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VisualAnemia
#1 Posted : 12/27/2011 10:07:32 PM

Chalgren


Posts: 225
Joined: 14-Sep-2011
Last visit: 23-Aug-2014
Location: Limbus
Hey all, I've been experimenting with different extraction techniques recently and found most of them successful regarding the yield and quality of the final product.

Using different H2O-MHRB-NaOH ratios and methods of processing the extraction I've ended up with quite similar results, however my latest and on-going extraction seems to have a shot at the #1 technique atm from eyeballing its probable yield and quality but time will tell.

I began using a simple yet effective extraction technique taught by David Barlow but after awhile I realized there had to be a better (more efficient) way and I began seeing some controversy in the theory's logic. Such as; If initial pulls are done with heptane, which is a more selective solvent than naphtha, the expected yield is estimated to be 2/3 less than that of an initial naphtha extraction.

The question reveals itself..; does initial heptane pulls affect the total yield or solely that of the individual pulls? As this would probably require more pulls with the heptane than with the naphtha in order to retrieve all of the DMT. Or, with heptane being more selective, does this mean that it simply pulls fewer impurities than naphtha and therefore a smaller yet significantly purer product?

I've used naphtha once and it yielded some ugly, waxy and yellow stuff I didn't want anything to do with it. So I went straight to heptane and voilá, off-white dense flakes with some cute powdery offspring. I did the math and the yield was about .4-.5%.

After some "testing" I was extremely satisfied with the quality, the weight accurately represented the suggested effects on various dosage charts out on the web. After my first 30mg dose I couldn’t even fathom to exceed that dosage, it was so reliable in strength and effects I was quite afraid of what 50mg would be like.

Back to the topic,
My previous extractions have been using a MHRB-NaOH-H2O ratio of 20g-5g-200ml until now, on my current extraction I attempted an increase in the NaOH to MHRB ratio; 1-1-15ml. The reason for this is entirely experimental and so far there's been two huge differences already, after vigorously shaking the 5L HDPE deionized water jug the solvents mixed together nicely and after as little as 5 minutes of heating in a warm bath, the emulsion had cleared.

This allowed the process to speed up significantly and I began siphoning of the heptane into a smaller container for further and more precise decantation. While doing this, I could clearly see small flakes of DMT scramble around in the glass pipette since the solvent was warmed and the pipette cool it quickly went opaque.

Second difference and improvement; After 1 hour of storing the solvent in a glass jar in the freezer a huge amount of DMT had already begin to fall out, this extraction was made with 250g MHRB and mixed with the previously mentioned ratio.

The process of this extraction has so far been:
1. Mix the NaOH with H2O slowly because of rapid increase in temperature
2. Shake the mix thoroughly to break up lumps of NaOH and allow it to completely dissolve.
3. Add the MHRB when the container has cooled from the reaction.
4. Add nonpolar solvent and shake vigorously for at least a minute
5. Allow any emulsion to clear alternatively put the container on a softly shaking surface and gently heat it. Warm water bath is a good choice for this as it will heat and cause slight movement which helps with removing the emulsion.
6. Decant liquid, if necessary (difficulties to separate layers) move the nonpolar solvent with some of the aquaes layer into a smaller bottle, making the separation easier.
7. Let the nonpolar solvent evaporate to at least 50% of its original volume in order to allow better precipitation on step 8.
8. Put the jar containing the nonpolar solvent in a freezer; beware of the fumes and the risk of contaminating other products in the freezer. Leave in freezer until the DMT has precipitated out on the bottom or/and no more precipitation falls out.
9. Reuse the nonpolar solvent and repeat steps 4, 5, 6 and 8. Until no more DMT is falling out of the FP.
10. Although I advocate NO use of any substance, I do advocate a responsible, respectful, spiritual and scientific approach toward this specific medicine considering its long history of use as a panacea by our ancestors. Yes, deep stuff.


Updating the topic with pictures ASAP.

Cheers

Edit/Update

Observing my second although first with Heptane yellowish product, however except its discoloration it does look good, will perhaps clean it up after I've weighed it.

Keepin' yall posted Smile

VisualAnemia attached the following image(s):
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olss 083.JPG (510kb) downloaded 837 time(s).
Mad, bad and dangerous to know.

There's magic out there!
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
VisualAnemia
#2 Posted : 12/27/2011 11:00:31 PM

Chalgren


Posts: 225
Joined: 14-Sep-2011
Last visit: 23-Aug-2014
Location: Limbus
Alright, first bump in the road!

