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BIG MISTAKE !!! on Rxtal PleaseHelp!!! Options
 
dropofahat
#1 Posted : 11/6/2010 8:47:09 PM

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abom thinks he screwed up big time on a recrystal with heptane

warmed up the spice in a tall shot glass and set in hotwater in a coffee mug to let the oils settle

(Screwed up here!!) put a piece of masking tape on top to keep out the air/particles

came back about 30 mins later and the adhesive from the tape melted down into the spice!!!!

abom could see the whitish glue mixed in with the spice!!

transferred the stuff to anther jar (got all mixed up) cause more adhesive was melting down the side of the shot glass

anybody got any ideas!!! to seperate or remove the glue?

abom has 1.5 gs of spice in there!!!


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WSaged
#2 Posted : 11/6/2010 8:55:25 PM

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I don;t know about separating the spice from the glue.

But I can advise on next time, covering with plastic wrap, sealed with a rubber band...then poking 1 or 2 small holes in the top with a pin to let pressure escape.

Keeps things clean & helps keep things contained if there is an accidental spin too.



Good Luck!

WS
All posts are fictional short stories depicting the adventures of WSaged!! None of these events have actually happened and any resemblance to any real persons or incidents is totally coincidence!!!!!!!!!!!!
 
dropofahat
#3 Posted : 11/6/2010 8:59:20 PM

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abom understands now, shouldn't have done it for sure. he thought it wouldn't melt

anybody????



abom is such an idiot, heptane is used for dissolving rubber cement!!! not to bright of me!!!



abom got the whole solution warmed up and it is clear now, what could abom do to pull the d from the hep
 
dropofahat
#4 Posted : 11/6/2010 9:44:42 PM

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pull it with vinegar possibly?

I'm dying over here!!!Laughing



warmed up the solution and it is now clear, so the adhesive is mixed currently (I think)

cooling it down the solution gets thick (lots of d in there), but I can see some deposits of greyish stuff on the bottom.
 
justine
#5 Posted : 11/7/2010 12:06:47 AM

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You could try to filter it with a coffee filter or a buchner+vacuum.
To see the world in a grain of sand, and to see heaven in a wild flower, hold infinity in the palm of your hands, and eternity in an hour.
- William Blake
 
endlessness
#6 Posted : 11/7/2010 12:15:37 AM

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personally I wouldnt smoke it and would move on to the next one, learn from the mistake... but if you really feel that its too much spice to lose, maybe make some extra big clean up. Redissolve in the solvent, salt with vinegar, defat, add base again, pull with naphtha, do a sodium carb wash, freeze precip and recrystalize.. and then see what you have at this point and decide if continue cleaning up or..
 
dropofahat
#7 Posted : 11/7/2010 12:21:34 AM

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thank you, endlessness and justine I thought I was in a vacuum there for awhile

yes, defintately will not be putting this in the bowl, but maybe it could be saved, possibley very easily?

I thought about doing a cleanup but not sure how to go about it?

maybe someone knows what the d will go into that any type of adhesive won't?

maybe vinegar? or as yousaid carbonate wash/

I've let it cool to room temp and it is crystaling like mad right know, but I have a thick paste on the bottom and the crystals are a very fine needle with a defined center, maybe a mix of the adhesive and d togehter?

could someone point a kem guy to this thread? I know there not probably monitoring the playpen, but I would think that one of those guys would have the answer.

any ideas would be much appreciated from anyone right about now!!

thanks again.
 
endlessness
#8 Posted : 11/7/2010 12:26:27 AM

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I just explained you what to do.... redissolve, resalt, defat, re-basify, pull, sodium carbonate wash, freeze precip, recrystalize.. Without knowing exactly whats in the glue we cant know what will for sure get rid, but these are many different clean up steps, increasing the chance of getting rid of unwanteds.. As I said, persnally I would avoid using that but if I did, I would do at least these steps I said, and maybe even recrystallize more than once
 
dropofahat
#9 Posted : 11/7/2010 12:28:58 AM

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your right, was hoping i wouldn't have to go the whole route tho.

thanks


just a few questions


defat after the vinegar?

