Extraction help needed.

[ILUSIAN]

Hey everyone

So this is my 6th extraction and this is the first time I have come across this problem, SWIM was about to do the first pull using VM&P Naphtha as SWIM is familiar with it. SWIM started to pull the Naphtha from the jugs and found it to be much darker in color than usual and instead of yellowish it was almost the same color as the MHRB (before the tek). The jugs have had the Naphtha in them for just over 12 hours at a temperature of about 120-130F. Is this normal or did SWIM mess up ? Any Answers are greatly appreciated

 

[Kash]

Thats odd.. Is this a naptha defat or extract after basifying?

Try letting it seperate for a few hours you may just have an emulsion.

 

[DudeMeetTyler]

it will happen.. i think it was something to do with particles being suspended in the naphtha.. search for red/brown naphtha it will come up..

are you using prepowdered?

 

[ILUSIAN]

Indeed sir, yes I am , Also the dmt randomly crystalized on the first pull, and now that I am done I have oily brown wax. This is the first time this has happened to me, I have had yellow wax but never brown. I did the Caustic soda wash 2x and pulled some really black gunk out , and then did the cold water wash.

 

[endlessness]

FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me

Hope this helps!

 

[ILUSIAN]

So swim was doing the STB tek and the Dark brown naptha occured, SWIM thought nothing of it as he thought it was just uber saturated. However when the naphtha was washed and dried and put in the freezer ,only brown goop percepitated. Looking up information SWIM attempted to do another wash , however swim does not know what components to keep much less what to try and freeze. Time is of the essence as SWIM must travel and hoped to have this done sooner than now.

 

[endlessness]

I would re-a/b it, as the link I gave you said.. do 3x vinegar pulls, base, re-extract, re-freeze. Extracting in a hurry is not good, but I hope it gets ready in time.

 

[ILUSIAN]

Thanks man , I shall try again , as for the MHRB and the original Lye , I added Xylene to try and pull some spices after the N,N .So hopefully I can salvage something.

 

[endlessness]

By re-a/b I dont mean start again with the mimosa, I mean get the very naphtha with the brown goop and add vinegar to it, and proceed as mentioned. Dont throw anything away till you're finished

 

[ILUSIAN]

Indeed that was the plan, the Xylene is just a side/ after project

 

[Kash]

So that picture of the measuring cup looks like a brown water layer, and a half emulsion of whitish clear top naptha layer. Are you sure the brown layer is naptha? Naptha sits on top of water.

 

[whitebread420]

I'm glad I found this thread because I am having a similar problem.

I'm doing a big extract with 500g of MHRB powder. I simmered while constant stirring for a long time .. like 8.5 hrs.

I basified with sufficient NaOH and started to extract with warm naptha. At first the layers were separate, then i gently stirred (constant) for 20 mins. I come back (should have been paying attention) and a emulsion formed. i let it sit over night but the naptha is VERY dark. I guess is sort of a good thing because that shows i had very effective cell lysis, which I think was a problem for me in the past.

I know i have to re-extract from my dirty naptha, but my question is how much pH4 water should i add per part naptha? and similarly how much NaOH (pH14) solution should I add to that to sufficiently crash out the spic? good thing i have a medium size sep funnel

thanks for the help!

 

[endlessness]

Whitebread, to clear emulsions check FAQ. To get rid of brown naphtha issue, also check FAQ.

FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me

FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me

You dont need to be exact with amount or pH. Salt out with vinegar 3x.. You can use roughly a fourth amount of vinegar per salting as you have naphtha. Then just add NaOH till you reach pH 13-14 (if you have pH meter), or add excess because too much isnt a problem.

Also your spice will probably not 'crash' efficiently, you should use a non polar solvent to pull from that after basifying.

 

[whitebread420]

thanks for the help. In the past i've done de-fatting or mini a/b and when i add basic h20 to the pH4 extract water it turns very milky, so in my head that was "crashing out" my vocab might be incorrect though

 

[endlessness]

No no, you are actually correct, but the thing is, to change from this cloudying to actual precipitation which you can filter, in the case of dmt, is a bit troublesome in my experience... Ive had success with pure dmt fumarate solutions and lye or sodium carbonate, and then just filtering after a few days to retrieve alkaloids, but with acetic acid/vinegar solutions, it clouds up but doesnt crash out in my experience. I think better use a non-polar to pull.

 

[whitebread420]

will do. I should expect it to become less cloudy after each pull, correct?

 

[whitebread420]

So I did a mini a/b last night on my first few pulls from my big soup. As I did more pulls the solvent became a more normal yellow, and then finally clear again when I was done.

When I reduced the volume of all my solvent, it became slightly darker, and now after freeze percipitating the crystals seem very dirty still ... almost brown. I just want someones opinion on the matter. Should i recrystallize with bestine? Does it matter if it's dirty if I'm going to make spice with it anyways? I'll try to get a picture up of it tomorrow, since it's only been in the freezer overnight so far.

 

[endlessness]

Check this link out, its relevant: IMPORTANT: spice color purity fallacy AKA is your dmt ok to smoke ? - DMT Discussion - Welcome to the DMT-Nexus

I would probably at least recrystallize part of it, then you can bioassay separately and see if you think its worth it