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Pink crystallization Options
 
jayjay001
#1 Posted : 2/11/2012 2:20:56 PM
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I posted this in my first topic, but I thought the subject matter was different enough that I thought the topic should be labeled differently.

Hey, just thought I'd let anyone who wants to know.

My heptane/whatever solution has been in the freezer for 3 hours now and it's already milky and there's visible crystalization on the side of the jar. I used more heptane than the 30ml called for with naptha, no more than 60ml each pull, because siphoning out 30ml was going to be a ***** (I have an inadequate mixing jar, too short and fat, so thinner layers, but it'll get replaced soon, and with larger quantities it won't matter as much). I also put 4 pulls all in one jar because there was so little each pull.

Anyway! I hope to report good news tomorrow!

*EDIT*

Ok, a few hours later I check again. There's more crystallization (although there's enough frost built up on the outside of the glass, and it's still milky, so it's not perfectly easy to see) but I noticed that some of the crystallization is a little pink. I was searching around the forum for posts on different colors of spice and read that red spice can be indicative of secondary alkaloids or certain plant oils being present in the product.

Just wanted to add, I let the lye mix sit (with one or two daily shakes) for about 3 days I'm guessing and for most of that time the container was sitting a couple feet away from a heating vent. Now, my house isn't kept particularly warm (the thermostat is kept to around 67F) but it's been somewhat cold so it's been running at least a few times a day. I checked the temperature of the jar immediately after it'd been sitting in front of the vent for the entire duration of one session of the hot air blowing and it was warm but not that warm. I probably rather vigorously shook it on those occasions as well.

Also, the original mixing container is glass, the jar in the freezer is glass, the turkey baster I used to transfer is glass.

The solvent I was using was Bestine, and the lye was Red Devil Lye, and on no occasion were there any spills or accidents that might have caused some sort of contamination with any of the materials used. I mixed the lye with the water using a cleaned stainless steel spoon.

When extracting the mixed/separated bestine layer from the total mixture I was very careful to avoid any lye making it into the glass. There were two or three occasions where a droplet of the lye mixture made it into the baster. One those occasions I immediately put all of the contents of the tube back into the lye mixture and cleaned the baster glass.

Ratios: (650ml water, 30g lye, 30g bark, between 45-60ml of bestine per pull, for four total pulls, all in one container)

Should I worry that there might be an unsafe contamination or simply a little extra material extracted from the bark?

*/EDIT*
 

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endlessness
#2 Posted : 2/11/2012 2:51:12 PM

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Does your bestine evap clean? Is red devil lye only NaOH? If so, its probably some plant material. Did you do a sodium carb wash? Sometimes nearly invisible droplets can come across and be suspended in your solvent, and then be together with your crystallize product. You could recrystallize and see what you get out.
 
jayjay001
#3 Posted : 2/11/2012 3:09:03 PM
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The bestine evaporates clean with no visible residue, the red devil lye is sold as pure NaOH and was also recommended in Lazyman's tek to use as lye, and I did not do a sodium carb wash (though I wanted to, I didn't get my hands on any before I got impatient).

I'm thinking of doing a heated bestine recrystallization, but I am curious if anyone thinks it's anything but extra plant material.
 
endlessness
#4 Posted : 2/11/2012 3:37:46 PM

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yeah there's the possibility its lye/basic material, it would not be good to smoke that... Even though lye doesnt vaporize at lighter temperatures, unvaporized particles can come across suspended in vapor and be harsh on the throat/lungs. Also general plant material would probably be harsh to smoke. So I definitely think at least with part of your product should be cleaned with re-x, so you can compare.
 
geko42
#5 Posted : 2/11/2012 4:28:58 PM

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swim agrees on the plant material.

as for the washes, look up making your own sodium carbonate.


basically if you heat sodium bi carbonate (baking soda) long enough and hot enough it turns into sodium carbonate. swim does his on a pan on the stove.
 
jayjay001
#6 Posted : 2/11/2012 8:25:09 PM
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*update*

Well, I took the jar out of the freezer, let it sit for a while to get to room temperature before I opened the seal and when I drained the heptane and looked at what I had, I found only tiny white snowflakes. I'm not sure what happened to the pink material, but I noticed that it was only ever on one spot on the side of the jar.

I'm drying the snowflakes now and I'll take a pic of the material soon but there's no visible discoloration at the moment.

So I'll update as things go.

I've never tried DMT before so I won't be able to give any meaningful comments on the subjective experience.
 
jayjay001
#7 Posted : 2/11/2012 10:45:47 PM
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A few updates.

When I was drying out the snowflakes, they all turned to liquid. I also noticed the bit of pink liquid/material when closely examining all the melted stuff. Actually, I should say there were a few really tiny crystals left in some of the liquid. There

I was assuming that too much plant oil/material got into the solution and made it dissolve (the pink crystals almost definitely melted into the solution).