Happened to place the jar in the lowest section of the freezer resulting in a inadequate temperature making the crystals float -.- Moved it up to the top, well I actually tossed the ice forms from the top, what MAN needs ice in his drinks anyway, right.

Some of the crystals seems to have dropped down, sticking to the bottom as I want them to.

However, if this progress doesn't continue but still ends up with alot of floaters I'll probably take out the jar for some further evaporation as I believe this might help the crystals to further precipitate and have a easier time settling down to the bottom.

Any suggestion on how I can sink these floaters to stick to the bottom? The floaters would probably get sucked up by the pipette during the move back over to the jug with the aqueous NaOH mix Mad

Have encountered this mishap once before and it magically resolved itself and I have no idea on how or why, so as long as divine intervention doesn't take place I'm in for some brand new extraction problem but with eager ENTHUSIASM TO SOLVE IT!
Mad, bad and dangerous to know.

There's magic out there!
 
Vodsel
#3 Posted : 12/27/2011 11:20:09 PM

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I wouldn't worry much about the floaters, you can always use a coffee filter to pour the solvent through, then leave the filter dry if some crystals get caught in it.
 
VisualAnemia
#4 Posted : 12/28/2011 12:18:18 AM

Chalgren


Posts: 225
Joined: 14-Sep-2011
Last visit: 23-Aug-2014
Location: Limbus
Vodsel wrote:
I wouldn't worry much about the floaters, you can always use a coffee filter to pour the solvent through, then leave the filter dry if some crystals get caught in it.


Wow, wont drying a product soaked in heptane mess up a coffe filter pretty badly? :/ It burns through rubber for gods sake Very happy

If not, I suppose I could give it a try, although I dont like the idea I suppose it's worth a shot.
Mad, bad and dangerous to know.

There's magic out there!
 
VisualAnemia
#5 Posted : 12/28/2011 12:28:59 PM

Chalgren


Posts: 225
Joined: 14-Sep-2011
Last visit: 23-Aug-2014
Location: Limbus
Latest update; I managed to avoid sucking up the floaters during decantation through crampingly-slow suction and tilting, now my whole body is aching.

Took a sniff and couldn't smell any traces of any residues from the solvent, reeked of good ol' DMT.

Weighed it up and was satisfied with results.

First batch, 250g prepowdered MHRB.

1st Pull: 1499mgs of DMT

Current Yield: .5996 = ~0.6%

For some reason my solvent was discolored early on during the DMT-shuffle stage, I assume it's because I heated it to much or for too long resulting in some plant fats and oils being pulled together with the DMT which consequently resulted in causing discoloration to the final product.

Because of the so-far high yield I'm considering purifying the current product with a heptane re-x since any impurities both fiddle with the weight/total yield and quality of the product. Less is more.

Whatever my final yield may be I'm looking forward to a HAPPY new years eve when all the annoying people has gone home to increase their already insanely high inebriation and I get to be left in solitude, atlast Smile
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Mad, bad and dangerous to know.

There's magic out there!
 
DoingKermit
#6 Posted : 12/28/2011 1:49:34 PM

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To be honest, I have only ever gotten good results using naphtha. I can't get heptane in my country very easily and it seems really expensive to buy in the US. I only ever get white/slight yellow using naphtha with an A/B extraction.

Why not just pull all the goods with naphtha (getting at least 1%) then cleaning it up afterwards with heptane if need be? Sounds like you want to recrystallize some of the spice you pulled with heptane anyways. Just a suggestion on how to save on costs.

Happy travels Smile
 
VisualAnemia
#7 Posted : 12/28/2011 4:10:48 PM

Chalgren


Posts: 225
Joined: 14-Sep-2011
Last visit: 23-Aug-2014
Location: Limbus
DoingKermit wrote:
Just a suggestion on how to save on costs.


Luckily regarding this matter, money is no object.

I most recently tried the product with 30mg and was rather disappointed with the quality, for correct measurements regarding dosing a re-x is a must and will be done ASAP.

Overall it was good with no adverse side-effects, so even though the quality wasn't as expected the purity sure holds its standards with a hint of fresh fruit and a smooth finish Pleased

By judging from the effects the 30mg represented the usual effects experienced by a 20mg dose and considering the circumstances of the extraction with the early discoloration I guess I had it coming.

This will however be my first re-x as I aim to achieve a purer product whereas the dosage charts stand correct as with my previous extractions.

