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Recipe help

Smokeit77

Rising Star
So bro is new to the self extraction cookout. Tried once a few years ago with little success. Mostly due to little faith and some personal issues but the crystals that came out didn't give any breakthrough. Had 1kg of MHRB and only used 50g to test a mars a/b tek but didn't have patience or nerve to try a decent amount although it was done right to a degree because you can't miss that flavor. Someone threw away the rest so it didn't go any farther.

Fast forward a few years and found another kg of mhrb but this time was different. Read a bunch of recipes for a/b mars, volvin and cybs' hybrid and worked out the best path to test 50g of powdered bark. Used muriatic acid instead of vinegar and got the PH down to 2. Used White Sea salt flakes, and then based with lye. keeping track of the amounts carefully, it was:
50g bark
300ml distilled water with a few drops of acid and ph of 2
Heated and let sit for an hour
35g salt dissolved in 100ml distilled water and added to the mix. stir for a while
50g lye added to 200ml cold distilled water and added to mix while hot.
Added another 100ml of water, shook it up and back in the heat for another hour or so.
Added 50ml VPN and rolled it for a few minutes then let it settle in heat bath. Repeated this about 4-5 times.
Pulled and put aside. Repeated. this 3x and put dish with 150ml vpn in freezer. FYI some where between the 1st and 2nd pull a separator flask arrived with some metal funnels and had to strain out the powder through some cheese cloth.
Pulled a 4th time and put in separate dish and into freezer (as a test to make sure nothing left to pull).

Immediate success - within a few hours plumes of crystals all over main dish. Not much of anything in 4 pull.

Only issue is. that VPN was super yellow- assumed from all the heat so let dish sit 24-48 hours and separated VPN.
Re-x'd in 4th pull VPN since in was mainly empty and put original VPN aside to use for another day. Still product came
out yellow so did a water was and re-x'd again this time leaving all the oils and heavy orange and came back with about
.5g of fine white/off white crystals. Preciped the oil dish and got another .5 of yellow. It dried no problem

Tested white and it had potential but it felt like not enough to get through.
Tested a heavier handed white topped with a little yellow for flavor and blast off. Game on and it's good. Actually like the 80/20 or 70/30 white/yellow mix and it's a little heavy but no cough and gives a. nice clean rid.

So now everyone's a pro and who needs a recipe right. Let's double it to have some but beakers are maxed a 1l so we'll almost double it and wing it - genius...

Tried about 85g mhrb with about 400ml distilled water and some acid. Slipped and PH as a little below 1 so added some more water back. Added in about 55g of pink Himalayan salt and about 200ml of distilled water but all the while trying not to use any heat. Let it sit for a while. Note: this was good quality salt but have no way to tell of it was truly pink or colored and what other sand/minerals were in with it but it dissolved and left behind a tinted mirky mix that visibly fogged up the acid soup but most should filter out with the mhrb power...
So now beaker is close to full of acidified mhrb soup and no room for base ingredients. Dump half in a mason jar for later and get back to work on the soup that's left. Fyi - strained out power before basifying this time.
After mixing for an hour or so, added 50g of lye to 100ml distilled water and mixed it up. Dumped in and soup went black...
Stirred around for an ahour or two and started adding VPN. 100ml pull twice and into the freezer. A 3rd pull to see if anything got missed and we off.

So last time the precip in the freezer was 150ml of VPN that covered 3 pulls.
Now it's 100ml per pull. The VPN still yellowed but not as much as the heated but was far from clear. Still, results couldn't be more different.
The first pull looked promising . Crystalizing although smaller and sparser. VPN with a milky haze in it.
2nd pull - let promising - minor crystal specs but hazy VPN.
3rd pull - nothing but some haze in the colored vpn but not the white milky flow suspended in the others.

Losing patience and thinking some serious evaporation should help things move along - stop the freeze, fan off the VPN plates to get rid of 75% of what's there and put them back in the freeze. What's left becomes an orangey goo looking substance mixed with some minor crystals that does solidify when dry. Turned into about 1.4g of what looked like the yellow spice from the first pull with the right scent. Very curious to see what a was and a re-x will do to it. Just not sure if it's tainted, a bad cook from be too nonchalant with the receipt or just what it supposed to be because of the quantity/ratio of ingredients used because it's the 3rd pull that's the headache.

