah HCl is safe and all that, but I figure if I have reagent grade h2so4 why not use it? I figure now that only na2so4 will probably come out of that reaction and will probably remain ionized and in solution. Then just a quick recrystallization and it should be good. Pretty handy that water works as a recrys. solvent.


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Offlineesin
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Re: mesc extraction q, about possible impurities / safety [Re: DadeMurphy]
    #3682619 - 01/26/05 12:41 PM (12 years, 28 days ago)

You can use it and will get better crystals with h2so4.

But it's not nearly as simple as salting out with HCl...


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OfflineEkstaza
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Re: mesc extraction q, about possible impurities / safety [Re: DadeMurphy]
    #3689438 - 01/27/05 06:46 PM (12 years, 27 days ago)

Try this, it's simple.

Things you'll need:
1.at least 2 glass or HDPE(should show a triangular recycle symbol with a 2 inside of it somewhere on the bottom) plastic jugs or jars. HDPE is preferred because strong lye solutions will etch glass and cause it to break eventually. I know first hand.

2. RedDevil brand lye

3. Muriatic acid (HCL or hydrochloric acid)

4. Acetone

5. Xylene

6. turkey baster

7. a glass or stainless steel funnel

8. cotton balls

all easy to get items (use NO aluminum)

You should not use any type of open flame at any point during this extraction.
Use adequite ventilation at all times.

Extracting
Prepare a solution of lye water by slowly mixing together 1 TBS of lye for every pint of cold water that you think you'll need to dissolve your tar. This will produce a little heat so don't be alarmed. Just swirl it around slowly as you add the lye a little at a time. This is what I will refer to as base or basic water.

Next add you tar. break it up if you can (anything to assist in it's dissolving). Make sure that you fully dissolve the tar as you want it all to be exposed to the base water.

Now add about a pint or so of xylene to the mix. You want enough of a layer to be able to draw off the xylene with the turkey baster later. Shake it all up and let it sit for an hour. If you can see that the xylene layer is separating back out, fine, if not, add a little more pre-made basic water and check again. Now shake it back up and put it away for 24 hours (every second of it).

24 hours later, you want to draw off the xylene so now you need to use the turkey baster to suck it up and put it in a new jar(a mason jar works fine). You don't want any of the water from beneath the xylene to come with it.

Salting
Now you want to mix your acid water in order to dilute it to the proper strength you want. Be very careful not to breath the vapors that come out of the bottle when you open it. HCL come very strong and it will burn you.

You want to add approximately 4-8 drops of HCL acid to 1 cup of water.
Slowly add this acid water to the xylene while gently swirling the liquids around in the jar. Add it all. Put the lid on the jar and shake it all up. Wait a few minutes and shake again.

Once it has returned completely to a separated state loosen the lid on the jar and place it in the freezer. You want the bottom layer(the acid water) to now freeze solid. The xylene will not freeze. Once the water is frozen, work quickly and pour the xylene back into the extraction bottle.

With the water still frozen solid, pour in a little warm water and swirl around and discard quickly. This helps get rid of a little more residual xylene. The rest will evaporate later.

Repeat the extraction and salting steps 4 to 6 times to get all of the goodies. You can reuse the xylene over and over again.

Evaporating
Now thaw out the water and put it in you evaporation dish. A large flat bottomed pyrex dish works best. Using heat(heating pad beneath the dish) or not fan dry it to evaporate the water from the dish. This may take some time depending on how much water you used.

Once all of this is dry you will see a crystalline residue left on the dish. Scrape it off with a razor blade. It will be a brownish powder. It can be used as is but the next procedure is simple if you've got this far.

Cleaning
Put a cotton ball in the spout end of your funnel so that it can filter.

Mix some acetone with your extracted alkaloids and pour it into the funnel with a clean dry jar to catch the liquids. You will notice some color draining through with the acetone. Wash like this with fresh acetone until little to no more color is draining through. Put the funnel somewhere to dry.

Once all acetone smell is gone from the funnel and it's contents you need to pour some hot water into it with it positioned over the evaporation dish. The hot water will dissolve the crystals and allow them to flow through the cotton into the dish.

Evaporate as before. The resulting crystals will be considerably whiter and more pure. This is not only for aesthetics, but also it makes for more accurate dosing.

You can put this powder in capsule to facilitate simple dosing with pre-measured amounts in each capsule. Look to www.erowid.com for dosing guidelines.


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YOUR EXPERIENCE WITH ANY GIVEN DRUG ISN'T THE DEFINITIVE MEASURE OF THE DRUGS EFFECTS.


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