I was going to recrystalize anyway, and I figured that would solve the problem with the plant material and or oil. I managed to get the bit of bestine heated and left the pink material in the shot glass I had. There was an extremely small amount of pink material, , I mean about the size of 5-10 grains of sand sizred. I can't say what other impurities were left but there was what looked like something that needed to be scraped from the bottom, but I dissolved it all into the bestine when it got heated, which I thought would be preferable.

I, unfortunately, spilled the shot glass and had no way to recover any of it. I'm not upset, given that I used only 1/4 of the 100g of bark I bought, mostly because I was worried I'd mess something up (lucky me I did >_> ) . I'm wondering if using way too more bestine than was recommended was part of the problem. It probably made it a lot easier to get a high impurity/dmt ratio, because there was so much heptane to pick up almost anything, even if I didn't pick up anything but heptane when siphoning. I'm also curious if the dmt crystals might have been easier to extract if I hadn't waited for the heptane to warm to room temperature before breaking the seal and taking it out.

Just a note, I have the leftover heptane and lye/mix saved for later use when I want to try it again.



Finally, I'm retrying the experiment with about 50g of bark and lye (actually, somewhere between 30-50g of lye, because my scale is pissing me off and I seem to have been told that anywhere between 25-50g of lye would give easily high enough pH for at least one decent pull) so I guess I'm a little impatient at this point, bad, I know.

I'm going to use the recommended amount of solvent this time, since the recipe is large enough that there shouldn't be problems siphoning off a normal amount.

If anyone has any thoughts or suggestions, I'd love to hear them.
 
jayjay001
#8 Posted : 2/12/2012 2:11:56 AM
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One more extra thought!

Is it possible that by letting the solution warm back to room temperature before I siphoned off the heptane from the crystals that the dmt simply re-dissolved back into the little heptane that was left over?

Should I just siphon and pour it out as soon as I take it out of the freezer?

 
jayjay001
#9 Posted : 2/12/2012 2:15:53 PM
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Finally, I'm retrying the experiment with about 50g of bark and lye (actually, somewhere between 30-50g of lye, because my scale is pissing me off and I seem to have been told that anywhere between 25-50g of lye would give easily high enough pH for at least one decent pull) so I guess I'm a little impatient at this point, bad, I know.

I'm going to use the recommended amount of solvent this time, since the recipe is large enough that there shouldn't be problems siphoning off a normal amount.


::UPDATE::

So I did two pulls of about 50ml and got the snowflakes again, this time without any pink crystallization. Took the jar out of the freezer, immediately poured out the heptane through a coffee filter, got a little pile of white powder there, dried pretty quickly.

Also scraped off some powder from the inside of the jar, also very white. I couldn't tell you how off it is from pure white, but it looks great to me.

There was a sizable amount of stuff left on the edges that was going to be a pain to scrape (I used a different jar for some reason and it's the exact wrong shape for that, don't know what I was thinking) so I just dissolved the rest in some bestine and figured I'd add it to another crystallization process.

All of the powder was salvaged, and even the stuff in the jar took a little while to redissolve into the bestine (though I didn't use much).

I noticed something else as well. The bestine layer that I had sitting in a jar left over from the first extraction was significantly more yellow than this bestine. I assume there's definitely something else trapped in the heptane, probably since the lye/mix was left sitting for much longer and heated, and so likely had a chance to release a lot more impurities.

Other than that, I only have the one pull, I haven't measured it yet (I don't want to transfer it from place to place any more than I have to, since I know I'll lose material) but I will soon. Unfortunately that doesn't give me an accurate yield from that pull since there was a lot of scraping left.


*NOTE* Will do sodium carbonate wash on leftover bestine and then try to freeze, see what comes out.
 
Dustee
#10 Posted : 2/24/2012 2:05:28 AM
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You don't want it to reach room temp. you want to pour it through a coffee filter asap. the liquid warms quickly, and when it warms the spice will melt back into the bestine.

SWIM gets a funnel with a coffee filter and immediately take the bestine out of the freezer and pour it through the filter catching the spice. dump/scrape what ever is on the filter on a dish and put in front of a fan on low.
All of these posts are purely fictional and any possible similarities with real events or characters posted are only coincidences.
 
Visty
#11 Posted : 2/25/2012 7:24:47 PM

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Would it help after you filter to put the filter with the spice back into the freezer as to avoid melting and then let it evaporate in the freezer? That is, I use ether which evaporates very fast, perhaps even in freezing conditions. I use a glass pot with a plastic lid which is not truly airtight. But when I opened up my freezer this morning I smelled the ether. So, something must have evaporated.



 
 
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