Second pull is in the freezer and theres already some (1h after putting it in) DMT falling out of the solvent, although considerably less than the first pull, I'd say 75% less, estimating a total yield of .7-.8%.

This hypothesis would also show a .2-.3% increased yield since the last extraction I made although of significantly lower quality and because of this I still stand by Quality > Yield.
Mad, bad and dangerous to know.

There's magic out there!
 
VisualAnemia
#8 Posted : 12/29/2011 3:18:57 PM

Chalgren


Posts: 225
Joined: 14-Sep-2011
Last visit: 23-Aug-2014
Location: Limbus
I must have made an error while weighing the previous dose.
This time I removed the paper I used as a bowl and simply put the spice right into the scale's own built-in bowl.

The scale hit 47mg and seemed to be balanced without any mg's jumping up or down.

Since this is about extractions I will give a link to the experience which this amount yielded.
From yesterday night I still feel partially destroyed and reborn.

More if this in the link I will be putting up ASAP. However the previous 30mg dosage was either correct and I must've simply gotten accustomed to 30mg experiences as I've done many of them by now OR it was a simple malfunction giving me a false number.

The 47mg dose was EVERYTHING I could POSSIBLY think of plus so so so much more Smile

In summary: The product is great, as usual Pleased
Mad, bad and dangerous to know.

There's magic out there!
 
VisualAnemia
#9 Posted : 1/6/2012 4:28:30 PM

Chalgren


Posts: 225
Joined: 14-Sep-2011
Last visit: 23-Aug-2014
Location: Limbus
I'm been slacking with keeping this topic alive quite alot recently, my apologies.

The final and second pull resulted in 650mg of DMT from the first 250g batch.

My choice to discontinue any additional pulls was because of the jugs seemingly worsening condition, it looked as if it had begin to thin out on its weak spots and therefore rendering it inappropriate for any further use.

Total of first batch: 250g MHRB - 2150mg DMT.
Percentage of yield: 0.86%

The product itself is good and reliable (completely dried out), the smoke is smooth and somewhat fruity Smile

Will proceed with extracting my 2nd 250g batch in a month or so, 2g~DMT lasts for somewhile Cool
Mad, bad and dangerous to know.

There's magic out there!
 
fidget
#10 Posted : 1/10/2012 7:41:26 PM
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Location: Under the carpet
Evisceratechuck wrote:

The process of this extraction has so far been:
1. Mix the NaOH with H2O slowly because of rapid increase in temperature
2. Shake the mix thoroughly to break up lumps of NaOH and allow it to completely dissolve.
3. Add the MHRB when the container has cooled from the reaction.
4. Shake vigorously for at least a minute
5. Allow any emulsion to clear alternatively put the container on a softly shaking surface and gently heat it. Warm water bath is a good choice for this as it will heat and cause slight movement which helps with removing the emulsion.
6. Decant liquid, if necessary (difficulties to separate layers) move the solvent with some of the aquaes layer into a smaller bottle, making the separation easier.
7. Let the solvent evaporate to at least 50% of its original volume in order to allow better precipitation on step 8.
8. Put the jar containing the solvent in a freezer; beware of the fumes and the risk of contaminating other products in the freezer. Leave in freezer until the DMT has precipitated out on the bottom or/and no more precipitation falls out.
9. Reuse the solvent and repeat steps 4, 5, 6 and 8. Until no more DMT is falling out of the FP.
10. Although I advocate NO use of any substance, I do advocate a responsible, respectful, spiritual and scientific approach toward this specific medicine considering its long history of use as a panacea by our ancestors. Yes, deep stuff.




There seems to be a missing step, of adding the heptane (or whatever solven) ??

All of my posts are generated by CrapChatBot_V2.012a. No real parson is associated with any of the content which may be spontaneously created.
 
VisualAnemia
#11 Posted : 1/11/2012 12:34:03 AM

Chalgren


Posts: 225
Joined: 14-Sep-2011
Last visit: 23-Aug-2014
Location: Limbus
fidget wrote:


There seems to be a missing step, of adding the heptane (or whatever solven) ??



Thanks for pointing that out! FIXED. Very happy
Mad, bad and dangerous to know.

There's magic out there!
 
Merkaba188
#12 Posted : 2/14/2012 6:26:26 PM
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I have had some of the exact same concerns as yourself, Evisceratechuck. I also have easy access to both heptane and naptha, and wondered what would be best to use as the NP solvent. After multiple experiments, to my surprise, I actually found that naptha is the way to go. The reason you are getting such poor results with naptha is also a concern I once had, I had the exact same problem with unpure waxy garbage. But there is a solution.

