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My first extraction (HALP pls!) =) Options
 
The_Curious_One
#1 Posted : 8/5/2011 6:50:06 AM
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Hello everyone, this is my first post on these boards but I have been reading the forums for several months now, and I'm happy to say that I'm finally amidst my first extraction using a varied STB method.

If someone could check out my process and tell me if I screwed up somewhere I would be very greatful.

Everything seems to be going okay so far, but one thing has me a little worried that I might have messed up somewhere. My naphtha is supposed to a be cloudy white color, but mine is just clear with no visible traces of DMT (before freeze precip).

I was a little confused about one part of Noman's Tek. It says, "Mix 15mL water and 1g lye per gram of bark in the mixing jar. For example: 50g bark would require 750mL water and 50g lye." Then it also says in the Remarks section on the same page, "Note that if pre-powdered bark is being used, 1.5 - 2X of the water called for will be required." I have powdered bark and I had to add at least twice the water that it said (for a total of around 1500mL) because it was so incredibly thick with just 750mL that it didn't seem like the powder was able to completely dissolve. So, with all that extra water it said to add if using powdered bark, it didn't mention the need to add any more lye to the solution to compensate. I didn't add anymore Lye though just because I don't know enough about Chemistry yet to second guess Noman's Tek which several people have used with great success.

So - What I did was mix about 100 grams of Lye slowly to 750mL of water and stirred until everything was dissolved. Then I added in 100 grams of finely powdered Mimosa Root Bark (from http://www.adenium.com.br/). After stirring for a while, the liquid was extremely thick and I could see that there was no way that all of the powder was going to dissolve into that much water no mater how much I stirred it. So at this point I went back to the check the Tek again and noticed that part in the Remarks section about doubling the water, so I did that and added in another 750mL of hot water.

I stirred the glass pitcher it was in until it had all dissolved into a black murkey (but now much more watery) liquid and then transferred it into a clear gallon sized glass wine jug. I placed the cap on the jug and shook and rolled it vigorously for several minutes until it had formed a fairly thick (2'' ish) brownish foam on the top of the black liquid. I let it settle for about 2 hours until pretty much all of the foam and bubbles had disappeared. The jug was still warm. I added 100mL of warm VM&P Naphtha (heated with warm water around a small glass) to the wine jug, and then decided to add another 100mL of room temp Naphtha just so the layer would be thicker and easier to extract with the turkey baster I'm using.

After adding the Naphtha I rolled the jug around (literally... it rolled easily on the carpet) for about 5 minutes, while turning it upside down and right side up every minute or so. After the 5 minutes of mixing, I let it sit for about 20 minutes to let it separate (even though it looked like it had separated completely almost right as I stopped rolling it back and forth).

I then proceeded to suck up only the top clear layer of Naphtha with my turkey baster and put it into a glass baking dish (approx 12''x6''Pleased. I only sucked up about 60-70% of the Naphtha at first since it was getting harder and harder to only get the clear layer as it got thinner and thinner. I made sure to not transfer ANY of the black liquid to the baking dish though. With this 60-70% of my 200mL of Naphtha I placed it in front of my patio screen door on the floor with a fan blowing over it to make sure all the fumes got blown outside. I let it sit like this for about an hour and when I came back a noticeable amount of Naphtha had evaporated. So I went back to the wine jug and decided to go ahead and try to get more of the thin layer of Naphtha that was left. After some patience and careful turkey baster work, I added another 20-30% leaving only an extremely thin clear layer of about 5 - 10% of the total Naphtha I had used left.

At this point I looked into the glass baking dish and the Naphtha solution didn't look cloudy at all like its supposed to, so I am a little worried, but I placed it in my freezer anyways. After 4 hours I'm going to turn the Cold setting on max (its on 6 out of 9 now), then leave it in for another 4 hours. Hopefully I'll be able to see some crystals by then.

Again I would greatly appreciate it if anyone could let me know if anything sounded wrong with the procedure I used. Also, does anyone know why my solution doesn't look cloudy at all like so many people have reported once the solution is saturated with the DMT...?

