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WET VS DRY spice wash + multi-batch question.

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hamhurricane

Rising Star
do you all do the wash on the spice while its still wet in the filter, or wait for it to dry out either in the collection dish (or on the filter) and then do the sodium bicarbonate wash?
i think the wash would be more effective on dry crystal, but could also loose more product, no?

ALSO

if swim has a couple of pulls some of high purity (unwashed or recrystallized) white spice, as well as some dingy yellowish spice, and some REALLY dingy brownish spice can they all be mixed together and will the spice sort itself out, or should the batches be segregated?

thanks!
 
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Swim always washes with cold ammonia. He usually mixes all the spice together then x-talizes, at least twice. He has never done a wash while wet i dont think. I would say that it would most likely wash away more spice than dry. You can mix the spice together if you dont mind, its all going to the same place anyway, but i suppose you could not, tasters choice. Maybe Swim will do an experiment next batch and divide the pull before it goes into the wash, and try to see if theres a difference in final weight.
 
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I always wash the naphtha with a saturated room temperature baking soda solution. I loose very little spice this way and it removes oils and any residual NaOH (at least a taste test/smoke test tells me it does). 2 minutes of swirling and seperate.

I wouldn't wash the actual crystals, you'll loose too much and it only washes the surface area of the crystal. Washing while spice is in solution seems to be the best way to get all the nasties out with minimal yield losses.
 
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acolon_5 said:
I always wash the naphtha with a saturated room temperature baking soda solution. I loose very little spice this way and it removes oils and any residual NaOH (at least a taste test/smoke test tells me it does). 2 minutes of swirling and separate.

I wouldn't wash the actual crystals, you'll loose too much and it only washes the surface area of the crystal. Washing while spice is in solution seems to be the best way to get all the nasties out with minimal yield losses.
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i have never heard of that method, it sounds very good. could you please write the steps down for swim? directly after the pulls have been collected you do this, or after they have been evaped and redissolved into a supersaturated solution? what is the ratio of water:naptha for 1 gram of spice for example, and approx how much baking soda is used. does this improve the color of the spice making it more clear/white etc?


yes i completely agree the idea of pouring ammonia over my crystals and watching them sift through the filter makes me cringe.

and after this is the product fully smokable or do you recrystalize again after the baking soda wash?

the reason im hesitant to combine my batches is one is REALLY dirty (def has brown stuff from the water layer) and i would hate to contaminate all of my spice while trying to clean it!
 
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adrian89987 said:
baking soda removes the oils as well?
Click to expand...

It sure seems to. Yellow oily spice dissolved in Heptane, washed with baking soda water, and completely evaporated down left clear crystals, no oil layer, no discoloration. I assumed the washes were somehow removing some of the discoloration. I always do my wash when recrystalizing.


Sorry I don't have exact numbers and volumes for you, but I don't measure them out. Follow the steps below and you shouldn't have any problems.

Steps:

1) get a glass and put a teaspoon of baking soda in it. Fill with about 100ml luke warm/room temperature water. Stir, stir, stir. It will not all dissolved, but we are making a saturated solution so that is fine. Let all soilds settle.

2) Dissolve freeze preciptated spice in enough naphtha that is does not cloud upon cooling. Less is better, but use enough to prevent precipitation. I use 1/2 pint canning jars for this.

3: take a baster/syring/nasal aspirator and suck up some of the saturated baking soda water...do not get any solid baking soda in the baster.

4: add until the volume of baking soda is about 1/4 the volume of naphtha.

5: Swirl around for about a minute, do not shake, do not heat.

6: After swirling I usually take my nasal aspirator (I like it better than a syringe or a turkey baster) and suck up some of the naphtha layer and squirt it into the baking soda layer...not sure if it helps or not, but it is what I always do. It just mixes it up a little better and it separates pretty quickly.

7: remove naphtha layer (top layer!) save and recrystalize normally (freeze or room temp, your choice :))

8: Trash baking soda layer (bottom layer!), or add more naphtha and attempt to recover any lost yield (I've tried without success, just not enough spice in there).

I imagine that this would work with naphtha just pulled from the basified mimosa juice (uncrystalized)...however, I like to freeze precipitate first. It seems to get a much cleaner product.

