help base with sodium carbonate

[mumbles]

69ron has a good post on this where he explains to swim a ph of 10.x is enough to freebase almost all of the spice. So swim tested it out and then after extraction dumped a shitload of lye in there and extracted again and only 200mg extra came out (from 500g bark) which is normal for even non ultra basified extractions (diminishing returns and all that). So there seems to be a lot of misinformation around about sodium carbonate. Swim used shellite (naptha) and there were no dramas in fact he uses it in washes.

would SWIY mind sharing:

- how much mhrb?
- how much acidic solution (before and after reduction)?
- cooking or long soak?
- was plant matter filtered out?
- amount of sodium carbonate added to acidic solution?

SWIM will be starting an A/B tomorrow to see how sodium carbonate fairs for him, and the answers to these questions would help SWIM suss out a few details.

you know, if SWIY doesn't mind...

-500g acacia
-~7-8L before reduction, ~600ml after
-3x 2hr cooks
-yes all plant matter was filtered out
-as much as swim could. its weaker than NaOH so expect to use heaps and heaps and test the pH often
remember to keep the solution hot and the naptha hot during extraction spice needs the extra push to get in there it seems. good luck

 

[Dimitrius]

69ron has a good post on this where he explains to swim a ph of 10.x is enough to freebase almost all of the spice. So swim tested it out and then after extraction dumped a shitload of lye in there and extracted again and only 200mg extra came out (from 500g bark) which is normal for even non ultra basified extractions (diminishing returns and all that). So there seems to be a lot of misinformation around about sodium carbonate. Swim used shellite (naptha) and there were no dramas in fact he uses it in washes.

would SWIY mind sharing:

- how much mhrb?
- how much acidic solution (before and after reduction)?
- cooking or long soak?
- was plant matter filtered out?
- amount of sodium carbonate added to acidic solution?

SWIM will be starting an A/B tomorrow to see how sodium carbonate fairs for him, and the answers to these questions would help SWIM suss out a few details.

you know, if SWIY doesn't mind...

-500g acacia
-~7-8L before reduction, ~600ml after
-3x 2hr cooks
-yes all plant matter was filtered out
-as much as swim could. its weaker than NaOH so expect to use heaps and heaps and test the pH often
remember to keep the solution hot and the naptha hot during extraction spice needs the extra push to get in there it seems. good luck

Thanks.

Are there any issues in using limonene with sodium carbonate, instead of naptha?

 

[mumbles]

No idea sorry. This is all newish ground but its worth a try. Maybe swim could split the based liquid into two and do a trial?

 

[Dimitrius]

No idea sorry. This is all newish ground but its worth a try. Maybe swim could split the based liquid into two and do a trial?

He doesn't have any naptha. He doesn't want to work with it anyway.

He does have heptane.....but he is really doing this to see how it well goes. He's done quite a few extractions with calcium hydroxide and would like to get a more efficient, thorough mixing by using his hotplate/stirrer.

There shouldn't be a problem with using limonene....he thinks? right? Can't be sure unless he's sure.

Anyone use limonene in this manner with sodium carbonate? If so, any comments to share?

Would be grateful.

Edit: Well, he just mixed 20ml limonene with 100ml saturated sodium carbonate solution, stirred very well and it separated just fine. No mhrb of course. May be totally different with the mhrb.

Unless someone can say for sure there won't be a problem (i'm sure someone's done this?), he will do a test stir & pull on a very small amount of the reduced basified mhrb solution and see what happens.

Cheers! and thanks mumbles for the fast replies.

 

[biopsylo]

There shouldn't be a problem with using limonene....he thinks? right? Can't be sure unless he's sure.

Anyone use limonene in this manner with sodium carbonate? If so, any comments to share?

Would be grateful.

Edit: Well, he just mixed 20ml limonene with 100ml saturated sodium carbonate solution, stirred very well and it separated just fine. No MHRB of course. May be totally different with the MHRB.

Unless someone can say for sure there won't be a problem (i'm sure someone's done this?), he will do a test stir & pull on a very small amount of the reduced basified MHRB solution and see what happens.

swim had a problem with thick emulsion, but a HOT water bath broke it flat. there doesn't seem to be many folks who have gone the limonene/sodium carb route--yet.

vinegar--sodium carbonate--d-limonene--FASW w/pics - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus

 

[Dimitrius]

There shouldn't be a problem with using limonene....he thinks? right? Can't be sure unless he's sure.

Anyone use limonene in this manner with sodium carbonate? If so, any comments to share?

Would be grateful.

Edit: Well, he just mixed 20ml limonene with 100ml saturated sodium carbonate solution, stirred very well and it separated just fine. No MHRB of course. May be totally different with the MHRB.

Unless someone can say for sure there won't be a problem (i'm sure someone's done this?), he will do a test stir & pull on a very small amount of the reduced basified MHRB solution and see what happens.

swim had a problem with thick emulsion, but a HOT water bath broke it flat. there doesn't seem to be many folks who have gone the limonene/sodium carb route--yet.

vinegar--sodium carbonate--d-limonene--FASW w/pics - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus

Thanks biopsylo. Had forgotten about that thread. 700mg fb from very old, improperly stored mhrb seems pretty good....plus a little spillage, lol.

We'll see how it goes with well-stored, high quality root bark + stirrer/hotplate.

He is keeping notes and will post how it goes...measurement, methods and all.

 

[Dimitrius]

Anyone know if the sodium carbonate powder can be added directly to the reduced acidic solution?

Or is it for some reason necessary to use a saturated sodium carbonate solution?

 

[mumbles]

Its a weak base so it would probably be safe to add directly. Just stir it as its added and you should have no worries.

 

[Dimitrius]

Its a weak base so it would probably be safe to add directly. Just stir it as its added and you should have no worries.

