sodium carbonate wash on D-Limonene

[NamRa]

Can you do a sc water wash with D-Limonene the same way you would do with naphta ?

 

[endlessness]

Yes, any non-polar solvent can be washed like that.

Its not recommended to do too many washes if youre playing with a more water-soluble alkaloid like mescaline, because each wash might carry a little bit of your alkaloid away, in theory. But even then one or two quick washes with small amount of sodium carb water are recommended.

 

[CheeseCat]

Thanks for that endlessness. Wouldn't using sodium carbonate in the water wash encourage the DMT to migrate out of the NPS?

I pulled some D-Limonene yesterday and salted with vinegar but neglected to do a water wash. I was following Q21Q21's tek and there was no mention of washing the D-Limonene so it didn't occur to me. Do you think I need to water wash it still?

 

[endlessness]

DMT will not migrate to the sodium carb water, no, it is too soluble in limonene as a freebase.

If you already salted your limonene with vinegar, there is no point washing your limonene with a sodium carbonate solution since your alkaloids are already with the vinegar fraction. Assuming you used lye to base your mimosa/acacia/whatever in the first place, then the sodium carbonate wash serves to remove any polar impurities that may have accidentally come across from an unclean separation of the limonene, such as some sodium hydroxide droplets. If you salt with vinegar, any sodium hydroxide droplets will be neutralized by the vinegar and will become sodium acetate. Depending on how you are considering retrieving your alkaloids from the vinegar, you could have some sodium acetate impurity together with your alkaloids.

What are you planning on doing with the vinegar? How are you going to crystalize/store/consume your alkaloids?

 

[CheeseCat]

My plan is to evaporate the DMT acetate, add sodium carbonate, then pull with 99.8% IPA (BLAB tek, step 6 acetate conversion). And then dissolve the IPA onto herbs for changa.

Would the sodium carbonate step above, eliminate the need for a water wash?

 

[downwardsfromzero]

That's a different use of sodium carbonate. Try looking at exactly why each of these processes is carried out.

In the first case, the DMT is already in the freebase form, dissolved in the limonene. What do you think the purpose of washing the limonene with sodium carbonate solution might be?


So, what is happening in the second case, where the acetate gets mixed with sodium carbonate? How does it differ from the first? How might the desired outcomes be differing in these two cases?

What do you imagine the "need" for a water wash might be? Why do you think it may be necessary?

 

[CheeseCat]

I figured it was a different use but then considered it might serve a similar function. But now that I understand that sodium hydroxide is converted to sodium acetate when combined with vinegar I think it would be unlikely that the sodium carbonate step in the BLAB tek would be able to clean any sodium hydroxide contamination.

The purpose of washing the limonene is to collect any sodium hydroxide that may have been caught in the transfer. BUT I don’t really understand why sodium carbonate is used as I thought water alone can clean NPS contamination?

The sodium carbonate step in the BLAB tek is to enable the DMT acetate to be converted back to a freebase by raising the pH and making it transferrable to the polar solvent. I think I have that right? :?

 

[downwardsfromzero]

I figured it was a different use but then considered it might serve a similar function. But now that I understand that sodium hydroxide is converted to sodium acetate when combined with vinegar I think it would be unlikely that the sodium carbonate step in the BLAB tek would be able to clean any sodium hydroxide contamination.

The purpose of washing the limonene is to collect any sodium hydroxide that may have been caught in the transfer. BUT I don’t really understand why sodium carbonate is used as I thought water alone can clean NPS contamination? [* ]↓

The sodium carbonate step in the BLAB tek is to enable the DMT acetate to be converted back to a freebase by raising the pH and making it transferrable to the polar solvent. I think I have that right? :?

Thanks for taking the time to answer my little quiz :thumb_up:

I think you've essentially nailed it, there won't be any sodium hydroxide left because it has already been neutralised by the vinegar. A timely sc water wash would of course have prevented this stray extra little bit of (now largely harmless) contamination from ending up in your product but since you will be converting back to base you now have the opportunity to clean that up. Even though it was most probably only a trace of sodium that came over in the limonene it would still have the potential to throw off dosing measurements a tiny bit.

↑[* ]While water alone can in principle clean up the NPS, consider also that carbon dioxide dissolves in plain water - think how this might affect outcomes since this is an extraction of a freebase alkaloid. There are two main effects that sodium carbonate will have when in solution - can you name them?

