got nothing from 100g

[sofakinold]

Hey people
I've been doing extractions for nearly 3 years. Started with a STB with poor results. Went thru some ups and downs and ended up using broken cell bark by freeze/thaw with a salted a/b with good results. Did not boil the brew after using the broken cell. Merely put the jar with acidified bark in the pot of boiling water I used to melt the salt. Was getting around 2% yield consistently. I had Hawaiian acacia confucia as whole bark that I broke up and put thru a blender. It did produce some goo which reduced when I started doing a naphtha de-fat at acid.

When that got used up I got a kilo of acacia bark powder. Yields were lower, goo was higher. The de-fat with naphtha did not improve that and seemed to be a waste of time on that bark. The crystals never formed as well and there was white stuff floating. Most of the time I could strain it with a tea strainer and get some nice crystals in the floating material. I did make Changa with the full spectrum extract that was good quality and made aya with lemon juice and citric acid from this bark that was good.

Anyway I got some better bark and stuffed that bag to the back of the pantry for a while, like a year. Continued doing extracts and improving my tec. I started filtering out all of the plant material after salting before adding my base. Got much cleaner spice with much less goo. My tec was producing consistent white crystals with some sticky in the dish. I was mostly making Changa and using low heat to melt the spice and rubbing my herbs into the dish to get up all of the extract. I really thought I had it down. After meticulously measuring and weighing everything out I got a feel for the % by the density and darkness of the Changa.

Then, after running out of fresh bark a few weeks back, I pulled that bag of old bark out again and put 100 grams in small plastic jar with water and started the broken cell process. The other night after 4 cycles I did the extraction. Put vinegar in with the bark and poured it into my reaction jar, repeated to flush the jar. Let it stand for a hour or so. Put the jar in the water to boil for the salt. Added the salt and did everything like normal. But when I filtered the plant material out of the fluid it did not have the strong DMT odor. I have been getting the odor every time since I went to filtering, on several batches of bark. So I added my lye. It got hot. Did a kind of grey then black in the jar, which is not normal, but, I did read somewhere that that can happen. Continued with 2 pulls with naphtha at temps over 120F and put it in the freezer.

The next morning there was white on the bottom of the dish and some floating white in the naphtha. When I poured the naphtha thru the tea strainer it caught nothing. I had poured it back into a jelly jar I keep in the freezer for my used naphtha. There were solid crystals on the bottom of the jelly jar from past extractions. The naphtha was cloudy in the jar. Put it back in the freezer. The white on the pyrex dish was minimal but there, so, I set it on its side under the vented stove hood with the fan on high to dry. Went for a bike ride and came back a few hours later expecting to seen some dry crystals. Nope, No crystals. Just some sticky I could smell some DMT, but not the strong smell I expect. And not enough of anything to fool with. Checked the jelly jar and the Naphtha was clear, the white had settled on the previous crystals. Some how I get the feeling when I dry out the jelly jar there is going to be sticky on my nice crystals.

So, What happened? The bark was poor at best. But I had gotten good spice and crystals from it before. Did it just get old in the pantry? I don't think I got the tec that wrong. Could it have been a temperature thing? I know the acid stage got to 200F and the base got to just over 140F with the exto-thermal reaction. The naphtha was cold when it went in the jar but should have gotten to temp. I used 90 grams of lye in a pint of fluid, that should have been plenty. But, I did not use pH paper. Since I did not smell the DMT at acid when I filtered out the plant material I have to assume it has to be the yield from the bark. The broken cell tec has been doing beautifully for me for over 2 years. I see no reason to have to boil with the salting.

Anyway, I've put another 100 grams in the freezer for broken cell again. And I will get fresh bark. If I get zip again the rest of this bag is going to the compost heap.

 

[padawan]

Sounds familiar. Layer of sticky white instead of the crystalline structures. It's not fats/oils - I've ruled that out through various means. My best guess is that some batches of acacia contain much higher % of NMT which doesn't crystallise and which traps DMT within that sticky mess. All the evidence points to this: smells right but doesn't crystallise and less visual on a mg-for-mg basis compared to the fluffy white stuff. I've been meaning to try out the dry ice carbonation method of separating NMT from DMT at the combined naphtha pulls stage - might be a worth a shot if you have the inclination.