With the method I have outline above I have taken yellow oily freeze precipitated spice that badly burns the tongue and turned it into clear spice that no longer burns (just a little bitter). My best batches of spice were made using this technique.

The taste and vaporization also seems to be improved.

Yield loss from about a gram is about 80mgs. I've read some threads about how yellow spice is better/smoother than clear spice. I dissagree 100% I think that crystal clear/white spice gives the best experience. I also think that after recrystalization melting it down in a hot water bath gives a denser, easier to smoke, and for some reason more potent spice.
 
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wow !~ really good tek tips ! I mean it - serious organic chemist notes from the bench-top ! ... but howcome I never need to wash..? What, am I lazy or something ..? .. not much of an organic chemist, perhaps. Also I always want to keep the oily dmt.

I don't really have NMR-spectrometer-proof of the purity, but I believe there are two colours for dmt-freebase that are 'pure' enough extracts to smoke, uncontaminated-oily-yellow and pure-white/see thru-shards. I keep both separate, and the yellow oils are a plant product ( I am assuming. ) The yellow spice is 'harsher' for sure, and the white is smooth as silk, unnoticeable even. But the difference is tollerable, I find.

I also belive that the 'brown', blackened or all-yellowy looking extract is highly contaminated and needs washing ... what's the browny-black stuff..? who knows... clathrate clutter and the whole gammut of gunk .. that is also being washed out...

I keep the ~10% yellow stuff as 'special' dmt, it includes 'jungle' alkaloids that make it way different, so why wash it white again..?. The oils conveniently pool-out in the (tilted) evaporation tray - yellow spice in a corner, and white, scintillatingly-seethru shards grow all around them. ... it's ready to scrape-and-smoke...! Add a little yellow to the white

But that browny-pulp-mill contamination colour... well it's going to make organic chemists out of all of you ! STB's and all that purifying - it's way more complex chemisry to have to master !

for eg, I got carried away looking things up - Just look at the keywords in here, about clathrate formation - they use the term "self preservation" - reminds me of dmt 'running' for it's life to form clathrates or find naphtha...




and then this one ... Clathrates are a broad class of molecular structures involving gasses, solids and liquids. They are studied in detail,
formed everywhere, in nature, in the lab, they are found in space, and ... in our extract jars ...



From this article we can glean the terms "guest species" for dmt-freebase, but what's the "host species" made of ? What's it's molecular structure at pH 11, 12, 13..? I have a hunch that "host species" are also stuff we need to'wash' out - cages of other molecules that trap contaminants.
 
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For clarification, I only do A/B extractions with pH pulls at ~11.5

However, I still find a need to occasionally do a wash. I can't always keep my pulls at 5-10 minutes. With long pull times the naphtha does pull some oils out (and probably some lye as well). I find the wash takes care of some of this.
 
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ayyyy

ok swim was about to perform this procedure, but it seems there is so much conflicting info about what to do, some people caution against the sodium bicarb wash because they claim it polarizes the spice and you loose too much product, is your method different acolon?
SO MANY WASHES!!
activated charcole, sodium bicarb, sodium carb, ammonia, and pure rechrystalization? how can anybody decide?

honestally im leaning twords just recrystalizing without a wash, wont all the discoloration/sodium hydroxide sink to the bottom leaving fine xystals?
or should i just do the acolon wash? swim is in hurry and might do an ammonia wash, but the idea of loosing 10% makes him shudder, what to do?
thanks
 
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honestally im leaning twords just recrystalizing without a wash, wont all the discoloration/sodium hydroxide sink to the bottom leaving fine xystals?
or should i just do the acolon wash? SWIM is in hurry and might do an ammonia wash, but the idea of loosing 10% makes him shudder, what to do?
thanks
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your crystals may also sink with the oily stuff.

sodium carbonate pH 8.5-10 or so works really good and is simple. it wont harm anything. It will help remove any residual lye (just in-case).

the yellow oil always went away in my friend of a friends case when they recystallized in warm hexane and decanted off the hexane after freeze precipitation. they oils remain in the hexane because they are very soluble. if one evaporates that hexane you will find the yellow oil.

also note that DMT oxidizes easily and yellow discoloration of crystals is probably a sign of this. yellow oil on the other hand is probably some other plant compounds. just a speculation.

i would not be so worried about people expressing high losses with doing washes. it may not be being done correctly and hence loss. if you have basic water DMT is not soluble in it. its that simple. its way easier to do by pouring the basic water through your organic solvent.
 
