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vinegar--sodium carbonate--d-limonene--FASW w/pics

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biopsylo

Rising Star
EDIT: pics are at bottom of post...
Hello all~~
over the weekend, swim performed an extraction on 100g mimosa hostilis using the FASW tek developed by Jorkerst and others. swim wanted to try this tek without lye, and it was suggested to start with an acid reduction on the bark (a/b) prior to fasw, and utilize only sodium carbonate for base. swim took pictures, and thought it might be useful for others to post his results. so here goes. oh, and swim hasn't uploaded pics yet, so hope this works out! swim would recommend first reading the original post and tek for this method here:

this is a slight modification, and does take longer, but does not require sodium or potassium hydroxide.
1. cut mimosa bark with shears, and add small amounts to coffee grinder, and grind it to near powder, then weigh it.

2. swim mixed approx 6 cups spring water, and 1 cup distilled white vinegar. added 1/3 of this to pot, poured in mimosa powder, and simmered/very low boil for 1 hour. this is probably longer than necessary. the Ph was 2.
Next, pour off liquid from pot into quart jar, trying to leave all solids in the pot. Let this stand for a few minutes, and there will be a layer of sludge at the bottom of the jar. swim decanted the top liquid again into another jar, and returned the sludge into the simmering pot. Add another 1/3 of the water/vinegar to pot, simmer another 45 min. Again, pour off liquid into a glass jar, and repeat as before.
Add remaining water/vinegar, and simmer another 30-45 minutes. repeat as before. swim rinsed the spent bark with a bit fresh water and squeezed it all out. combine all washes, and simmer/reduce to roughly 600ml.

3. next, swim measured 80g sodium carbonate and dissolved it into 200ml spring water in a small jar. --Ph 13 (ph 13 is not supposed to be possible with sodium carb) best estimate with old ph papers.
4. then he added this water to the mimosa tea--Ph of tea now 12.

5. next, swim measured 75ml D-limonene, and poured it into basified mimosa jar. swim used 1200ml nalgene bottle. invert 20 times. swim actually shook it and formed a nasty emulsion.

(a quick note about compatibility of d-limonene and plastics....they aren't very. if you must, store it in PET plastic, but not long term. better to use glass or steel. the plastic pipette swim used started literally melting in d-limonene, and prompted him to look up the compatibility.
6. swim pipetted the d-limonene into a 70ml glass jar. here you can see the emulsion.

first swim added a bit sodium carbonate, then a pinch of salt to try to break the emulsion, to no avail. finally he put the glass 70ml jar, and the mimosa jar into a hot water bath, and it worked great!
7. swim added 75ml d-limonene again to mimosa jar, shook for a few minutes, then pulled it off as before. then for the third pull, swim used 50 ml d-limonene, for a total 0f 200ml. swim combined these, and poured thru a funnel with part of a cotton ball in the neck. droplets of dark base water got stuck in cotton. swim was careful not to bet too much in there.
here is the spice saturated d-limonene, notice a little loss-also not the best measuring equipment!
8. time for fasw-fumaric acid saturated water. 450mg weighed, and dissolved into 75ml distilled water. 25ml added to d-limonene, and inverted 20 times.
9. suck the fasw from the bottom of the jar, into another clean jar. added another 25ml fasw to the d-limonene, and repeated as before. then again with the remaining fasw. swim then combined all the fasw that is now laded with spice, poured it thru cotton, and into glass evap dish.
swim scraped it up after fan drying, and weighed 1.42g spice fumarate.
10. time to freebase. swim measured 2x the weight of spice fumarate of sodium carbonate, and dumped it onto the spice in the evap dish. started to cut it in with 3ml distilled water.
fully basified, and chopped:
11. next swim dehydrated 50ml acetone with .5g sodium sulfate (didn't have any baked magnesium sulfate) the sodium sulfate did not clump, or change shape, so swim assumed acetone was quite dry to start.
12. swim added 1/3 of the dry acetone to a small jar with the freebase spice/fumaric/sodium carbonate powder.
then decanted, poured thru small funnel with cotton in the neck to catch any powder chunks.
added another 1/3 of the acetone, repeated as before. followed by third acetone wash. the yellow color of acetone diminished with each wash. then, oops!--spilled approx 15 drops from last wash:roll:
all the acetone was put in the clean evap dish to yield .70g.
swim has not tried any...yet.
just wanted to share this extraction experience with everyone. this seems to be a new twist of a fabulous tek, and it went rather well for swim.
any suggestions to make this info more useful is appreciated.
cheers:d
 