 

[CheeseCat]

Ahhh, ok I think I understand now . Water can contain carbon dioxide which means it could potentially be slightly acidic. Adding a small amount of sodium carbonate raises the pH and protects the transfer of the freebase DMT.

Sodium carbonate in solution raises pH and also helps to attract base impurities.

So with regard to my original question (post #3), it’s not too concerning that I didn’t sc water wash my limonene pull because any sodium acetate impurity (neutralised sodium hydroxide) is largely harmless (but may throw dosing off a bit). AND when you say, “since you will be converting back to base you now have the opportunity to clean that up”, you are referring to the sodium carbonate step in the acetate conversion that not only converts the DMT acetate to freebase but also absorbs the sodium acetate. Then, using 99.8% IPA I can safely pull the DMT freebase and evaporate on herbs. Is that correct or am I a bit off?

 

[downwardsfromzero]

Yes by Jove, I think we're getting it The other thing about sc solution that I was hinting towards is ionic strength. Having dissolved salts present in the water decreases the solubility of DMT freebase in it and thus reduces losses during the water washing process. One more thing, the basicity of the sc won't enhance its capacity for absorbing lye - that remains sufficient nonetheless.

One thing to watch out for is that the freebased paste with the sc has been completely dried out so that there is the minimum carry-over of sodium salts by moisture in the IPA pull. Of course, since you'll be evaporating onto herbs this could be judged to be less important. Furthermore, if your IPA is freshly opened the 99.8% should still be valid but it will absorb moisture from the air fairly readily until it reaches the azeotropic concentration (~91% v/v or 87.7% by mass) where it becomes desirable to lower the water concentration with a drying agent.

 

[CheeseCat]

Thanks downwardsfromzero! That was a big help. Very interesting about the IPA azeotropic concentration! Thanks for the detailed response

 

[Sakkadelic]

when i tried pulling with ethanol from a sodium carbonate and dmt paste in the past and using that to make changa, the changa never dried out due to sodium carbonate contamination pulling moisture from the air. I used 95% ethanol that I dried using magnesium sulphate but i think i did not do the drying properly. so make sure that your IPA is as dry as possible and the dmt/sc paste is dry when you do the pull, if you dry it and then leave it hanging before the pull it will reabsorb water.

 

[CheeseCat]

Cheers Sakkadelic. I'll buy a new bottle of IPA which should mean it'll be around the 99.8% mark. Once I've mixed the DMT acetate and sodium carbonate paste together I was planning to dry it thoroughly in the hot water cupboard and then immediately pull with IPA.

I've read you can also use sodium carbonate to dry IPA so maybe I'll give that a try at some point.

 

[downwardsfromzero]

Ethanol is fairly hard to dry completely. IPA is a little more forgiving perhaps since it forms a phase that is immiscible with aqueous solutions of high ionic strength. It does contain more water by volume in the azeotrope though, hmmm....

If you want to get really OCD scientific about drying out the SC paste, after the heat treatment you could seal it in a tub with some calcium chloride, magnesium sulfate [both anhydrous ofc] or dry silica gel as desiccant. Let that stand for several days to a week if you're not in any particular hurry.

 

[CheeseCat]

Would replacing sodium carbonate with pickling lime be a better option? I've read that pickling lime has poor solubility in water which should eliminate the chance of any base being soluble in the alcohol?

Are there any disadvantage to using pickling lime in this way?

 

[surquillo]

Ethanol is fairly hard to dry completely. IPA is a little more forgiving perhaps since it forms a phase that is immiscible with aqueous solutions of high ionic strength. It does contain more water by volume in the azeotrope though, hmmm....

If you want to get really OCD scientific about drying out the SC paste, after the heat treatment you could seal it in a tub with some calcium chloride, magnesium sulfate [both anhydrous ofc] or dry silica gel as desiccant. Let that stand for several days to a week if you're not in any particular hurry.

Fractional distillation with a dean-stark trap for dry IPA, one could also use zeolite 3a molecular sieves.
absolute ethanol can be achieved by distillation over elemental sodium.

Edit: Also, you can obtain fairy pure IPA by adding it into a strong basic solution of NaOH, it will separate layers, separate the bottom layer, neutralize with an acid and discard. Keep the top layer. I only did this with isopropanol. Reference: US4454359A - Process for drying alcohols - Google Patents

Would replacing sodium carbonate with pickling lime be a better option? I've read that pickling lime has poor solubility in water which should eliminate the chance of any base being soluble in the alcohol?

