Re-X problems

[zargoman]

SWIM had 15g of very light yellow, fluffy spice after some extractions. While he is very content and .07 will easily send him and his friends into hyperspace, he has never been able to get any decent amount of white or shards. So he decided to re-x this 1g at a time, and now has about 1g left of slightly lighter yellow spice, and 1g of very dark orange spice. Something is very not right here.

This was his method:
boil pot of water, and into this put a pyrex measuring cup. Add 50ml of VM&P naptha to the cup, and wait a minute for it to heat up.

Add gram of spice, and stir for a few seconds till naptha is concentrated: decant, leaving a light yellow oily layer on the bottom.

Freeze-precip the decanted naptha, and add 20ml of naptha to the oily goop, decant into second jar, and freeze precip that too.
Pyrex cup was then washed with degreaser to remove oily goop, and then rinsed very well and lengthily under hot tap until cup was very clean.

On the first try, this yielded a few tiny, white x-tals, and mostly lighter yellow spice. This was not fluffy and white, and was actually fairly hard and took much scraping to remove.

The process was then repeated (4 or 5 times now), and seeing no increase in white crystals, SWIMs come here because there is no way 15g of spice which has always worked well could become 1g of hard, not crystal white, spice without SWIM not doing this right. Was this goop the oils? Drying the oils (which SWIM only started collecting on last attempt) has resulted in a hard, light yellow, spice-like substance. SWIMs going to buy some baking powder, convert it, and try a carb wash tomorrow.

What is going on here?

 

[endlessness]

Mistake 1 (VERY important one!) : you threw away stuff before your final yield was achieved!

Never throw away anything, because if something goes wrong, you can recover, but throwing away ends with this possibility...

So wait, you had 15g and you re-x 1g at a time, using 50ml for each g? So then you put together all the 50ml (x15=750ml naphtha) and freeze? or did separately for each pull? Hopefully it wasnt 50ml for the whole 15g.

Did you throw away your naphtha after retrieving your crystals? How long was it freezed for? Maybe it wasnt saturated enough and not enough crashed, or maybe most of your dmt was still in that goop you threw away. Option B youre screwed, option A youre screwed if you threw post-freeze naphtha away, but if you still have it you can evap it down to a small amount and freeze again.

 

[zargoman]

Yes, that lesson has been learned the hard way

they were frozen separately, scraped out, and then the re-x process was attempted again, 1g at a time. It was frozen for 8 hours per round, and while not enough to crash all of it, was enough to see a decently thick layer of almost the same color spice as went in. New naptha was used for each re-x "round". The used naptha was not discarded, and is being frozen for the next 12 hours.

SWIM thought maybe the spice was being oxidized very quickly somehow, but that doesn't make any sense to him, as far as he understands the process. Alot crashed out just by letting it sit at room temperature for 30 seconds, and if one was to dip their finger into the hot naptha and air dry, it would be coated with a very thin light-yellow spice residue. SWIM is really confused as to why this happened.

 

[endlessness]

Ok at least you didnt tthrow the naphtha away. Considering one can re-x using 30ml hot naphtha per g impure dmt, you can hope that it simply isnt saturated enough and hence not much crashed out. If the used naphtha doesnt result in more crystals after this freezing, take it out of the freezer, evap till its just a little left (like a fifth or whatever) and freeze again. Hopefully there will be your crystals

 

[zargoman]

alright, that's happening right now.


Do you have any idea why it didn't end up being more pure/white/crystalline, even without the oily goop? The spice didn't look much different from before this was started, and didn't change at all in color after the first round was completed. Could it be my naptha is somehow off? Would a carbonate wash work better?

 

[endlessness]

did you do an evap test in your naphtha? Do you have an MSDS on it or can somehow check detailed ingredients?

would you say the goo that stayed on the bottom was a considerable amount compared to the dmt that dissolved, or was it just a bit?

 

[zargoman]

Evap test was good, no residue at all. The naptha is Plasti-Kote VM&P Naptha. This http://www.inlandreno.com/oldsite/pdf/m190001300.pdf MSDS has the same CAS number (100% Aliphatic Petroleum Distillates). The goo on the bottom was very significant, and throughout the entire process, easily amounts to over 8 grams... It was roughly 40% of each attempt at re-x... Which would explain the missing ~12g. Is it possible that if the scale was off and the naptha was over saturated... any remaining spice would simply melt in the hot conditions... in which case the goop was a little bit of plant oil and lots of spice?

 

[LandOfOz]

I would say you are not actually rexing, just redissolving.

when you heat naphtha you will pull all the dirties too. you either need to use a huge amount of room temp solvent then evap-->FP or do a series of jar switches.

the following is the almost ritual i perform. its overkill and many steps but its the best part of my day when i do it. my fav part of the whole dmt extraction. there are much simpler and better written directions out there. if you are using a waterbath to heat yoru base liquid and solvent you can actually just do the multi-jar decanting process outlined bellow when you remove your solvent from the jug.


first i dissolve my funky 1g spice in 50ml boiling heptane. this will form yellow hep and a layer of oily dark stuff at the bottom. remove 90% of the solvent and add clean solvent to the jar. heat to a boil and decant 90% of solvent. you can do more pulls, but the more you do the more of the dirties you dissolve. i do it until the hot solvent nolonger crashes spice out when i blow on it(about 2 or 3).

the idea here is that most of the contams will fall out of solution first and stick to the jar. each time u change the jar you are removing a % of the contam.

freeze the now saturated solvent(can be done in an hr or two as most of the dmt will fall out t room temp. oryou can evap in 15min, its up to you but it is 15usd/quart here)

this will give you damn clean frz-precip style fluffy spice. the solvent should still be stained yellow.

you could either repeate this, or go onto the extended naphtha cleaning/crystal growing, or be done.

for this you take your now cleaner spice and dissolve in a large amount(lets say 150ml) naphtha. heat and stir until dmt is in solution. you dont need to boil for this one, just heat until you can see some fluid movement when viewed from the side. remove the beaker from heat and allow it to sit undisturbed for 20min or until it begins to cloud. decant the solvent into a new beaker. heat and repeat the process again. now frz-precip the solvent in a new clean beaker. should be very nice now. i like to form this into xtals.

to do this i dissolve the new spice in the smallest amount of clean naphtha you can. cover the spice in your beaker with solvent and heat. once warm start adding more solvent and allowing to warm until all the spice is dissolved. pull the beaker from the heat, cover, and set aside in a safe place. the longer it takes the temp to drop the better your crystals will be. you can even slowly turn down yout hotplate to lengthen this. i let the jar sit on my ceramic heating mantel until its cooled some. i also(overkill) wrap my beaker up in a shroud of insulating fabric that was once a heat shield inside an oven. but whatever, thats all not needed.

just cover the hot solvent and slowly bring it down to room temp. then open the jar and set in an air stream. evap the solvent all the way orevap until xtals are desired size then decant and fp for a faster go at it.

google growing big crystals. it applies to dmt perfectly. ive used a seed crystal in saturated heptane just as it cooled enough to start crashing out. got damn near all the spice in the solvent onto that seed.