 

[sofakinold]

I get that. I also have figured out the the blistered sticky carries some of the DMT and was primarily NMT. Still it is a pain to remove and makes the crystals difficult to handle. Best reason to make Changa from the full spectrum extract. Besides I like the effectiveness and control you have with the Changa.

It does not answer where the DMT went. 100 grams of bark at even 1% should have given me a gram of spice. My best guess is that the DMT has become oxidized or some other degradation. I do not know what would alter the chemistry to prevent it from being extracted. Or if oxidated N N-DMT comes across in the extraction. So, anyone know the chemistry? Is there a means to make it worth recovery? Decarboxylation?

 

[AcaciaConfusedYah]

Hello,

Welcome to the nexus. It's a good idea to edit the original post to remove mention of bark purchase. It's in the Nexus Attitude not to mention any discussion of vendors or purchasing bark. The information about the timeline of barks likely is not the extraction issue. If a mod sees it, they'll just edit it anyways.


Generally speaking, DMT stores very well in bark. Some people have been doing extractions on bark they've had for 10 years. I do not think oxidation is your source of loss, as oxidized DMT will be extracted with freebase DMT. In the bark, the DMT is likely in a salt form - probably DMT tannate.

How much NaOH did you use? Too much, and I find that to be more troublesome than "not enough." In a liter of water, 100 grams of bark should require the same amount of NaOH as 50 grams of bark. Some people don't really understand the concept of pH, so they think NaOH should be scaled to the amount of bark. Unfortunately, this is a common practice and very wasteful. Not only that, but excess NaOH will increase viscosity of the aqueous layer and make separation more difficult while decreasing surface area exposure.

A liter of water should not need much more than 10 - 15 grams of NaOH --- pending how much acid you used. Most people think the idea is to apply chemicals as they would an insect spray- "I don't know if it is dead yet. It stopped moving 4 minutes ago, but i'm gonna finish unloading this full can of raid, just in case..." Again, pH is very misunderstood by most kitchen khemists. And then who writes most the teks that are shared on the web? The ones who don't know why they are doing it - but read it somewhere... so it's just regurgitated and repeated.

Another thing - i, personally, never found much value in adding NaCl to an extraction, considering that NaOH (in excess - per most people's practice) will be in a very high concentration. The Na+ ions from the NaOH should be plenty. And, again, more suc stuff = increased viscosity = extractions are more difficult than understanding the concepts and optimizing rather than regurgitate.

I realize that my comments kinda "call out" the folks who had been writing and rewriting teks long before I knew what DMT was. However, if they are offended - I encourage them to look into my comments and decide if 50 grams of NaOH is considered "efficient" or meets the ideal of: use less, get more.


Here:

Hey there!

This is a topic that i've been inclined to address, lately. I made a post on another thread. For ease, i'm going to quote myself:

Lack of considering new approaches leads to stagnation. In three - four years, I think that most teks will be adjusted to add IMPROVED quantitative amounts of material and reagents. For example: the claim that adding more NaOH is going to help break an emulsion. Actually... maybe not. As more NaOH is added to the solution, viscosity increases and will make it MORE difficult for separation.

Also, the amount of NaOH suggested, in the popular teks, is absurd! Even in 1 liter of water, way overkill and wasteful. I understand why people have written them as such - most won't take the time to bother monitoring pH though out the process. I think the authors assume most people will read [half of] the tek and just start dumping chems in. And... that's happened. Lol.

But, pH and pOH have a logarithmic relationship with concentration (molarity). One mol of NaOH is roughly 40 grams. Ok, cool - molarity is determined by dividing the amount of NaOH (mols) by the volume of the solution (liters). So, let's say you use a mol of NaOH (~40 grams) and one liter of total solution: 1 mol / 1 Liter = 1 mol/L (this is a solution that has a concentration of 1 M (Molarity).

pH or pOH can be related as: pOH = -log(OH); pH = -log(H); and pOH = -log(1 M NaOH) = 0... but, pH and pOH are complimentary. The pH = (14 - pOH) = (14 - 0) = 14.

The concentration needed to achieve a specific pOH or pH can be as followed:
[H] = 10^-(pH) ; and [OH] = 10^-(pOH)....