Are there any disadvantage to using pickling lime in this way?

Wash your extracts if they contain active contents with brine, if neutral use molecular 3a sieves

 

[CheeseCat]

One thing to watch out for is that the freebased paste with the sc has been completely dried out so that there is the minimum carry-over of sodium salts by moisture in the IPA pull. Of course, since you'll be evaporating onto herbs this could be judged to be less important. Furthermore, if your IPA is freshly opened the 99.8% should still be valid but it will absorb moisture from the air fairly readily until it reaches the azeotropic concentration (~91% v/v or 87.7% by mass) where it becomes desirable to lower the water concentration with a drying agent.

This is very helpful, I still have a few queries though downwardsfromzero. Firstly, why is sodium carbonate carry-over considered less important when evaporating onto herbs? Given that any carry-over may affect the accuracy of weighing/dosing suggests that sodium carbonate isn’t removed during the evaporation process.

I also came across this in the Dry Technique Extraction process section - "Decant and/or filter acetone and collect, being careful not to allow any particulates into the collection vessel. The bases used should not harm the quality of the product, but may interfere with the accuracy of weight".

I would have thought that even minimal sodium carbonate in the end product would be unhealthy to smoke? But it seems that minimum carry-over is considered ok and not harmful. This is actually reassuring as even though I was super careful pulling IPA from the sodium carbonate there looked to be very fine particles that may have made it through on the last pull.

I currently have some sodium carbonate mixed with A.floribunda flowers that were washed and reduced down to a small amount of liquid. And now there’s a strong smell of semen in the air! :lol:

 

[downwardsfromzero]

You're right about the dosing accuracy being affected. I was coming more from a perspective of the herbs remaining as a residue, combusted or not, and this residue would hold onto the sodium carbonate rather than the latter flying around as dust.

now there's a strong smell of semen in the air

Well, whatever floats your boat. Science can be pretty exciting at times

But seriously, you can just evap and repeat the IPA pull, with or without filtering. A handy trick for filtering smaller volumes is to use a glass Pasteur pipette with a small pea-sized ball of cotton wool. You can use glass or stainless steel drinking straws or turkey basters as a domestic alternative.

Get the packing just right and you can clean up fairly small particulates without too much trouble. Having some kind of stand and clamp is highly desirable for this; clothes pegs (the sprung type) are a possible starting point. Ingenuity is always your friend in the kitchen lab.

 

[CheeseCat]

Well, whatever floats your boat. Science can be pretty exciting at times

Haha :d I’m discovering plants can yield quite unusual smells! In this case, very reminiscent of the Ornamental pear tree. It’s not as strong now, thankfully.

But seriously, you can just evap and repeat the IPA pull, with or without filtering

Just to be crystal clear, if there happens to be a very small amount of sodium carbonate carry-over then this is considered harmless when smoking with herbs or vaping? (it’s likely the end product will be a goo with the sc (if any) trapped in it).

I still don’t really understand why it would be harmless to ingest though? Sorry if I’m missing something obvious! I guess I’m a little paranoid about the sc in the final product due to reading: “Direct skin or eye contact, or inhalation of powder or crystals can produce irritation, rash and sometimes burns” and “when sodium carbonate is heated then it decomposes to form sodium oxide and carbon dioxide gas is evolved.”

Thanks for the filtering tips! I found this video on filtering which illustrates what you’ve described perfectly. I should definitely be able to make it work:thumb_up:

 

[downwardsfromzero]

The decomposition to sodium oxide only occurs at ridiculously high temperatures (unlike many carbonates, it survives melting at 851 °C without decomposition), and sodium carbonate itself is significantly less dangerous than, say, the hydroxide. It's a question of amounts, too - and in this case the amounts are tiny. It should still be treated with respect in amounts above a mere pinch since inhalation or eye contact would be unpleasant at best, but we always wear eye protection in the lab anyhow.

FWIW, sodium carbonate slowly absorbs CO₂ and moisture from the air to form the sesquicarbonate and the bicarbonate. I really wouldn't worry about a few specks of the stuff, likely measurable in the microgram range but nor would I get complacent about purity because that's where your concerns could start to become more relevant. Sodium carbonate still belongs way down the list of scary chemicals - I'd rate it as no more scary than washing powder.