Thanks again for all of the knowledge you all have amassed here and it's nice to meet you all!


 

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Shattered_Symmetry
#2 Posted : 8/5/2011 8:01:33 AM

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Hi curious welcome to the nexus,

Don't worry about the extra water you added added as pH works on a logarihtmic scale not a linear one, ie doubling the amount of water does not require you to double the amount of lye. I have heard people say that provided the liquid goes black and sludgy then you should be ok. In addition mixtures with high pH dont tend to form emulsions as easily so if after one of your carpet rolling sessions it wont separate it might mena the pH is too low so bung some more lye in and stir.

The additional 100ml naptha you added will need to be evaporated down as befreo precip. freeze precipitations work better on saturated solutions so by diluting it with more naptha the cold temperature might not bring your spice out of solution. It is an easy fix however you just need to evap a bit and your spice should come out just fine. If not much comes out after nine hours I would be tempted to leave it in the freezer for 24 total to see if it makes a difference.

Also I wouldnt worry if your basified bark seems think and sludgy, its normal.

Other than that if you stuck to nomans tek you should be fine.

Best of luck dude!
 
The_Curious_One
#3 Posted : 8/5/2011 9:43:06 AM
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Well I did evaporate some of it down already when I pulled the first 60 - 70% of the Naphtha layer. I put the glass baking dish in front of my screen patio door with a fan blowing over the top of it. After 1 hour enough of it had evaporated that my Naphtha didn't even cover the entire bottom of the baking dish, so thats when I went back to the wine jug and turkey basted the rest of the Naphtha out so I would have just enough to cover the entire bottom of the dish, even though it was extremely shallow.

Should I have evaporated more? I just thought that I needed enough Naphtha to cover the bottom at least.
 
Shattered_Symmetry
#4 Posted : 8/5/2011 10:12:19 AM

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if doing freeze precip swim doesnt usually evap at all. if naptha was used in correct proportion and is saturated the crystals will form during freeze precip and the naptha can be poured back into the extraction jars to be used in more pulls with an evap at the end to get the last bits.
 
Noman
#5 Posted : 8/5/2011 3:07:46 PM

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[quote=The_Curious_One

" For example: 50g bark would require 750mL water and 50g lye."

So - What I did was mix about 100 grams of Lye slowly to 750mL of water and stirred until everything was dissolved. Then I added in 100 grams of finely powdered Mimosa Root Bark[/quote]

When you added the second 750ml of water, all you did was get the ratio up to what I initially suggested, not the double water ratio for pre powdered bark.
But that doesn't seem to have given you a problem anyway. If the naptha separates after mixing, you have enough water.
You may not have a problem at all actually, depending on what comes out of the freezer.
Naptha can often be clear as a bell and precip lots of nice white alks.
You did right to evap some of the naptha off. By adding that second 100ml, you made it less saturated and less likely to precip. Some, like Entropymancer, have suggested that .4ml per gram of bark would be better than my 1:1 ratio, so you may need to evap off 75% or so to get a good precip.
Do a few more pulls, see what happens, don't throw anything away, and post your results.
 
The_Curious_One
#6 Posted : 8/5/2011 6:23:11 PM
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Thanks for the reply Noman. Now that I re-read my post, I forgot to mention it, but I did remember to double the original 750mL of water since I was using twice the amount of bark that your example used. So I had 1500mL of water/lye solution, then added the bark, but it was still extremely thick after stirring, so then I added water until my container was almost full (just short of 2000mL), then transferred it into the wine jug, then added a little more water (maybe about 100 - 200mL). So I had probably around 2000mL or maybe a little more by the time it was ready to shake up.

As for how it turned out, I removed my 12x6'' glass baking dish from the freezer after 8+ hours of letting it precip without disruption. After removing it from the freezer, I poured off the Naphtha through a coffee filter inside of a funnel in a glass.

