• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Sodium carbonate wash - impossible emulsion?

Migrated topic.
West-en

West-en

Rising Star
So, for the first time I decided to try a sodium carbonate wash, mainly to get a purer product. A naphthapull was placed in a airtight container and a water solution of Na2CO3 (converted from NaHCO3) was added (about half the volume of the naphtha). Then, I - as many had told me - shaked the hell out of it for a little more then 30 seconds maybe, I then let it rest and left the place for an hour or so. Well, when I returned it didn't look like I expected.

There was a foggy water layer in the bottom, and a much less thick layer of foggy yellow naphtha on the top (don't know if it's more or less pure-looking). But, in the middle there was a huge clear white layer, which I at first thought were some precipitation. This is not the case however, it seems like an emulsion of some sort (very milk-look-alike).

So for a couple of hours I've tried getting rid of this and it just won't let go. Removing and adding more water to clean out the Na2CO3 does not seem to improve the case, and by just decanting the naphtha-layer I know I've lost like 75% of the yield.

I was told this should not happen, so the question is of course what I've done wrong? How concentrated solution of Na2CO3 should I have? (Eyeballed a decent amount) How do I get rid of this? Any ideas would be greatly appreciated! 😉
 
Sort by date Sort by votes
A very tiny pinch of sodium carbonate is enough

SWIM never had any emulsion in this step, even shaking the hell out of it... thats weird!

SWIM would try adding more water I guess, but you said you already tried...

Maybe pouring loads of pure salt, like with usual emulsions, could work..

tell us how it went (and lets see if anybody else has anything more to say)
 
Upvote 0 Downvote
Fiashly said:
"water solution of Na2CO3 (converted from NaHCO3)"

Could it be that there was left over sodium bicarbonate in the solution? Just guessing.
Click to expand...
According to the wiki, it does not seem to be a problem. Let me quote:
Get a glass and put a teaspoon of baking soda (or 1/4 teaspoon of sodium carbonate) in it. Fill with about 100–150mL 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.
Click to expand...
Since it accepts baking soda as a fine alternative (NaHCO3) to washing soda (Na2CO3), I can't really see it as a huge problem. Though I'm quite certain my sodium carbonate is in fact, pure sodium carbonate (excessive time and heat in oven).

Since posting this thread I've been dumping huge amounts (well, quite a bit at least) of table salt (with iodide if it matters) into my ugly emulsion. It actually greatly improved the speed of water separation. A huge layer of water was quickly formed on the bottom, but hardly any more naphtha (a little bit, maybe). The naphtha seems to be trapped inside the middle layer, the emulsion, even though more water has left it.
How can I free this naphtha? Should I try heating?
 
Upvote 0 Downvote
Emulsion dissolution done! My biggest yield ever is now precipitating in the freezer.

How to get rid of this kind of emulsion:
1. Heat to 30-50 degrees Celsius in waterbath.
2. Add salt. Loads of it. The layer of salt on bottom of jar before it all dissolves can be 1/10-1/5 of the thickness of your whole solution. If you have less water than naphtha, add some.
3. Await formation of waterlayer.
4a. Suck up and squirt out emulsion into the waterlayer with a large syringe. Repeat until homogeneous.
4b. Stir gently to make the emulsion widen over the waterlayer, but not enough to break your naphthalayer.
5. Repeat 3-4 until the divorce of those layers has been completed!

Did wonders!
Peace. 😉
 
Upvote 0 Downvote
I just had a similar thing happen (first attempt, btw) and this is the only web page I finally found that was relevant.. and solved my problem, so thought I'd post.

Differences for starters is that I let the sodium carbonate wash stay in very briefly, disposing of it within a couple minutes...at least until the last couple water washes when it took longer to separate, but sounds like the same situation.

I believe I used too much soda, and there wasn't enough water in the world that was gonna pull it back out again, though I tried. (half this batch got 1 round of soda wash, then pure distilled water 2 times, the other half got it worse because I used 3 sodium carbonate washes until I switched to water ).

could see very thin solvent layer right on top, but just below, completely cloudy (top view)

added-salt-to-sodium-carbon.jpg


As soon as I sprinkled salt in, the solvent layer appeared. Adding heat helped bust up the fatty globs of emulsion, but more and more salt was required for the one that was super saturated with soda.

added-salt.jpg


Now I have a very clear result, but is too dilute for freezer. so am going to let it evap for a couple days and try again.

my concern is that i washed it all away... I wonder what the results were of the original poster..? I will let you know how it goes
 
Upvote 0 Downvote
it wasn't green until the sodium carbonate wash --round 3 or so (i mean i let some evap on its own before starting, and it left no trace)... ok, so water wash was bad idea.

sooo when it was swimming in sodium carbonate, I should have just added salt. got it. still have some to work with so will make adjustments. thanks
 
Upvote 0 Downvote
so you are extracting dmt?

Im sorry but it shouldnt be green, there's just no way! One or more of your chemicals used has some potentially toxic additive you are unaware about. You should try finding out which chemical and find a better one.. I personally would really never ingest/vap any of the stuff coming from this green naphtha
 
Upvote 0 Downvote
Uh, ditto on the green... and how could sodium carbonate possibly be responsible for the color? I would scrap that and start from scratch. You don't want to be ingesting rust inhibitors, and it looks like you used a bunk solvent.

West-en - There's never a need to leave a sodium carbonate wash to sit for any period of time. Get it in, get it out - that's the ticket. Pour in enough to raise the PH to 9 or 10 (it just takes a pinch - and as far as volume goes, you only need maybe 10% distilled water to solvent), shake it up for about 30 seconds, pour off the clean naptha and repeat as necessary. And if you're finishing up with a water only wash, get it in and out even faster.
 