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I hadn't heard that it was possible to do a wash with sodium bicarbonate (baking soda), infact I'd understood that you needed Sodium Carbonate (washing soda) for it to work right. Glad to hear otherwise though. Can anyone compare the 2 washes - I've only used Sodium Carbonate. With it I've added 1/2 quantity of SC to solvent and shaken vigorously, as it doesn't form an emulsion. I don't know how well this would work if some of the MHRB sludge was retained in the naphta. I then removed the SC water and did two washes with pure water to remove any SC retained in the solvent. Result was white, though with a slight yellowish tinge, spice.
 
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Sodium bicarbonate is an amphoteric compound. It has a pKa of 6.3 in water which causes aqueous solutions to be mildly alkaline:

HCO3- + H2O → H2CO3 + OH-
Sodium bicarbonate can be used as a wash to remove any acidic impurities from a "crude" liquid, producing a more pure sample.

Sodium bicarbonate reacts with bases:

NaHCO3 + NaOH → Na2CO3 + H2O


This is from Wikipedia. I am not so good with my chemistry, but it appears to have a pH of 6.3 in water, is that right? This seems way to low. However it does react with sodium hydroxide to create water and SC.... Can someone help me with this. What is the max pH that sodium bicarbonate in distilled water can reach? I mean honestly I'm not too worried as my loses are minimal, but if I understand correctly it seems like some of the spice could be converted back into a salt, is this correct? If it is correct, what salt would form? This also means that if this wash was let to sit too long losses would be substantial.
 
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pka is different then pH. pka is the pH at which half of the substance theoretically is ionized and the other half is neutral.

you can fit about 8 grams of sodium bicarbonate in 100mL water so whatever the pH of that is, is about the highest pH you can get it to be. you can do some math to figure that out (if you really want too).

sodium carbonate is more basic and you can dissolve more of it in water.

although i don't see too many reasons why any of these compounds or any basic water solution would cause you to lose spice in a wash, my friend of friends use sodium carbonate and that works fine. there are ways to prove this but it takes some precision and is more work then really is necessary. alright well there is one thing. sodium carbonate and sodium bicarbonate make good buffers. they keep a solution from changing its pH drastically when you add another base or acid. this may make them better then ammonia.

the whole thing is if the water is basic DMT is not soluble in it. you could technically use NaOH however the whole point is that people are trying to get rid of left over NaOH.
 
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swim rexytalized two batches, the first was the REALLY dirty bath, and swim dissolved and kept pouring off letting the black goop settle to the bottom and pour off, pretty crude but it seemed to work ok.

the second gram of yellowish spice just all settled to the bottom and what was poured off seemed to contain nothing a sodium bicarbonate wash will be the next step.
 
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hamhurricane said:
swim rexytalized two batches, the first was the REALLY dirty bath, and swim dissolved and kept pouring off letting the black goop settle to the bottom and pour off, pretty crude but it seemed to work ok.

the second gram of yellowish spice just all settled to the bottom and what was poured off seemed to contain nothing a sodium bicarbonate wash will be the next step.
Click to expand...

Let us know how it goes! If you can. get a before wash and after wash weight on your crystals.
 
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ok acolon my friend has finished the procedure, the two main difficulties were deciding how much solvent to use, you said so much that it would not fog upon freezing, which would be more than in the initial pulls meaning for a gram i would be working with approx. 500ml seems like way too much?

my other problem was when melting down the unwashed dmt a fatty oil immediatly would settle to the bottom should swim just keep pouring off from the oil or dump it in as well, how much dmt does this oily crud contain? i poured in as much as wouldent stick to the sides of the beaker (its really sticky) and it fell to the botom of the sep funnel, then stuck btw the water and the naptha layer, the naptha did not become clear after washing nor did the sodium bicarb soln turn cloudy...
its in the freezer now, will update

EDIT: the amount of solvent used was perhaps too little as the soln fogged after about an hour of freezing, acolon do you think this might have reduced the yields, i still have the water, is sodium bicarb insoluable in naptha?
 
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