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Adding salt *decreases* my yields?? Options
 
merkin
#1 Posted : 10/31/2019 7:40:47 AM

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Well, I realise this experience runs completely 180° to pretty much everything I have read here but for me it is consistent. At first I suspected it was the bark not being so good but finally I did a little test to prove to myself I wasn't going crazy.

"Increased yield" is the opium of extraction and so I went for, first, Cyb's Max-Ion tek and then when I was pretty disappointed Cyb's original hybrid Salt tek but results were similar. Repeated 'Max Ion' (50g bark each) with 4 different types of salt - "organic" sea salt, uniodated, himalayan pink, NaCl AR lab supply, coarse uniodated salt. All delivered the same result - yield around 0.3%

I then tried a basic A/B - boiling the powder mix x4, reducing and straining, basing and extracting without any salt. Yield = almost 3x = 0.8%!

Since I am no chemist I question myself and methods. So in frustration and to at least try and get a handle on where the problem lay I boiled 200g of the same powder (MHRB), filtered and reduced to approx 2 litres. I split into 4 portions of 500ml. To three of them I added the salt solution proportional as per Cyb Max Ion (30g/50g bark and liter of DH20). Then I did the basify to 12+pH and extract x3 on each of the four with the same solvent (1-1-1 mix Hexane, nHeptane, Zippo Black).

Results: (as "scientific" as is possible for me trying to do everything the same)
1. Himalayan Salt - yield .35% (178mg)
2. NaCl AR Salt - yield - .3% (152mg)
3. Uniodated Rock Salt - yield .3% (148mg)
4. No salt added - yield .95% (472mg)

The salt added yields were pretty much identical and the no-salt more than 3x as much. In all cases temp of the liquor wasn't above 40°C and the result was clean very lightly yellow crystals.

I have since done a complete extraction following the basic A/B on 100g MHRB (the same bark) - 4 boils, filter sludge...etc and got a yield of 1.4% - my best yet! NO SALT was used and I no longer feel like I'm going crazy!

Am I missing something here? I guess I will avoid adding salt from here on, but why is my experience 180° opposed to everything I read which seems almost universally to consider the salt teks as superior and high yielding?




 

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leratiomyces
#2 Posted : 10/31/2019 10:32:54 AM
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Do you mind me asking what the final volume of the 4 aqueous solutions was, before extraction with solvent.
Any emulsions in the four runs?
All four runs extracted with the same volume of solvent?
All four runs shaken with the same intensity and for the same time during extraction?

 
merkin
#3 Posted : 10/31/2019 11:03:26 AM

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Sure:
The total liquid for the four was around 3200ml before splitting into 4 bottle (saline incl).
Minimal emulsions, recovering always at least 90% of solvent added each time (50ml).
Pretty much equal treatment in terms of shake time and intensity etc.

My mission was to try and be as consistent as possible to get some semblance of proper comparison.

I find the first pull usually has the most emulsion/solvent loss and time taken to settle. From pull 2 it pretty much gets down to almost nothing and a nice clear separation line very quickly. I like to filter the sludge phase a lot before beginning with the base as my experience with emulsions when the sludge was in the bottle (like for stb) has not been ideal.

Emulsion on first pull - little bit frothy:

**Oops! Correction of total liquid amount - it was 2200ml *without* the litre of saline. Was 3200ml split 4 ways (I use a 750ml kjeldahl flask due to its nice long, widish neck for pulls- ie 4x~750ml is the liquid qty I was aiming for for each test sample).
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Eaglepath
#4 Posted : 10/31/2019 12:06:09 PM

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Thanks for sharing this. I will do an extraction soon and this time I will test without salt.

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merkin
#5 Posted : 10/31/2019 3:39:16 PM

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What made me stop and test/investigate:
I had been going through a bunch of powdered bark trying different solvents (due to lack of anything called "naphtha" in my country) and kept getting really crap yields. I was doing Cyb's Max Ion tek to the letter (no acid boils). I assumed that the only answer was that I had bunk bark.

Moderator wrote:
Edited.


Then I happened upon Gordo's video and gave his tek a whirl. To my surprise, using nHeptane as solvent (which I had used before), I was kinda blown away by the result which was waaay more than I had been getting previously. And very clean crystals too! So there was nothing wrong with the bark after all. I then tried a regular A/B which is what everyone recommends rather than gordo and learned to filter the sludge. Again my results were superior. Then when I went back to Max Ion mixed with filtered and reduced A/B boils, I was back in the low yields again! So now I thought it was the type of salt I was using...because everything I read says salt is good!
 
leratiomyces
#6 Posted : 10/31/2019 7:22:41 PM
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I'm still lost.
After you reduce your your aqueous phase you have about 2000ml, I'd this correct?
You then split his 4 ways?
Then to 3 of the experiments you add 30g salt dissolved in 1000ml water? Is this correct?
So your final aqueous volumes are 1500ml, 1500ml, 1500ml and 500ml. Is this correct?

If the above is correct, then can I suggest that extracting 1500ml of aqueous solution with 50ml solvent is not very efficient, and may explain the difference.

Perhaps I have not interpreted correctly.....
 
merkin
#7 Posted : 11/1/2019 4:57:44 AM

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After reducing from the acid (ortho phosphoric ~3.5pH) dH20 boils (200g MHRB bark) I had just over 2000ml finely filtered bark liquid.

