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white precipitate in cold naptha, not crystals tho

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dropofahat

dropofahat

Rising Star
just going to jump right in, could not find a suitable answer for this after ahwile of searching (+weeks)

Lye, water, napthat STB

2 1 gallon jugs w/ +/- 200 grams mhrb (+/- 1gram lye to 1 gram material to 15 mls water each jug)

went with the +/- 80-100 ml naphta pulls (before went with more naptha, wanted to try this method out that I had read)

used distilled water in one jug, tap and distilled in another (distilled jug got new(just purchased) lye, other jug got leftover (+/- 1 year old) lye)

first couple of pulls went well (white to yellowish, one got filtered and humidity was high and while drying congealed back to mush)

After these pulls (using new naptha each time) this is what is happening.

Pull naptha (both jugs in one jar) and I put it into the fridge. It clouds over within 5-10 minutes, but instead of crystals on the sides a whitish cloud settles to the bottom portion (but suspended somewhat not all settled), some crystals (very few) will set on the sides and I will get a yellow crust sometimes where the top fo the naptha sets against the jar.

When I try and dry it out, I will get waxy spice (w/smell) but a acrid as well. Some of the naptha will drain (I use individual tea bags cut and put over a jar with a rubgber band for filter- works very well for crystals-small holes no spice gets thru, but not thick enough hold the spice in the filter) and it evaporated and was bright white with chaotic structure (not like spice) and had a yellow ring on the outside.

fats suspeneded?

lye in the napthat? tried a baking soda wash and when i refreezed the naptha, the white cloudy stuff just congealed better.

very stumped, hurting my flow, only +/- .7 out of 400 g's after 4-5 pulls (mhrb is older, +1 years, but was a an +/-.8% producer before, had it stored in fridg mos fo down time)

please do your majik oh sweet nexus. let me know if you have any questions.
 
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Buy some coffee filters. Consider an a/b. Did you defat the minosa? Sodium hydroxide isnt very soluble in naptha so you are probably seeing fats. You should be evaporating your naptha down before you stick it in the freezer.
 
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how long did it stay in the freezer?

I disagree with mumbles on one point, because I think an A/B with mimosa defat is a very wasteful process, but thats my personal opinion. STB will be just fine, just recrystallize your product if you're unhappy with that yellow ring (which can be many things.. Check this thread out )

As far as not crystallizing, well maybe its just very small crystals. I wonder if you left it long enough in the freezer. Leave for at least 12 hours. Also you can pre-evaporate your naphtha a little bit.

Regarding how much to pre-evaporate and how to recrystallize, check the FAQ.
 
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in the past I have had very good results with STB , white to yellowish white crystals no problem. never had to rextallize before, but not against having to do it. but somehow these pulls after the first couple are different, that's also why I went with the less naptha for less evap. First couple pulls went like majik, but similar pulls after are getting this cloudy white precipate.

I'm not an expert, but no spring chicken either and haven't had a problem with getting full on crystal growth within a couple of hours. I have left the whitish precipiatate in jar in the freezer for +24 hours, and no real changes except very small crystal growth and more congealed, defined yellow ring. In my experience, I have been able to see dots of crystals in just a few hours, and if it doesn't hit by then, I would need to evap down.

Has anyone seen this specific issue? or something similar? I have dried out the crystals/material from the whitish prec and it is waxier with a more acrid smell.

As far as the filter, in my opinion coffee filters are too thick for small amoutns +/- 500 mgs of spice pulls. Individual tea bags emptied and cut down the middle work perfect for me. lay in over a small jar and use a rubber band around the top to keep it in place and make a depression in the middle. take your jar out of the freezer, knock down the xtals, swirl, and pour into the filter, tea bag filter lets the solvern thru, but no crystals. the purer the crystals, the more that won't get stuck (very few do anyway). Pull the filter off and put it on a ashtray (clean) over a spoon or something(so it's not laying on the surface) and it should dry with a +/- 1 hr (cause of th airlfow above and below)

Also, if you get any xtals or wax on the filter, you can save the filters, put them into a jar with hot solvent and swirl, the solvenet will release the caugth stuff and you can recapture. I save al of mine.

on the lye, I am getting a chemical smell and when some of the naptha evaped off of my pulls with the "white cloud" it was a brigh white powder with chaotic strucutre? Lye?

Thanks for the help guys, any other ideas
 
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didn't get real solid answer on this. so I tried some experiments

only thing that I had done significantly different from previous was that I used very little naptha so that I could go straight to xtals. but as above after a couple of ok (not great) pulls, i started getting a cloudy precipitate, but no to not alot (1 -2) crystals forming. I would dry them out, but they wer very waxy, not crystalline.

So, i decided to put about 3 times more naptha in and let it sit for a bit, pulled the naptha and evaporated down to a slightly cloudy condition(1/4 the amount). threw it in the freezer and BOOM, got the whole bottom of my baby food jar thickened with crystals (+1/4 inch thick high) and all up the sides about 3/4 inch.

best pull yet on this run, not sure what happened.

