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A Vovin's Tek Diary Options
 
SuperRad
#1 Posted : 8/22/2009 6:07:50 PM
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Yesterday I started on the first steps to Vovin's tek.

My MHRB is from FV, and thus was already FINELY ground when I got it (go straight to step 2 Smile).

The preparation of acidified solution went as planned although there was ONE moment where I accidentally left the burner on during the heat bath (hopefully I didn't kill all the DMT).

Filtering the acidic solution was a HUGE pain even though I have a vacuum filter. I filtered the first acid wash, but for the second I just decanted it as best I could. I did a complete filtration after the final acid wash, and it took over an hour and used at least 15 filters just for that step.

Next time I'm definitely skipping the filtration step and treating the extraction from the defatting step on as if it were an STB (just adding more lye for the basification and keeping the MHRB powder through the whole extraction).

Anyhow, the acidic solution has been sitting in my fridge overnight and sure enough there is a significant layer of sediment, even though I nearly tore my arm off pumping that vacuum pump. I wish I had received a variety of filter papers with my vacuum filter, but I just have a 100pk of "medium" flow rate filters which are simply too fine for entheogen filtration.

I will be decanting and reducing in a couple hours, I figure I will probably have questions along the way and if not, this might serve as a good diary of the individual experience in attempting such a technical tek.
 

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SuperRad
#2 Posted : 8/23/2009 12:12:31 AM
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The decanting did not go so well, 90% of the sediment came up readily with the liquid. Oh well.

I evaporated the whole thing down to a little less than 400ml. It took a long time.

At this point I was thinking to myself that I should just do a STB next time.

Then I started defatting. A LOT of pink fats have separated into the naptha. Hmmm... maybe A/B extractions aren't so bad after all Smile. I'm letting the second defat separate, hopefully the third comes out a lot clearer.
 
SuperRad
#3 Posted : 8/23/2009 1:50:01 AM
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By my third defat, I began to suspect that the "fats" in the naphtha was actually an emulsion. Oh well!

I basified and have added my first volume of naptha. I stirred vigorously and now I'm waiting for the layers to separate. I'm not going to use a heat bath this time. I'm just going to wait as long as it takes for the volumes to separate cleanly. It's been ~15-20 minutes since I mixed and there's still a lot of emulsion, but I can see a clear layer slowly growing at the top. Patience patience patience.

I am SO not looking forward to evapping the naphtha down. At least I'm freeze precipping and not evaporating the whole ugly mess. With my emulsion troubles I'll probably have to do a recrystalisation or two Sad.
 
SuperRad
#4 Posted : 8/23/2009 5:22:04 AM
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Well that was trying! I think I may have bitten off more than I could chew, but my reduced naphtha is sitting in the back of the freezer.

I feel like I messed up in a lot of spots, and I had really dreadful issues with emulsions. Even after adding more base water. Next time I will know how to deal with them better (I figured out a simple method to clear them up but, of course on the final naphtha pull). I probably also used excessive heat baths on the basified solution.

I'm truly expecting failure here, unlike 69ron's mescaline tek, this one is NOT on autopilot. Next time (if there is one) I will be going with an STB until I have better control over my organization and focus.

It was still fun playing chemist Pleased

I'll post what happens, if anything. Smile
 
SuperRad
#5 Posted : 8/23/2009 5:55:18 PM
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After 12 hours in the freezer I see that flakes of SOMETHING have settled to the bottom of the plate. It doesn't look like much right now, but there's probably at least 20 little flake formations. Assuming it's DMT and not ice, I'll have a couple bowls worth.

Lets just hope these crystals keep growing/precipitation over the next 12 hours (when I'm planning to do the first collection.
 
SuperRad
#6 Posted : 8/24/2009 7:19:41 AM
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I poured off my first plate of frozen crystals. The plate looked pretty full!

I let it out to dry, while I evaporated to poured off naphtha for a second freeze.

As the first plate was drying, I noticed pool of naphtha falling out of the crystals. Concerned that the warming solvent would redisslove the crystals, I put the plate on some mild heat (hoping it would evap the naptha quicker).

BIG MISTAKE. In the blink of an eye most of the crystals melted. Though I was depressed, I let the plate continue to evaporate, then put it back in the freezer. Once everything had resolidified, I scraped it all up. All in all I ended up with a nice little strip of hardening alkaloids.