So, let's assume you want a pH of 13. (A.k.a. pOH of 1)

[H]= 10^-(13) = 1.0x10^−13 M ; [OH] = 10^-(1) = 0.1 M.

Ok, so we need 0.1 M solution of NaOH. So M = (mol/L) ; then (M)(L) = mol.

We know that the volume is 1 L. We know the molarity is 0.1 M, so (0.1 M)(1 L) = 0.1 mols.

NaOH has a M.W. of ~40 grams/mol. So, 40 (g/mol) * 0.1 (mol) =....... wait for it..... wait for it.... 4 grams.

People have been adding 50 grams!!!!!! That's 10x more than theoretically needed. I decided to test the theory - you can see the results here. (Also, I never updated the final results - I performed a second pull - smashing the old yield percent of ~1.4 %..... we're well over 2 %, now.... 2 pulls, ~ 10 grams of NaOH)

Why are the teks designed with such inefficiency and wastefulness?" If you even used 10 grams of NaOH, you'd be fine. So, my theory is that most people DO read and repeat (or try, lol). Only a few ask why.

Take care,
ACY

P.S. - if any of the above seems like alien language, just ask. I'll try to simplify it if I can, but I think it would be most rewarding to dig into the topic and learn what the explanation means, rather than the simple answer.

 

[sofakinold]

So, for volumes;

I start with an 8 oz plastic jar with 100 grams of powdered bark. Add disilled water and shake, let stand and add water till it is no longer thick. That generally is a full jar. (with 50 grams that is just over half) Do at least 3 freeze/thaw cycle with stand times to allow full absorption to make the broken cell. (this time it was 4 cycles)
I shake and add some vinegar, then pour it into my reaction jar. (8 oz) Then put another 4 oz of vinegar into the plastic jar, shake and pour, to remove more of the bark. Repeat if necessary. Then add vinegar to at least 20 oz in the jar.

Starting with 8 oz of distilled water in a pan to boil for dissolving the non-iodised salt. Add it to the reaction jar. There is then room for lye and solvent. But I did a complete filtration of the plant material that left only 1 pint in the reaction jar.

I have found this tec to be very efficient at removing a high % of alkaloids from the plant material. And several times tried to get more out of the spent material by basifying and boiling with no results.

As far as the amount of lye. I have generally used equal parts to bark weight and have gotten pH above 14. With only 1 pint of fluid I saw that as overkill but went with 90 grams.

 

[AcaciaConfusedYah]

Well, if you find the method to be efficient (for you) I guess just keep trying. We all do things a little differently. I prefer to let nature and a little technology do the work for me... tannins from the bark, magnetic stirrer/hot plate, pH monitor (or paper), about 10 grams of NaOH, 250 mL of solvent and .... oh, wait... that's all. I don't bother lysing the cells via freeze/thaw - the tannic acid and stirring does that for me. I just have to turn on a switch.

The stirring and heat release the tannins and lyse the cells. Over a short period of time, the mix naturally drops to a pH of 3 (prefect!) and then titrated with a solution of NaOH to maintain a pH of (just above 13)... one single pull +1.4 % yield... second pull (same solvent from the first, just reused) and then I'm retrieving well over 2% yield DMT. Only 2 pulls...

I was really only there to add things and remove things. I let stirring, contact time, surface area exposure, and realistic quantities do all the work for me.

I got the bark in 2015. No loss in potency.

I'm thinking you might have degraded some of the DMT with the massive amount of NaOH. Please, read the text that I quoted and ask questions if you need further explanation of any part. I don't mind helping. However, i strive for certain goals - low quantities of reagents, optimization, time efficency, less manual work, reclaiming solvents after you precipitate DMT and minimizing the process that leads to fats/oils making it to the organic solvent (naphtha).

I understand acacia confusa is a different creature than mimosa hostilis, and it can be tricky to isolate the fats/oils.

I have published one of my first attempts at improving acacia confusa extraction - though I would like to rewrite the procedure to include more accuracy and emphasize safety.
If you're interested in how I got beautiful, large, white crystals from ACRB, let me know and Ill dig up the link. Is called "The MAD Tek" --- MAD = Microwave Assisted Drytek.

The yield from the MAD tek was average - 1.5 - 1.0%. However, the "Low-Lye" approach has been much more fruitful in yield and building my understanding of optimizing procedures.