Upvote 0 Downvote
thanks for all the feedback. i'm grateful.

i agree that it seems most likely it would be the solvent that made it green (becaue this is a known issue), but I really don't think it was the naphtha in this case. As I said, it did not turn green until the sodium carb wash, and then not until the 3rd wash -->I know now, and this is big: I used way too much sodium carbonate.

I believe the green is either because I used WAY too much sodium carbonate, or because the sodium carbonate is not pure.?? What I did was to make a saturated solution (sodium carbonate and distilled water), then squirted about 1/2 cup of the solution into each 2 cups of pull (2 batches). I suppose that alone is like 3-4 times too much.. but then: For one of these I did this 3 times (!), so when I say emulsion, I mean it was mostly a blob of soda. The 2nd one wasn't as bad because it only got the soda wash one round (took much more salt to clear things up with the other one). Then both got a couple water washes. Why? well, i read it on some extraction guide and i'm experimental :p i suppose, but at this point I'm more interested in getting SOMEthing out of what i have left. lol. so i would be ever so grateful for further advice.

I see the ph prob of doing a water wash, but was hoping because of all the soda/base, I might still be OK.Long story short (also hadn't found info on the salt fix at that point). I have started anew (or 2nd round), but am still evaporating the green stuff just to see what comes of it (won 't use it though).

my questions at this point are

-is it more likely the green was from *too much* sodium carbonate (because i used an extremely large amount, i think), or that it is bad/contaminated? it's arm&hammer 'all natural super washing soda'

-my pulls are quite brown (due to prepowered bark if what i've read is true), should I just go with those and not worry about a wash, maybe esp because I'm new at this? (btw, i'm committed to STB for now because that's the state of all the bark i have)


thanks again for your feedback. i welcome additional perspective
 
Upvote 0 Downvote
Stick with the conversion to ensure a pure food-grad material, but SWIM has used super washing soda with naphtha, heptane, acetone, and IPA and has never seen green anything. Check to see that contains no phosphates or perfumes, should say right on the box. SWIM's not sure, but he doesn't believe contaminated naphtha is green right off the bat, rather it turns green when mixed with certain things.
 
Upvote 0 Downvote
he doesn't believe contaminated naphtha is green right off the bat, rather it turns green when mixed with certain things
Click to expand...

hmmm, interesting. so... if i just take unwashed pull and precip and it's not green at the end, does that mean it is safe to assume it's safe? I suppose not.

only says 'contains sodium carbonate' which sort of implies there are other ingreidents, maybe.. but it is not listed more formally, like no official 'ingredients:...' section.

think what i'll do is take small portion of pull and do a sodium carb wash with a tiny bit --do it the right way with much less-- and see what color it is...
 
Upvote 0 Downvote
upon more reading, I see what you say (what you've all been saying too) that the naphtha is probably the problem, even if the greeness didn't show up til later on. seems I need to really start all over and use a different, cleaner solvent. thanks, all
 
Upvote 0 Downvote
update: Decidedly non-green results have been obtained from the same batch that produced the green, but this one did not get soda overdose. I'm hoping anyone who finds themselves in a similar predicament might find this documentation useful (and perhaps those with more experience will tell me if they think it's safe // what these results indicate). apologies for the cell quality pics

the image shows the color progression from 1) unwashed pull (darkest naphtha pull from same batch the green stuff resulted from), 2) thin layer in pyrex dish (after 2x sodium carbonate wash), 3) mostly white crystals

first-spice.png


While this does not prove that the naphtha is uncontaminated, it is supporting evidence that perhaps the sodium carbonate (or something other than naphtha) caused the green (i used many many did i say many times as much as was needed in the green images above)---> This time, for about 1 cup of pull I used only 2 tablespoons of saturated sodium-carb solution, for 2 wash rounds (pic 2).

It seems another (much smaller) factor in the green-ness may be the inherent greenness of plant material (??). (pic 1, you can see a green quality to the dark brown (granted the naphtha is in there too), and pic 2 greenish brown as well, but faint). The pulls are so brown. I was trying to track the color as I cleaned it up a bit, looking for the sources of that green. And it occurs to me that the brown aspect may 'clean up' better in a wash, leaving the green part behind. (will know more next time with same prepowered bark and different solvent)

I feel confident about the purity of this batch (my novice status considered) seeing how surprisingly whitish it turned out. Upon getting these results, I was re-inspired to check the original greenish-bluish stuff that's been evaporating. It is now slightly cloudy with little crystally bits, so it's now in the freeze. We shall see. I am still wary of it (its green phase), don't get me wrong, but would like to at least see what the final color is.
 
Upvote 0 Downvote
ok let me put it this way: The fact that there was ever any green at all shows that there are unknown (and as said, possibly toxic) impurities in your chemicals. BUT, the green might be only a secondary indicator, it doesnt mean that the only impurity present is green and neither it means that if using the same products and green is not there, you are safe.

as I said, I would personally NEVER ingest/smoke anything extracted with chemicals that at some point turned green, no matter if in the end one got a whiter colour product. I would say forget that and look for new products. I would say get new solvent (make an evap test and check label/msds and so on), get new sodium carbonate (making it yourself from pure sodium bicarb is the safest) and start all over again.

That being said, if you still wanna use your product, I would STRONGLY suggest AT LEAST getting new clean solvent and recrystalizing your crystals at least twice. but do as you wish

good luck!

(oh and, check this thread it relates to the subject here )
 
Upvote 0 Downvote
awesome, endlessness, that helps me a lot in deciding the right steps to take. I was planning on getting known-cleaner solvent, and see more the value of starting that way in the future, certainly. but you also helped me to get a better grasp for 'how clean/dirty could this stuff possibly be'. thanks for supplying me with some missing, very relevant details.
 
Upvote 0 Downvote
Back
Top Bottom