3rd pull had no crystals, no milkyness but a haze in it that settled also like a dirty pull. Evaped and looked like some orangey residue coating the base of the dish. No worries - just dry, scrape and clean...Wrong...- it condensed and settled to looks like that orange thing that's sometimes floating among the crystals but a whole dish of just that. Problem is that after 2-3 days, it condensed but won't solidify. Spread it out thin and it looks like it dried after a while but go to scrape it up and it's just as oily as when it first evaporated. So waiting for this was holding up the other wash and re-x but now it seems this stuff is unusable but what is it. Doesn't have the aroma of spice nor the odor of VPN and behalves like pure oil. Is there anything to this or garbage?

Anyone with any info or suggestions/similar experience, please tell what this is and what's best to do with it. Hope there's no issue with the rest. Sure something has to come off of it to get the color out but it's a heavy start, 1.4g from about 44g of bark is close to 3%. Lets see what happens...
 
As far as yellow oil, here's an old post that includes some info you might find interesting:


This is by far the most ambiguous fraction that comes out of the xylene/toluene pull. Some of the yellow oils that have been isolated from Mimosa have been speculated to be plant fats and oils; another fraction of yellow oil is suspected of being an oxidation product of DMT.9,12,16,24 When spice is extracted with xylene/toluene or diethyl ether (without using naphtha first), it also tends to come out with a bright yellow-orange discoloration.13,15,17,24,28 The most substantial evidence that there is more than one compound in the yellow oil is the ambiguous solubility of the material. Yellow oil is separated from jungle spice based on its solubility in naphtha, while at the same time a yellow oil can be removed from DMT (extracted by standard straight-to-base methods) based on it's insolubility in hot naphtha. Clearly these must be different yellow oils.

To further complicate the issue, it's very difficult to isolate the yellow oil on its own. This is evidenced by the fact that many people doing otherwise normal extractions report obtaining a yellow-colored product when the naphtha pulls are done heated.9,16,24 These yellow crystals are sometimes reported to be qualitatively better in terms of effects than pure DMT.16,28,32 Also, when washing the crude jungle spice extract with warm naphtha, some extractors report that any N,N-DMT they recover from this process is strongly yellow-colored, and that this pigment seems impossible to remove by typical purification methods. Unfortunately I haven't been able to find any experience reports specifically using such yellow-stained DMT.17,24

Investigating the possibility of the yellow oil being DMT N-Oxide, I found a 2005 paper reporting the isolation of this compound from a methanol extract of Acacia confusa, but it contained no description of the physically observable characteristics of the compound (such as color), only the measured NMR data.3 This is only useful in that someone with access to proton NMR spectroscopy who obtains a sample of yellow "oxidized" DMT could use this information to conclusively establish the identity of this material. One home extractor who did some TLC analysis on whole and purified extracts of Mimosa root bark described DMT N-oxide as a yellow oil, though I can't corroborate this decription in the published literature.12 On a related note, one home extractor has discovered a method for reliably converting bright white spice into a yellow oil (without using any synthetic reagents); the nature of the process indicates that the yellow oil it isolates is in fact an oxidized derivative of DMT (see III.4 Delafonze19's Preparation of Yellow Spice Oil).32

Looking at the Radio879's LC-MS of a crude xylene pull of jungle spice reveals a peak at 205.1 m/z, which corresponds to the expected molecular ion of DMT N-Oxide, so it seems like a pretty good bet that this chemical is generated as a side-product of the extraction process.19 It may exist in the bark as a trace component (there is a barely perceptible peak at 205.1 m/z in the Vepsäläinen paper reporting the characterization of yuremamine), though it's possible this trace peak was an artifact of the isolation process as well.8 It's also possible that the sample analyzed in the paper was from a different subspecies, or even an entirely different Mimosa species than is typically purchased as root bark (see V. Botanical Confustication)19,29

I don't think you have to focus on the acid ph so much or use pink sea salt, but I'm not very familiar with the method you're using. 3% yield sounds great and you could do different clean up methods if you like, so whatever is up with the oil may not really matter all that much?
 
So trying a water wash and re-x'd twice to remove some gunk and separated the results into .8g of yellow spice and .5g of cleaner looking spice. A little surprised that these weights are still over 1g. Acceptable since it was able to pull a little oily gunk out of it and had that original oily gunk put aside so probably safe to say it's pretty clean. Tried another small pull just to see if anything was missing and it was empty. Could probably do another water wash on the yellow spice and see what happens but think a test run is in order first. Would like to try the cleaner spice and then a salad mix to see what's there.

FYI - running the first pull on the other half that was left from last time ( a little more carefully and with more attention to detail) = so far results look promising...
 
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