Most of what was poured into the coffee filter was just tiny little powder DMT, not clumped together like what was left stuck to the glass dish. It looked as fine of a powder as table salt or something. The rest of what was in the dish was still very damp. I tried to pour off as much Naphtha as I could, but there was still an obvious amount left in the glass dish. I remembered reading that the DMT will melt back into the naphtha once it reaches room temperature, so I had to improvise.


I started scraping up as much of the crystal splotches on the glass dish as I could, but all I have to use is the small blade of an Exacto Knife... so needless to say it wasn't very effective. All I could scrape up was a bunch of damp clump of white stuff that resembled wet sugar. I started getting little piles of the soggy wet white stuff on my exacto knife blade so I could scrape it onto a fresh coffee filter paper. After scraping several clumps of the white stuff onto the coffee filter it was becoming harder and harder to get what was left with my shitty little blade, so I decided to pour the Naphtha I had just filtered back into the glass dish and put it back in the freezer.

As for the clumps of soggy white powder on the coffee filters, I've had them sitting in front of a small fan on a low setting for several hours now, but they still crumble to smaller clumps as soon as I touch one with a blade or anything. One of the coffee filters (the one that the Naphtha was poured into) looks even finer of a powder, like tiny little bitty crystals resembling a several grains of salt scattered out.

Here's a pic of the coffee filter with the larger clumps of white crystals on it. I don't think the other coffee filter would photograph very well considering how fine and small the crystals were on it.



How long do the crystals take to fully dry? And what is the best method you have found for drying them once you take the glass dish out of the freezer? Thanks again for the help Noman, hope to hear from you again when you get a chance. =)
 
The_Curious_One
#7 Posted : 8/6/2011 2:37:03 AM
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I figured I would post an update on the status of my first extraction. The crystal clumps finished drying on my coffee filter and left me with just enough for a few hits worth in the new glass oil burner pipe I just bought. Here's a pic after my first bowl was loaded.


Unfortunately I didn't breakthrough, or even come close to it really. The feeling I got reminded my of being under Nitrous at the dentist office. My face and body went mostly numb, there was a slight burning sensation on my lips where they touched the pipe to inhale. As far as the visuals went, everything became somewhat blurry, and upon closing my eyes I could see images of random things along with patterns that continued to progress. After opening my eyes though I didn't really see anything that wasn't there, everything just appeared a little blurry and out of focus for a while. My body felt heavy and I didn't have much energy for a few minutes after the hits I took, but that was about the extent of my first "trip". Rather disappointing really. =/

I think part of my problem is after the crystals melted down and I was able to vaporize my first hit's worth of smoke, I began losing my motor skills rather quickly as I exhaled my first hit and inhaled my second. I tried to get a third hit's worth but I was becoming kind of light headed as I went to put the flame below the liquid in the pipe again, so not much smoke vaporized and I only got a small puff for my final hit. I was too disoriented to try a 4th hit, even though there was still a small amount of liquid in the bottom of the bulb.

I'm now out of the crystals I had dried out, but I have another batch in the freezer now (same amounts as before just refined the process a little this time). So I should be drying another coffee filter of crystals in a few more hours.

I'm also starting a new extraction using Marsfold's A/B Tek. I just got done adding half a gallon of the water / vinegar solution to a pound of bark powder in a crock pot. It's been on high for about an hour and a half now, so I still have about 4 and a half hours of the Polar Extraction before I start preparing the water / lye solution.

One thing I'm wondering about though - Why is there such a massive difference in the amounts of Lye called for with different Tek's? Noman's says you should use 1 gram lye per 1 gram of bark, but Marsfold's using only 70 grams of lye for 454 grams of bark. Thats a pretty massive difference there. I suppose it could be because Marsfold's uses the extra step with the crock pot / water / vinegar, but I'm not so sure...

Anyone have any insight on this? Thanks again for the help.
 