Sweet.

Thanks mumbles.

SWIM should be basing by tomorrow night...or the day after tomorrow.

 

[biopsylo]

We'll see how it goes with well-stored, high quality root bark + stirrer/hotplate.

He is keeping notes and will post how it goes...measurement, methods and all.

wishing swiy the best with this one.
i was thinking about citric acid instead of acetic for the soak or boil might be preferable. any thoughts here?

 

[biopsylo]

another thought on using sodium carbonate:

what if after the acid soak/cook, the mix is condensed till it is like a slurry.
then in a pot or pyrex dish, one was to add heaps of carbonate and mix it in with a potato masher till it is semi-dry. adding a bit more hot water if necessary. in this fashion, it would be much more like basing out fumarate salts, where just enough water is used to moisten it.
obviously, one should have an estimate on how much sodium carb 'needs' to be added to fully basify, and reach maximum ph for sodium carb.
then wait an hour or so before pulling with d-limonene. keeping the whole operation warm would prob be advantageous as well.

does this make any sense, or would this be more efficient in an aqueous phase?

 

[Dimitrius]

We'll see how it goes with well-stored, high quality root bark + stirrer/hotplate.

He is keeping notes and will post how it goes...measurement, methods and all.

wishing swiy the best with this one.
i was thinking about citric acid instead of acetic for the soak or boil might be preferable. any thoughts here?

SWIM is using a 10% phosphoric acid solution...bring the water to pH 3.

 

[Dimitrius]

another thought on using sodium carbonate:

what if after the acid soak/cook, the mix is condensed till it is like a slurry.
then in a pot or pyrex dish, one was to add heaps of carbonate and mix it in with a potato masher till it is semi-dry. adding a bit more hot water if necessary. in this fashion, it would be much more like basing out fumarate salts, where just enough water is used to moisten it.
obviously, one should have an estimate on how much sodium carb 'needs' to be added to fully basify, and reach maximum ph for sodium carb.
then wait an hour or so before pulling with d-limonene. keeping the whole operation warm would prob be advantageous as well.

does this make any sense, or would this be more efficient in an aqueous phase?

Do you mean reduce it down, then add sodium carbonate and mix until it's pasty, but still wet?

where just enough water is used to moisten it.

Sounds like a method more suited for calcium hydroxide.

 

[fourthripley]

Its a weak base so it would probably be safe to add directly. Just stir it as its added and you should have no worries.

Adding carbonates to acids creates A LOT of CO2 and has a tendency to froth right up, leading to loss of much of your product- all over the floor- unless you are careful.

 

[Dimitrius]

Its a weak base so it would probably be safe to add directly. Just stir it as its added and you should have no worries.

Adding carbonates to acids creates A LOT of CO2 and has a tendency to froth right up, leading to loss of much of your product- all over the floor- unless you are careful.

Thanks for the warning.

SWIM plans to test a very small amount, both basing and pulling, to see if he encounters any problems.

He will be careful.

He will make sure to do the small test in a very large, over-sized vessel.

 

[biopsylo]

Adding carbonates to acids creates A LOT of CO2 and has a tendency to froth right up, leading to loss of much of your product- all over the floor- unless you are careful.

the idea here that i am entertaining has to do with this release of energy. (im no chemist, for sure).

when basing out fumarate salts with sodium carb on a dish with a minimum amount of water, there is hissing, and heat released. chopping it in at this stage seems to do a great job. its like the action is at the surface, and it is distributed by cutting it in.

my line of thought here is that if there is lots of extra water present, then the energy and heat released will be adsorbed into the water, and it might not be as efficient . i could obviously be completely wrong.

 

[amor_fati]

Something to take into account here:

As the conjugate base of a weak acid, a solution of sodium acetate and acetic acid can act as a buffer to keep a relatively constant pH. This is useful especially in biochemical applications where reactions are pH dependent.

The concentration of sodium acetate could completely cripple an extraction if not taken into account. This probably wouldn't effect a dryer technique so much, however.

 

[mumbles]

Interesting. Should probably stick to phosphoric or hydrochloric. Swim doesn't think excess NaCl will be a problem.

my line of thought here is that if there is lots of extra water present, then the energy and heat released will be adsorbed into the water, and it might not be as efficient . i could obviously be completely wrong.

If its added with caution and mixed in swiy will be able to gauge the amount of frothing and then speed up or slow down from there.

 

[Dimitrius]

So.....

- 150g mhrb

- 900ml h20 (pH 3) heated & stirred for several hours

- filtered & collected

- 700ml h20 (pH 2) heated & stirred for several hours

- filtered & collected

- 700ml h20 (pH 3) heated & stirred for several hours

- filtered & collected

- solutions combined & put in fridge overnight to allow any sediment to settle

- solution decanted off of sediment

- 1800ml solution reduced to 600ml, simmering on the stove, over a couple days

--> 100ml of reduced solution separated as a test

--> solution was heated & stirred while 13g sodium carbonate was added, 0.65g at a time (no frothing or bubbling up occurred, no matter how fast the base was added; solution gave of that ammonia smell)

--> solution stirred & allowed to react for 10 minutes

--> 20ml limonene added to solution while it was being stirred and heated

--> allowed to stir in for 5 minutes

--> wonderfully nasty emulsion formed, turning the limonene layer into an oily layer of brown foam

--> a hot water bath was attempted to break emulsion; it seemed to let up ever so slightly, but didn't seem to be doing the trick

---> SWIM was not happy; grrrrr


He put the 120ml test solution into a jar for later experimentation & possible recovery.

He's not sure what he will do with the rest of the solution. He will probably either evaporate it down and proceed with lime. He may try lye.

He's tired and sick, and will have to work on this at a later time.

 

[endlessness]

Salt is your best bet to break emulsions, loads of it