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I finally started my first extraction Options
 
Mugen
#1 Posted : 7/1/2013 3:58:33 PM

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I'm at step 8 of Noman's tek. so I thought I'd write about how it went so far.

My first experience was sloppy to say the least. I slowly dumped out the whole mega-mix into my sep-funnel only to realize That the clumpy bark had gone in too and that couldn't possibly work. so I dumped it back into the jar and began to clean out the funnel. I made some light spills along the way. and I'm sure from all the re-pouring I got enough splashes to get some emulsions in the batch.

I have about 100 ml of clean naphtha in the freezer out of the 200ml I should have from what I put in to match the 200g of MHRB I used. now I'm nervous as I'm hoping I'll get something out of this.

I still have a mix in the sep-funnel with a substantial layer of naphtha so I'm sure I can get more. I just decided to give it a day so that it can hopefully separate some more with a few more agitations along the way. I'm hoping that will win me back some product.

I'm expecting a low yield this time around but I'm crossing my fingers for a gram. I'll be happy with half. I still have more root bark so I feel that next time I do this I might just do a better job and score a higher yield after having learned from my mistakes.

One thing has been bothering me though, in step 7 of Noman's tek it says "Leave the last NP extraction in the jar for a day or two." NP I assume is Non-polar, is that reffering to the original mix of naphtha bark water and lye. I sure do hope so cause If that's not the case I'm doing something wrong here.
See you later Space Cowboy...
 

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pfxtc
#2 Posted : 7/1/2013 4:10:18 PM
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I remember my first... hiding jars under my bed and then somehow sneakily transferring them to the freezer when I was in High School. As far as naphtha is concerned I think getting about 1/2 per pull is wise (so 100 out of 200 is fine). This way you're not stressing about getting 'every last drop' and you're sure the naphtha being pulled is clean and lye-free. I've never used a sep-funnel and am not sure if they're worth it. I always liked using little pipettes for small-medium extractions like yours. I've found that heating the naphtha in two ways can be tremendously helpful:

1) Get a pot of boiling water going. Put clean naphtha in a mason jar and submerge that into the boiling water. This safely heats up the naphtha (which allows it to 'pull' more).

2) Put the naphtha in the mixing jar. Put this mixing jar in a hot bathtub or hot sink or hot pyrex dish. This will continue to heat the naphtha. You can either make your pull in 10-15 minutes before it cools down or you can wait about 24 hours (only leave it in the water for 10-15 minutes). I'm not sure if waiting longer = you lose the 'point' of heating it, but I do it regardless. I find that letting naphtha sit over 24 hours ALWAYS pulls more then heating it up and only letting it sit 10-15 minutes.

That step 7 is basically saying after you do your 3-4 naphtha pulls and you're getting really small pulls in the freezer, you should put the naphtha back in the jar (or use new naphtha or whatever have you) and let that sit in the mix for 2-3 days. This allows the naphtha more time to 'pull' the crystals out. After your first few pulls the yields will lessen and the naphtha will need more time.

There's two ways people use naphtha as far as I know. One way is to recycle (most effective I think). You put the naphtha in 24 hours, lightly mix it for a bit or slowly roll, and then you pull this out and freeze it. After the crystals precipitate out, you can pour that same naphtha BACK into the jar. The benefits of this = cost effective + you're sure you're getting everything. If you use new naphtha and just throw it away you might be losing all kinds of alkaloids or you may just be dealing with too much damn solvent.

As far as emulsions, I'd do some research but if I remember correctly adding small amounts of SALT and using the BATHTUB hot water thing I recommended earlier always cleared those right up. I wouldn't worry much about emulsions until you do a pull or two though. Let us know how it goes. If I were you I'd take EVERYTHING and put it back into ONE jar and use a pipette to 'siphon' off the top layer of naphtha. You only need to get 1/2 of it; just do a few extra pulls and you're good. I've done a lot of STB's... working now on my first A/B which has been interesting.
 
Mugen
#3 Posted : 7/3/2013 4:12:31 AM

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Thank you for the response pfxtc Smile

I have a question about this nice piece of advice you gave me; Should I introduce the warm clean naphtha to my original batch that I still have in the mixing jar to pull more dmt? or should I start a whole new batch to incorporate that method?
See you later Space Cowboy...
 
pfxtc
#4 Posted : 7/3/2013 7:26:04 AM
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Mugen wrote:
Thank you for the response pfxtc Smile

I have a question about this nice piece of advice you gave me; Should I introduce the warm clean naphtha to my original batch that I still have in the mixing jar to pull more dmt? or should I start a whole new batch to incorporate that method?


It wouldn't matter if you 'mixed' them, it's all the same stuff. You don't wanna use too much naphtha. Better to use smaller amounts that are more concentrated when you freeze them. More naphtha doesn't equal bigger pulls. What I would do is let your naphtha sit for 24 hours or whatever you're doing, freeze it, then heat it up before you put it back in.
 
Mugen
#5 Posted : 7/3/2013 9:02:02 AM

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alright, and so this way I'm still working with the same batch I made in the first place to pull more strays? I was wondering if this old "soy sauce" I have here would yield any more product. what you're saying sounds effective.
See you later Space Cowboy...
 
Mugen
#6 Posted : 7/4/2013 11:35:31 PM

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I started another pull and began to add those steps. I made the mistake of buying a large separation funnel so I have to take care when pouring into the funnel and let the fluids pass down the side to prevent splashes that would cause emulsions. I used the heating methods and simply poured my batch without care into the sep-funnel only since it was safer for me this way, I'll need a long hose to prevent splashes next time to prevent this next time.

splashing along the way when I suddenly saw my emulsion. didn't know what it would look like till i saw that 3rd layer of stuff that had no were to go. then it dawned on me. we heat the stuff up to get a good separation. I needed something hotter than my bath tub. and pouring boiling water over this spot would take forever. so I grabbed a Hair Dryer to heat the area where this emulsion sat. It magically began to separate, dancing around like a lava lamp. And now I'm sitting with a well separated batch. I think my solution will come out as clean as my first pull, which was around 500mg of clean white powder. My 2nd pull is about 300mg of honey tinted stuff so I probably got some unnoticeable emulsion into it. and now I'll have to wait for the third to see how this heating technique comes out but I have faith in it turning out clean

thanks for the advice pfxtc. It helped allot.
See you later Space Cowboy...
 
Sykosis
#7 Posted : 7/9/2013 4:37:18 PM

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Sometimes your pulls get slightly more yellow or honey colored as you let the mix sit. Also the solvent your using has a big effect on that to, Naphtha will pull trace amounts of other alkaloids the longer you let it sit. Heating a solvent in a hot bath will make it more soluble which may have accounted for the other alkaloids. If you are concerned you did get some lye in your end product you could perform and Sodium Carbonate wash on it, Then go one step further and recrystallize.

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