I will never NOT use the "Low-Lye" approach when handling MHRB (unless we find something more simple... but, it literally takes about a total of 30 minutes of effort though the whole thing. The total time is irrelevant, because nature and technology do the hard work for me.

For ACRB, I use an improved version of the "MAD Tek." But, i dont extract ACRB anymore. If I am going to use ACRB, I'll save it for some oral DMT adventures.


Take Care!
ACY

(In the uploads, those are pics from the ACRB that was extracted via MAD Tek.) link to post with pics

 

[sofakinold]

I think I found my DMT

I had put another 100 grams in for freeze/thaw. After the third thaw today I went ahead and did the extraction. Put the broken cell bark and 8 oz of vinegar in the double boiler on low for an hour, stirring regularly. Transferred it to the reaction jar and melted the salt in distilled water. Then added the hot salt water and shook it up every few mins for a half hour. Filtered all of the plant material as normal. And slowly added the lye. Perfectly normal.

When I went to get the naphtha jar from the freezer it was much whiter than it had been. When I poured the naphtha into the reaction jar I noticed the sides of the jar was coated with clumps of white crystal and the white stuff was no longer floating. It had become fluffy crystals on the bottom of the jar and it was rather thick. So I guess the DMT was in the naphtha all along. The sticky NMT was on the bottom of the dish that I had washed away as not worthy. Oh well that's life.

 

[AcaciaConfusedYah]

I think I found my DMT


When I went to get the naphtha jar from the freezer it was much whiter than it had been. When I poured the naphtha into the reaction jar I noticed the sides of the jar was coated with clumps of white crystal and the white stuff was no longer floating. It had become fluffy crystals on the bottom of the jar and it was rather thick. So I guess the DMT was in the naphtha all along. The sticky NMT was on the bottom of the dish that I had washed away as not worthy. Oh well that's life.

Hey! That's great news! I mean, I'm sorry to hear of the minor loss, but now you know how to approach the situation if it ever happens again.

What kind of precipitation dish/jar are you using? Sometimes a jar can make it difficult to retrieve the alkaloids. I tend to favor a pyrex baking dish for precipitation. Everyone will likely have a slightly different approach. I like the pyrex baking dish because it's got a large portion that is flat, and the curves are gentle. This makes it much easier for scraping and collecting the alkaloids.

That NMT is a tricky beast! Have you tried a defat on the back end of the extaction, rather than the start? Some people call it "back-salting" or a "mini A/B."

It's super easy and I find it to be much less hassle than the defatting the bark, itself. If you hadn't given it a shot - it might be worth taking a look.

In simple terms - do which ever method you feel comfortable with. If I'm planning to back-salt the DMT, then I'll usually just start with a STB and skip the addition of an acid. So, let's just assume that you did which ever method you prefer and you've got naphtha with DMT plus plant fats/oils. Make an acidic solution with the preferred acid (I like citric acid - cheap and no odor.) After the pH is about 3, then add the solvent to the water and shake it really well, numerous times, followed by separation. The intermolecular interactions cause the DMT freebase to convert to a DMT salt (DMT citrate or maybe DMT acetate if vinegar is used) and transfer from the organic layer to the aqueous layer. The oils and fats remain trapped in the organic layer. Decant one of the layers (I prefer to siphon the aqueous layer, from underneath the organic layer, using 1/8th inch inner diameter tubing that is sold for ice makers.)

[Cut about 3-4 feet of tubing. I like to have a small valve to control flow, but it can be done without. To start siphon, don't suck on it... we're not siphoning gasoline! Hehe, jk. So, take the ice maker tubing to the sink and "prefill" the tube with water. After the tube is filled, apply a finger to each open end of the tubing. This traps the water in the tube. Due to cohesion and adhesion, the water and tubing have a capillary effect and you won't have to worry about the water "falling out" of the tube when you remove your finger from one end of the tube and insert it into the jar. Once in place, make sure the other end of the tube is lower than the jar, and remove your other finger/open the valve. The aqueous layer should be easily siphoned from underneath the organic layer - gravity working in your favor.]

After separated, add enough NaOH to bring the pH to 13, and then treat it like a normal extraction.

Take Care!
ACY