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Odd result after use of dry ice (A/B, ACRB) Options
 
TxRx
#1 Posted : 2/18/2014 2:07:17 AM

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Maybe someone can check my tek for errors...

In summary, I performed an A/B extraction on 100g ACRB, using citric acid, NaOH, deiodized salt, and heptane for nps. The initial dry result was 3.5g of material, fluffy white stuff and goo. Mechanically separating the nice stuff, I opted to try dry ice to clean up what was left. I decanted the solution off some brown gunk that wouldn't dissolve easily, then treated 5x with dry ice (rewarming in between), yielding some yellowish gunky chunks. Poured the clear nps solution off into another jar and chilled in the freezer for a couple days. Instead of crystalizing, its just a sort of white sludge (a bit poached eggwhite looking). What the heck is this stuff? It was in solution when it was pouring into the jar prior to chilling, so it can't be the NMT carbamate right?

Detailed what I did:

Day 1:
- made up some acidic solution 40g anhydrous citric acid + 4L distilled water (pH ~2.2)
- Chopped bark with shears, and ground it to a coarse coffee grind level in a blender. Added 250mL acidic water and froze/thawed 15 times over the course of several days

Day 4:
- Did 4 acid boils. 1L of acid solution diluted by a half, light boil for 1:45 per boil.
- Strained contents through cheeze cloth in between boils.
- gently reduced to final volume of 750mL

Day 5:
- Slowly bassified with 80g NaOH (temp rose to 50C)
- Did 4 pulls with +30mg heptane +1-2tbsp kosher salt
- Pull procedure: 2mins agitation/swirling. ~5mins (or until separated) rest in warm water (45-55C) 10X per pull
- Collected 111g yellowish opaque nps liquid and froze overnight (-20C)

Day 6:
- Decanted nps off jar and dried 1h under fan to a weight of 3.5g
- Mechanically separated white fluffy crystals (0.5g)
- Readded nps, warmed and dissolved most of the goodies, brown sludge would not easily dissolve. Decanted nps to another jar.
- Treated with dry ice 5 times: Added 5-10g chunk, swirled the bubbling chunk to ensure saturation with bubbles, final temp ~5-15C. Warmed back to 50C in bath until most precipitates were redissolved and repeated.
- After last dry ice treatment, decanted rewarmed solution off yellow sticky gobs into another jar for chillling
- After several days in the freezer, fluffy white sludge has come out of solution, but is not crystallizing like DMT normally would.


EDIT:
Attatched photos:
1. Dried crystals from combined pulls
2. Dried crystals from combined pulls
3. Mechanically separated fluffy crystals
4. Weight of nice xtals
5. Left over goo
6. Immediately after dry ice stops bubbling, everything is out of solution
7. Warming it up, most stuff goes back into solution
8. After all dry ice treatments just yellow gobs left, clear nps poured into another jar for freezer
9. Sludge that precipitated out in the freezer, but didn't crystallize
10. Poured off sludge to another jar, only an insignificant mass of crystals seem to have formed from 3g of initial goo material
TxRx attached the following image(s):
acrb extract2.jpg (304kb) downloaded 305 time(s).
acrb extract3.jpg (366kb) downloaded 305 time(s).
acrb extract3b.jpg (303kb) downloaded 305 time(s).
acrb extract4.jpg (273kb) downloaded 306 time(s).
acrb extract5.jpg (339kb) downloaded 306 time(s).
acrb extract6.jpg (236kb) downloaded 303 time(s).
acrb extract7.jpg (253kb) downloaded 303 time(s).
acrb extract8.jpg (244kb) downloaded 302 time(s).
acrb extract9.jpg (206kb) downloaded 302 time(s).
acrb extract10.jpg (342kb) downloaded 302 time(s).
 

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starway6
#2 Posted : 2/18/2014 2:19:10 AM

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Very nice crystals!Smile
Since you used dry ice.. did it rid the acrb of the nmt.. leaving mostly dmt?
You should know when you vape it!Smile
 
TxRx
#3 Posted : 2/18/2014 2:34:57 AM

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The stuff treated with dry ice didn't seem to form any substantial crystals (see the last pic), so I'm at a bit of a loss as to what happened to it all.
 
arcologist
#4 Posted : 2/18/2014 6:02:03 PM

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Did you use heptane to do the dry ice reaction? I only tested it using xylene and naphtha, but in theory it should work the same.

I think part of the reason why there isn't a large amount of crystals after the dry ice is that a large portion of them were already removed in your first two steps of day 6, making the effect less dramatic than if you had just added the dry ice directly to the solvent from day 5.

When I have done this process my yields have been between 0.6% and 1.0% for ACRB. Most of the literature agrees that there isn't much more than 1% DMT in ACRB, and some bark may be better or worse than other bark.