I used more naptha and got cleaner crstals (new naptha for all pulls previous as well) and didn't have the white cloudy precipitate. go figuer, anybody got a hypthosis?
 
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To me, coffee filters are just simply inefficient. Spice gets caught in the fiber. Although this can be resolved by putting in warm solvent again, why waste the time? Jars are a waste too, way too much product loss from stuff stuck on the side. Once again this can be solved by redissolving, but once again, why waste the time. Get some flat pyrex trays and you'll watch your yields increase. Decant solvent in freezer, flip tray upside down for a few hours to get remaining out, then dry in front of a fan. Every single crystal can be scraped up at this point with a razor blade. No product loss, no wasted time.

Sorry, didn't mean to get off topic dropofahat.


How long did you leave your solvent in there before you pulled the first time? How about the second time?
 
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yes, coffee filters are too thick, but small tea filters (individual work well-especially with pure spice), but you do lose some even to the tea filter, but you do save alot of time since you drop it on the filter air can flow on top and bottom, I've had the dust dry and usabel within 30 minutes (low humidity day) after pouring.

and the dry the jar is okay, but yes you do have to dissolve, but not much loss.

when you say decant in the freezer, are you free precipating in a flat tray with a top, then decanting, the drying?


first pull was mayber 3-5 hours? next pull was +12 hours. I never had the above mentioned problem with cloudy whiteness when I had used more naptha, so I went back to that and it worked got a +.700 pull this last time and it 's looking strong.
 
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I like your idea, wasn't meaning to knock that or coffee filters... To each his/her own.


Yeah, what you said. SWIM does way smaller amounts than 400 g, more like 50 g's. Then he puts all four pulls into a 750 ml pyrex flat tray, evaps until cloudy, covers, then puts in the freezer. Once the precip has taken place, he then decants off into his collection jar for reuse. After decanting, he covers the tray again, flips it over in the freezer for a couple hours to get the rest of the solvent off the crystals. After that, take out of the freezer, take the lid off, then put in front of a fan for a half hour or so to get whatever remaining solvent may be in there. Once the tray smells like lovely spice, a razorblade retrieves the goodies with ease.
 
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I have had this happen also, I was warming up my basified solution in a hot water bath in order to draw as much spice into my naphtha as possible. The naphtha was very saturated. I was getting lots of clouds at room temp. once in the fridge I was getting very a fine precip ? Adding a bit more naphtha, maybe allows it to hold longer and form larger xstals at a colder temp? maybe more Naphtha holds more fat or impurities?

I'm not 100% sure. I wont be doing STB any more. I got good yeilds but I find the BLAB to be much easier and safer.
 
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heavenly, not a problem, i am going to try your style here on one of my next pulls. the tea filter works well for quick drying, but when you not in a hurry it would be nice to not have to have the extra steps/loss. the problem I had with the jars is it took so long for the bottom to dry out, and even after scraping the jar would have alot of residue. i've seen a few little pyrex dishes about the size of a half sandhwich that I think would work perfect for what you are saying.

house, yes that's what i was thinking. I would get a very fine precipitate, very waxy as well. maybe without a defat, the napthat is holding too much fat to really xtal out? my first couple were nice lite yeller, but after a couple of days of sitting, that's all I could get (very small cloudy precipiate). When I went to more naptha, problem gone.
 
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i get this white stuff everytime. i do 4 pulls and its usually on the latter 2 pulls mostly just the 4th. the 4th will usually be nothing but this snot like white jizm. ive left it for days at a super cold freezer and it never makes cystals.
when dried its a fine powder yellowish beige smells stronger than the dmt. i dont know what it is but its not pure NN-dmt thats for sure. it has a different feel when smoked and is much weaker in potency.

strange that you got it from the first pull. since i re-use my naptha during pulls i figure its some other alkaloid that saturates the nahptha but doesnt fall out until its super saturated by multiple pulls.
i dont know its just my guess...
 
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that is how I would describe it , jism like.

not on the first pull tho, after a couple.

it smells like d, but not clean, more acrid? gave my nose a little bit of irritation.
 
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dropofahat,


Not sure where you reside, but Walmart sells a flat 750 ml pyrex dish with a cover for $3.79

BEST $3.79, I've spent! I have about 20 of them because I use them for all sorts of extractions, they're very handy.
 
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I'm on my second batch right now and I've noticed the white jizm as well.
In the jar of recycled naphtha it looked like oil sitting at the bottom. As soon as it hit the tray with the naphtha from my pulls it turned into that milky white snot consistency.
 

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Dude, this thread is 6½ years old.

Welcome to the Nexus, BTW!

Have a look at the recently active Naphtha composition threads.

How did you recycle your naphtha?

EDIT: recrystallisation can be helpful, too. (Not as a means to purify naphtha, of course!)
 
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