Noman
#8 Posted : 8/6/2011 3:00:55 AM

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The massive amount of lye called for in STB teks like the one I wrote is because the lye takes the place of the cooking to break down the MHRB.
A/Bs just use enough lye to break the alkaloid base free of the acid salt - typically pH 13.5.
They both work, just in different ways. It's a matter of preference.
As for your crystal recovery, everyone finds their own way on that, but remember to not expose your precip vessel to open air after you've poured off the naptha or moisture from the air will condense on the cold glass.
 
The_Curious_One
#9 Posted : 8/6/2011 3:19:31 AM
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Thanks for the explanation about the different lye amounts Noman.

About the crystal recovery though, maybe that's where I messed up before. Should I leave the glass baking dish covered after draining off the Naphtha until it reaches room temp, and THEN uncover it to air-dry it with a small fan blowing on it from about 3' away?

Also I have another question regarding light exposure. When I was drying my crystals I didn't really think about doing it in a dark place, so I'm wondering if maybe that's why I wasn't able to hallucinate very much at all with my first set of crystals. Is the potency affected from 1 days worth of (not very bright) light exposure while air drying?
 
Noman
#10 Posted : 8/6/2011 3:59:06 AM

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The_Curious_One wrote:
About the crystal recovery though, maybe that's where I messed up before. Should I leave the glass baking dish covered after draining off the Naphtha until it reaches room temp, and THEN uncover it to air-dry it with a small fan blowing on it from about 3' away?

Also I have another question regarding light exposure. When I was drying my crystals I didn't really think about doing it in a dark place, so I'm wondering if maybe that's why I wasn't able to hallucinate very much at all with my first set of crystals. Is the potency affected from 1 days worth of (not very bright) light exposure while air drying?


You got it exactly!

A days worth of light shouldn't degrade your product. It's likely smoking technique. You need to get the amount shown down in two big hits right behind each other. Hard to do with a chicken bone base pipe but possible. It takes a bit of getting used to.

I'm glad you're trying out different teks. Marsofold's is one of the best. Find one that works for you and then adapt it to your methods. The specifics don't matter as long as you're using the right basic methods. I like A/Bs for large extractions and STBs for smaller amounts.
 
The_Curious_One
#11 Posted : 8/6/2011 5:23:10 AM
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I'm in the middle of heating my bark in the crock pot (for the 2nd time out of 3 total).

The first time, when I added the half a gallon of the water / vinegar solution to the powdered bark, after it was done sitting for that first 2 hours, it was not boiling at all, but it was very hot. I poured about 3/4 of the liquid off, but a small amount of the brown gunk spilled over the side as I was pouring it off into my glass pitcher.

I ended up getting a little sludge in liquid I poured off, actually about 40% of what I poured off seems to be sludge. After it sat on my counter for the next 2 hours while another 25% of the gallon water vinegar solution was in the crock pot, the liquid in the glass pitcher separated and there was a much thicker brown layer on top with a more clear watery layer on the bottom.

After the second 2 hours was up, I noticed that this time the brown stuff in the crock pot was boiling and bubbling unlike the 1st time. Is that strange? Is the liquid in the crock pot / glass pitcher supposed to be this thick? It seems like it was too much powder for that amount of water and not all of it is able to dissolve, but hey what do I know.

Thanks for all your help so far Noman, would appreciate any further input you or anyone can provide.

Edit: CRAP I fell asleep and accidentally left the final boil phase going for about 6 hours instead of 2 hours... when I woke up some water had boiled over the side into a small puddle around the crock pot. I decided to just go ahead and pour the rest of the liquid from the pot anyways even though it had been cooking far too long... what I was left with was a TON of vegetable sludge at the bottom of the glass pitcher. I'd say it was close to 40% sludge by the time I was ready to transfer the liquid part to the Wine Jug. Is this normal?... and could I have messed this whole attempt up because I heated the last 25% of water / vinegar / bark solution for 6 hours instead of 2?

I sure hope not. That would be a waste of a pound of bark. =/
 
Noman
#12 Posted : 8/7/2011 7:40:33 PM

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As long as you didn't burn it, it's fine.
 
 
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