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Hey, hadn't seen this before. SWIM's glad to see that it works. Yield seems a bit low, however. It'd be great to see some A/B enthusiasts work on perfecting this.

Edit:
Perhaps SWIM spoke too soon. He's actually not quite sure what % yield is pictured. Can SWIY clarify?
 
the yield was 1.42g fumarate then 700mg fb from 100g very old, improperly stored bark. also there was a little spillage that would have been a few mgs.

there is certainly heaps of room for improvement.
 
biopsylo said:
3. next, swim measured 80g sodium carbonate and dissolved it into 200ml spring water in a small jar. --Ph 13 (ph 13 is not supposed to be possible with sodium carb) best estimate with old ph papers.
4. then he added this water to the mimosa tea--Ph of tea now 12.

I have no idea how I missed this thread.

Like you, I suspect your pH measurements a little bit off. Me and another member did a standard A/B (pH 4, acetic acid, 3*60, reduced) and despite adding 100 or more grams of sodium carbonate, the pH didn't raise over 10 in the mimosa mixture.

I'm wondering if you remember how hot was your water since solubility of sodium carbonate indicates you have used hot water.

21.6 g/100 g (20 °C) --> 80g would than need 400ml
45 g/100 g (100 °C) --> 80g would fit in 200ml

I suspect the lack of yield would be because of the use of the sodium carbonate.

Anyway great to see you gave it a go. I might re-do your experiment to get more answers in this "sodium carb" saga.
 
I have no idea how I missed this thread.

Like you, I suspect your pH measurements a little bit off. Me and another member did a standard A/B (pH 4, acetic acid, 3*60, reduced) and despite adding 100 or more grams of sodium carbonate, the pH didn't raise over 10 in the mimosa mixture.

I'm wondering if you remember how hot was your water since solubility of sodium carbonate indicates you have used hot water.

yeah, i must have posted it on the weekend or something, as i got 0 responses initially. (this was 2009)
there is room for improvement, just dont know if it will ever be better than a limetek.

there was loss on fb conversion, after 3 acetone pulls, 200 proof ethanol was added, and became quite yellow. this was never weighed or added to the results.

cant say how hot the water was. quite sure the ph was over 10 tho, as the mimosa went from grey to dark brown, black
 
^^thanks -that write up was done when all the excitement over fasw was going around.

yep, better to stay away from PET with limo. last time it was acquired it came in HDPE #2.


just made a sodium carbonate saturated solution, and checked ph with a borrowed digital ph meter = ph 11.6

same solution checked with paper gave a 13.

not sure whats going on.
 
biopsylo said:
endlessness said:
I doubt sodium carb can bring ph up to 13, I guess papers are less accurate ?
have you, or will you try it to compare?

The same thing happened to another poster. He checked the solution with papers and was pretty sure it was 12/13 but when he used a pH meter he got 9/10.

I haven't had the same experience since I used narrow point pH papers but I needed ridiculous (300g) amounts to get the pH of the mimosa mixture to 11 with sodium carbonate. The poster I mentioned earlier used about 90g (thinkso). I don't recommend using pH papers (atleast not the 1-14 type) when dealing with sodium carbonate.

Also you can easily make (I have done this) a sodium carbonate saturated (20/100) solution and the pH will be ~12 (theory, it's usually a bit lower) but when added to the mimosa solution things go crazy (low).

700g of sodium carbonate "dissolved" (not possible though) in 100g of H20 will give a pH of 13. Theory calculated.
 
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