- Then I split this into 4 bottles giving just over 500ml each bottle.
- Added 30g of each type of salt to hot ~300ml dH20 (3 types)
- Added saline to each of 3 bottles individually = ~800ml final volume.
- Added ~300ml dH20 to 4th bottle to bring volume to same as other 3, ~800ml to push solvent layer into the thin neck of the flask to pipette the solvent out.
- Then basified each bottle with ~50g NaOH directly into the liquid, confirmed pH12+.
- Then extracted each individually with 50ml solvent x 3 pulls (150ml total solvent each bottle, 600ml for entire process) heating each bottle every pull in water bath (anova sous vide heater) at 35°C. Solvent was never heated directly.

Make sense?

(Second pic - separation layer pull #2 onwards is usually very clean, all that bubbly frothy stuff is gone now and it separates quite fast from here on in)
merkin attached the following image(s):
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leratiomyces
#8 Posted : 11/1/2019 6:52:12 AM
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Thank you, makes perfect sense.
You've been meticulous in keeping conditions the same while altering one variable.
Given your attention to detail, I don't have an obvious reason to explain your results. Sorry.
But I will be pondering on a possible explanation...
 
Loveall
#9 Posted : 11/1/2019 12:16:20 PM

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So your final salt concentration is ~4%? You can try brining it up to 8% and see if you get better results. Just a thought, not sure if that's your issue.
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merkin
#10 Posted : 11/1/2019 12:46:00 PM

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Thanks Loveall. So if I understand you correctly I should basically try doubling the amount of salt given the above amounts of bark boils - ie add 60g salt per 300ml dH20 adding to the 500ml bark acid liquid?

I still have all the materials (did 3 pulls) - is it worth adding more salt at this point? I usually just do a final pull with xylene or toluene to FASA after leaving everything a week or two as I have found the fourth pull to be pretty worthless for freeze precip, with this bark anyway.
 
Loveall
#11 Posted : 11/1/2019 1:04:44 PM

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Yeah, 2x the salt may work better. I think in CYBs Tek one ends up with an ~8% salt solution, but someone correct me if that's wrong please.

And yes, you can try dissolving more salt (e.g. 34g) directly into one of the 800ml splits that is giving you issues. Test one out first to see what happens after a new pull. Good luck.
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leratiomyces
#12 Posted : 11/1/2019 9:00:32 PM
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You might want to try taking one of the low yielding aqueous salt solutions that has been already extracted x 3 with naphtha, and extract it with xylene x 3, then proceed through the usual steps. Measure what yield you get from the xylene extractions.

At least this experiment will tell you whether the issue is poor extraction of dmt or destruction of dmt.


 
merkin
#13 Posted : 11/14/2019 8:02:02 AM

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OK, adding extra salt as recommended had no material effect on yield. That pull (#4) yielded less than 40mg for both bottles I tried, while the unsalted bottle yielded 87mg.

Haven't tried the xylene yet but tbh I'm not that confident it will deliver much. But surely the spice is still in the soup? Or perhaps its been destroyed or made otherwise inaccessible. Nevertheless I will do it when I have the time.

I don't really understand the chemistry here, suffice to say I don't think I will ever add salt again!

In the meantime I just did a straight A/B pull alongside without salt on 50g powder and yield was 1.4% over 3 pulls. Pretty much what I was expecting. That definitely takes the bark quality out of the variables.
 
some one
#14 Posted : 11/15/2019 11:54:02 AM

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Interesting observation, thanks for sharing.
To be sure another person should try the same salt vs no salt test.
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Exitwound
#15 Posted : 2/18/2020 5:14:33 PM

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Wondering if someone has update to this, OP? Smile
 
Hailstorm
#16 Posted : 2/18/2020 8:13:39 PM

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I have searched through 10 pages of results, but nothing relevant comes up.

Does anyone know if there is a sound explanation on the forum of how an increase in the ionic strength of a DMT solution works on the molecular level?

Do added Na+ and Cl- "fit in the gaps" between water ions and increase the "charge density" of the aqueous layer, decreasing the interaction distance and increasing the number of ions interacting, so DMT has more ions around to "push off of" and "float to the surface" faster?

If so, is it really important how fast it moves out? And the separation speed is not important (outside of resolving emulsions), isn't adding net-neutral material (Na+ and Cl-) to the basic solvent only going to dilute it by placing extra Na+ ions in the way of OH- groups that could instead bond with DMT salt cations and free up the freebase?
 
merkin
#17 Posted : 2/19/2020 5:27:38 AM

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Exitwound wrote:
Wondering if someone has update to this, OP? Smile


Not much to update. Basically gave up on the salted 'soup' - even a Xylene/FASA extraction yielded very little spice while the other non-salted yielded a further ~250mg as fumarate.

I have since extracted on another 250g mhrb batch (same bark) without salt and perfectly happy with a ~1.8% yield. I have no knowledge to evaluate the chemistry of this as I just follow recipes, but as I said above I will not use salt again!
 
blue.magic
#18 Posted : 2/21/2020 5:49:58 AM

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Given that DMT freebase is practically insoluble in water, I would consider salting out unnecessary.

AFAIK it is used to improve partitioning coefficient in liquid-liquid extractions, but given the above, I would not use salt at all.
 
 
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