If you think your way is best keep doing it the way you do, but since you say money is no object, please just give my way a try at least once.

What you should try doing is using naptha as your NP solvent, but DO NOT use heat during the extraction. I know this sounds backwards, but heating actually creates more problems than it solves. When mixing the naptha with the base solution, don't shake it vigorously, just roll it around slowly to avoid emulsions. As long as the naptha mixes into the solution for a short amount of time with no visible separation, it WILL pull enough DMT to the NP without the need of heavy agitation. Because of the fact that you did not shake it there will be no emulsion, and no need for heating the jug before or during pulls. Even without heat the separation process should not take very long, maybe 10 minutes at the max. If an emulsion does form, pour table salt into the jug and it will break down the bubbles at the top and wait a little longer. If there is still an emulsion, add some more NaOH and use a glass rod to slowly stir and break up the emulsion. Though, this should not come into effect as long as you roll the jug instead of shaking.

Another concern I had about using no heat was the possibility of getting a smaller yield. I found that using heat during the extraction does add a small percentage to the yield, however most of the extra weight is oil and tannins, stuff we don't want in the solution. The small increase of yield from heating is not worth an impure product.

You can get that extra percentage of yield in other ways than heating. I usually do a pound of bark at a time, and doing 4 large sized pulls of naptha is the way to go. I do 4 pulls right after another with fresh naptha, and combine all 4 pulls together in one glass dish instead of freeze precipitating each pull separately and re-using the solvent. This will give you a consistent product instead of 3 or 4 different purities. Because of the fact that you used 4 large pulls, you want to evaporate quite a bit before putting in the freezer. I don't make an exact measurement, but I usually eyeball the 4 combined pulls and evap down 50-75%. You now only have to freeze precip one glass dish instead of 3 or 4 separate evaps.

By the way, try to acquire a flat glass baking dish (like a casserole dish) and use that to combine pulls and freeze in. This will work better than jars do to evap down to 50-75%, and all of the product will freeze to the bottom of the dish. There will be no floating crystals and no need to filter the naptha. You can simply cut a hole or lift up one corner of the saran wrap you covered it with and pour off the naptha, leaving you with nice crystals to scrape off the bottom of the dish. Make sure to pour off the naptha quickly after removing from the freezer, and after pouring off ALL naptha quickly replace the saran wrap around the corner you lifted up and let the dish come to room temperature before removing the wrap to let the remaining naptha evaporate, otherwise condensation will melt your crystals.

You might then think that using naptha instead of heptane and combining pulls will create a more impure product than separate heptane pulls, but this is where your beloved heptane comes into play. Once you're done scraping the crystals from the bottom of your dish, place it all in a test tube and do a recrystallization! There are a lot of threads on how to do this, but I just do it quick and simple (no charcoal or anything other than hot heptane). Add a small amount of hot heptane to your DMT-filled test tube (just enough to dissolve the spice), let it separate, and use an eyedropper to suck up the clear heptane on top of a yellowish layer. Put this in a glass dish and repeat 3 or 4 more times. Combine these mini-pulls of heptane into a small glass dish or shot glass, throw away the remaining yellow gunk at the bottom of the test tube, and let it all slowly evaporate until you're left with a huge yield of pure crystals.

*EDIT*
I forgot to add that another way of increasing your yield is to NOT throw away your solution after the 4th pull. This is the only place you want to use heat. After doing 4 nice pulls of naptha, add the jug to a hot water bath and do 1 or 2 large pulls of xylene or toluene and get that jungle spice! The teks out there make it sound difficult and lengthy, but it is actually pretty simple. Take your 1 or 2 pulls and air evaporate the solution in a glass dish similar to the one in your freezer. It takes days to evaporate, but not much actual work time is needed. Every 12 hours or so go scrape the goo around to let the solvent evap quicker, and once it seems to not evaporate any longer, scrape the goo into a test tube and do the exact same re-xtal instructions I wrote above. The only difference is that you want to KEEP the bottom layer of gunk after the mini heptane pulls, this is your jungle spice (and let me tell you it is magnificent). And the top layers of clear heptane you separate with an eyedropper you want to keep, because that will yield a small amount of white spice.

By doing all of this you will definitely exhaust ALL actives out of your bark, and have a HUGE yield!
 
 
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