I have lye, sodium carb, and lime. which base would be the best you think? (I know this is uncharted territory, any direction would help

I'll go thru the carb wash info, haven't done pone yet.

thanks for taking the time
 
dropofahat
#10 Posted : 11/7/2010 3:52:09 PM

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okay, shot glass with adhesive and spice mix was left out and crystals started forming and a glob of dark orange stuff sat at the very bottom.

broke of the crystals and proceeded to redissolve in hot water, glob got bigger. siphoned of the clear liquid on top and put in jar. left some liquid inside and the glob as well (shook up the glob and a white (adhesive?) film formed on top, glob is still cohesive with what I think is the adhesive) put that aside

took the clear (slightly yellow liquid) and poured 1:1 vinegar and shook until almost clear, seperated the liquid vinegar and salted again (this time the vinegar has a film between the bestine and the vinegar). first salting is clear as day tho. I don't think i'll combine these two for now

Got a question??

Defat?? it says use a solvent for defatting? if I use a solvent wont' the adhesive possibly go in it? or can i use another solvent? (I have xylene, naptha, bestine at hand)

I've looked it up and masking tape adhesive is a for of POLEYETHYLENE from what I can tell, not a lot of safety info, but doesn't seem dangerous (except maybe for smoking!!!!)
 
endlessness
#11 Posted : 11/7/2010 4:00:09 PM

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you shouldnt redissolve the crystals in hot water leaving the blob behind.. you should redissovle the whole thing in acidified (with vinegar) hot water and it will all dissolve.. then you defat using a solvent (and yes the point is to get the adhesive to get out of the water with your salted alkaloids), and this solvent is discarded.. then proceed with basing and extracting with solvent

also i think maybe you should spend some time checking the wikis and different extraction teks, as well as the FAQ.

good luck
 
dropofahat
#12 Posted : 11/7/2010 5:05:12 PM

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don't redissolve and leave the blob behind? I had asked for clarificaiton earier and you said "you already told me", so I took it for granted to redissolve the liquids. no details were given.

I spent about +/- 1 year of going thru this forum for information and have done many extractions all the while searching for answers and reading befor I even once signed up to request guidance or information.

I would love to spend all of may waking hours looking thru mislabled and hijacked threads to find a possibly similar situation or a step in an extraction that would give me an idea.

I request help for a stupid mistake I made in the newbie section, sorry for that. I guess I should have asked the standard "why is the sky blue" or "what is stb?" and I might have gotten a better response in the newb section.

don't worry about responding, i'll figure it out.
 
endlessness
#13 Posted : 11/7/2010 5:14:09 PM

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Sorry I dont understand..


quoting myself:

"you should redissovle the whole thing in acidified (with vinegar) hot water and it will all dissolve.. then you defat using a solvent (and yes the point is to get the adhesive to get out of the water with your salted alkaloids), and this solvent is discarded.. then proceed with basing and extracting with (new) solvent"

do you not think this is a good suggestion ?
 
dropofahat
#14 Posted : 11/7/2010 5:24:45 PM

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no I do think it is a good suggestion, but your previous directions from yesteday were a little sparse.

and i took them for what they were, and went ahead and redissolved the solven and threw away the blob (didn't think i would need it)

and went to mixing with vinegar and seperated. now i've got the vingar liquid with the d ( I know there is d in their because the solvent went cloudy when vin was added, now after shaking it is clear)

this has just become an experiment for now, i may or may not be able to save the work i put into this extraction, so be it.



 
endlessness
#15 Posted : 11/7/2010 7:36:15 PM

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as I said to many people in this forum: Never throw anything away before you get your final yield. DMT never disappears, unless you throw it away

Sorry if my instructions werent clear enough for you, I thought when I said redissolve in solvent, it was implicit that I meant redissolve the whole thing, and salt with vinegar I also thought was pretty clear that it wasnt just use hot water but water with vinegar (also because dmt in freebase form is barely soluble in water so I thought you would have figured you had to use vinegar so it dissolves as a salt). Next time Ill try to be clearer.

You say that your dmt is in there because solvent went cloudy. It may be so, or it may be otherwise, we'll only really know once you freeze/evap it. I hope it does work. If it doesnt, remember for next time to not throw things away.

good luck
 
dropofahat
#16 Posted : 11/7/2010 8:26:19 PM

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not a problem, I did redissolve in solvent with heat only, that is when the glob formed, but it had a film on it as well. I took that to be the adhesive, if i could get out the solids that I can see then I thought that might help. I also added more clean solvent because it was so saturated it was precipitating within minutes.

the glob did crystallize with d, but it was also solvent mixed in, if I can salvage some and learn in the process then i will go ahead. in uncharted territory here.

I went straigh to salt with the captured clear solvent and vinegar.

now i have salted vinegar (from what i can tell), there maybe no way to seperate the adhesive or not, but I will take y
our suggestions and move forward

thanksl
 
 
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