It weighed .37g making for a .66% yield. I tested 50mgs and it was able to send me to hyperspace. Twice.

Right now I've redissolved the remaining .32g in clean naptha and placed it back in the fridge. Once I collect the DMT off of both plates I will do one or two additional recrysalizations, I noticed that a fair amount of goop was left after redissolving the DMT, but a couple drops also visibly made it into my freezing plate.

WOO HOO, I have 6-8 good launched left, and three more ounces of MHRB comming.

I will be trying food grade dry/fasa teks next as they seem to fit my style more Smile
 
Fakkz
#7 Posted : 8/24/2009 7:17:56 PM
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Glad to hear that the extraction wasn't a failure, Vovin's tek is one of the more difficult ones. With MHRB I am happy to do a STB, I get better yields that way, and don't stink up the house with an acid boil.

Two for two on extractions so far, well done!
 
SuperRad
#8 Posted : 8/24/2009 10:46:51 PM
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Fakkz wrote:
Glad to hear that the extraction wasn't a failure, Vovin's tek is one of the more difficult ones. With MHRB I am happy to do a STB, I get better yields that way, and don't stink up the house with an acid boil.

Two for two on extractions so far, well done!


Thank you! I was quite eager to use my schmancy vacuum filter and other lab setup, but when your lab is a kitchen it's isn't as easy to keep everything orderly Smile.

I looked at the measuring cup I had used to redissolve the crsytals and to my dismay, it looks as if there are a bunch of crystals in it! And looking at my two freezing plates, neither show much crystal activity.

So to those out there planning on doing recrystalizations, warm the naphtha well, swirl it well, and use a container with a wide enough bottom so that the impurities can settle out without covering up any DMT.

I'm going to have to combine my two freezing plates, scrape the one that has the impurities/crystals and put it in my "impurities" container, redissolve ALL THAT dmt (without carrying junk over) and crystalize once more.

SOOO much work (but I only PRETEND not to like it Laughing )
 
SuperRad
#9 Posted : 8/25/2009 2:42:52 AM
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OH darn! I forgot to post some super essential tips, that apply to any tek not just A/Bs

First! If you are putting something in a heat bath, wipe the container off once you take it out of the water!!! This sounds obvious, but I forgot last time and had to fish two melting water drops out of my freezing plate before they dissolved too much DMT.

Second! Be SUPER vigilant about which heaters are on/off. I made so many mistakes in this department I'm surprised I even got anything.

Third! If you're using a sep funnel and get emulsions, sometimes the only way to get them out is to pour out the bottom layer slowly until only a little bit remains, then tilt the sep funnel so that the top solution layer "compresses" the emulsion bubbles. Pour out as much of the emulsions as you can without pouring off the top layer. Then abrubtly drain out the top layer into a SECOND container. The lower layer should contain most of the emulsions, use a spoon to stir and break the bubbles. The second container should have a tiny amount of the lower layer, but by magic there shouldn't be very many emulsions left. Put the two back in the sep funnel and then mix very gently and place in a heat bath. Now they should be good to separate without those stupid emulsions contaminating either volume! Also, tipping the sep funnel slowly over and over helps break up the emulsions, albeit in a slower fashion than the other method.
 
SuperRad
#10 Posted : 8/25/2009 5:38:03 AM
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The recystalizations are going smoothly, everything has been combined into one plate. When I scrubbed a freshly unfrozen plate earlier I was greeted with nice, tiny crystals, but they were whisked away with some new friends Smile.

I tried very hard to keep my dmt-melting pot warm and melt away ALL the dmt, but some dmt crystalized in it again! So I melted it in more warm naptha and poured this off onto a second plate and just let it evap. Scraped 80mgs waxy crystals, they certainly don't look very pure but I'm certain there's a blastoff or two in there. There's still a layer of yellow stuff I don't want to smoke in my melting pot, but there's also a few more tiny x-tals! Probably hard worth it by now, maybe ~5mgs tops... but I wants them!

And now I have one big motherload mama in the freezer. Tomorrow evening I expect to see my first pure harvest, then one more evap and freeze and then I'll let what's left to evap completely
 
 
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