Another possibility is that some of the DMT in your acacia was DMT N-oxide, which will have different (i.e. less) solubility in non polar solvents like naphtha (not sure for heptane). I did an extraction where I was only going to yield 0.5%, but then realized that almost half the DMT was oxidized (yellow goop). I used zinc metal to reduce the N-oxide to DMT, bringing my total yield to ~1%.

Another possibility is that the NMT/DMT separation was incomplete in the dry ice step. Having even a small amount of NMT in the mixture will disrupt crystal formation.

You could try redissolving the white sludge and evaporating. This might help with crystal formation.
 
mailorderdiety
#5 Posted : 2/18/2014 7:32:03 PM

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hi arcologist. really great response. i'm super curious about the zinc process. i found some that looks good where i get my lye. i'd really like to try this method. the only thing is i'm getting many different approaches for doing this on both the nexus and other sites in a google search. Could you elaborate on your zinc process. and also how does zinc effect nmt? i saw some posts by dr. sister using zinc and formaldehyde. I'm not too keen on using formaldehyde. or is the dry ice method the best method for separating nmt and dmt and simply converting dmt oxide over to dmt with zinc? sorry i know nothing about chemistry. i simply follow techs here.
 
arcologist
#6 Posted : 2/18/2014 9:08:49 PM

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mailorderdiety wrote:
hi arcologist. really great response. i'm super curious about the zinc process. i found some that looks good where i get my lye. i'd really like to try this method. the only thing is i'm getting many different approaches for doing this on both the nexus and other sites in a google search. Could you elaborate on your zinc process. and also how does zinc effect nmt? i saw some posts by dr. sister using zinc and formaldehyde. I'm not too keen on using formaldehyde. or is the dry ice method the best method for separating nmt and dmt and simply converting dmt oxide over to dmt with zinc? sorry i know nothing about chemistry. i simply follow techs here.


They are complimentary but separate techniques. Here is a description of the zinc reduction process. It needs to be pure zinc metal, not zinc oxide, etc. Formaldehyde is not necessary (that is related to converting NMT to DMT and doesn't seem to work in my experience).

Here is the original thread which describes the dry ice NMT separation. I haven't put together a comprehensive tek yet but it's on the list of things to do...
 
mailorderdiety
#7 Posted : 2/18/2014 9:38:13 PM

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thank you arcologist. i'll review both of those links carefully
 
starway6
#8 Posted : 2/18/2014 11:47:35 PM

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..arcologist..Smile
Ive asked this question before about your dry ice tek..

So ill ask it agsin about your cleaned up acrb [cleaned by dry ice] asuming you have removed the nmt leaving mostly DMT...

My question is.. is your dry ice cleaned [acrb spice] totaly free of nmt without the nmt.. same experiance to mimosa spice?

[asuming you have tryed mimosa before?]..

Does your dry ice cleaned acrb spice feel just like mimosa with its intense visuals ..fraCTALS ..BUZZING...ALIENS...AND EVERYTHING ELSE THAT YOU GET WITH SOLID dmT?

I mean dmt is dmt regardless of the sorce and experiance should be the same..

Thanks.....
 
arcologist
#9 Posted : 2/19/2014 5:29:24 PM

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starway6 wrote:
..arcologist..Smile
Ive asked this question before about your dry ice tek..

So ill ask it agsin about your cleaned up acrb [cleaned by dry ice] asuming you have removed the nmt leaving mostly DMT...

My question is.. is your dry ice cleaned [acrb spice] totaly free of nmt without the nmt.. same experiance to mimosa spice?
Thanks.....


It's exactly the same as mimosa DMT (maybe even more pure, since it has been cleaned up more). I also additionally convert the DMT to fumarate and do the zinc reduction to further purify it.
 
TxRx
#10 Posted : 2/19/2014 5:32:01 PM

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Thanks for the response arcologist.

I did use heptane for the dry ice reaction, not for any special reason but just because it's what I have handy.

On closer inspection, the 'sludge' (pic 9 original post) I got that wouldn't crystallize was a mix of slime and tiny free floating crystal flakes. (Impossible to get a pic of unfortunately)

After moving that sludge to another jar, there were a few crystals attached to the jar (pic 10 original post) These were dried and rxd at room temp ~50mg (pic 1 below) Looks like DMT

After freezing the sludge for a while I sucked off the ice cold heptane until it was all flakes. Dried. rxd at room temp to ~100mg yellowish crystals (pic 2 below)

I was not aware that free floating crystallization was a possibility!

This brings my total yield to ~0.75%. I will definitely be checking out the zinc dust option. Thanks for your input.
TxRx attached the following image(s):
rx1.jpg (224kb) downloaded 200 time(s).
rx2.jpg (223kb) downloaded 198 time(s).
 
 
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