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Failed extraction attempt from P. Australis Options
 
omega-scar
#1 Posted : 11/17/2009 10:11:18 PM

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Plant material was Phragmites Australis roots.
Tek used: Marsofold's (+defatting , as sugested on the site)

. ~400 gr roots cleaned, chopped and grinded
. solution of ~3200 ml tap water with ~600 ml 9% white vinegar was prepared
. plant material was boiled 3 times (50% of solution first, then 25%, 25%) and resulting "juice" collected through strainer

three days later:
. "juice" was mixed with ~300 ml solvent (containing toluene and xylene) and then "shaken hard"
this created a thick layer of what SWIM understood is emulsion

two days later:
.some rock salt added to the jar, slowly stirred and then jar heated reducing the emulsion considerably
.the top layer , which now looked more clear (like the solvent) but still with some 'foam' was sucked up with a syringe and discarded
.the defating step was repeated two more times, at about 15 min intervals, only this time gently mixed with a wooden spoon and not shaken hard
.six Tablespoons of caustic soda granules (drain pipe cleaner) were premixed with ~400 ml water and added to the jar (actually 4 Tbls's initially and then decided to make some more with another 2 Tbls, because the juice in the jar "did not turn black"Wink.
this resulted in some darkening of the light yellow solution from the jar, but it was certainly not black but rther a somewhat brown color. SWIM atributed this to the using of different plant material and not a too low pH, altough he did not have a pH meter.
.~250 ml naphta (Zippo lighter fluid) was added into the jar then gently stirred
.everything was stirred gently, let ~3 hours and then the clear layer was sucked with a syringe and put into a pint mason jar
.pint mason jar with resulting solution stayed 3 days in a freezer (that freezez ice cream hard Cool , so this was certainly not the problem)
.the jar was then shaken and the solution was quickly poured over a funnel into which a filter cofee paper was put.
.after all the solution was strained, the filter did not contain any crystals at all

SWIM waiting for forum members opinions as to probable cause of complete failure.
 

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Infundibulum
#2 Posted : 11/17/2009 10:42:17 PM

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Try evaporating at least half of the naphtha then stick in the freezer again. If there's too little spice (i.e. too diluted) then it won't get freeze-precipitated. If it doesn't work either, then evaporate the naphtha totally in case you may get something.

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fourthripley
#3 Posted : 11/17/2009 11:11:31 PM
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Were your rhizomes straight from the ground or dried first, the dry weight is what you would calculate your % from, water weight will throw your estimates right out. I've never seen a % for this plant, Trouts notes list the dmt content as weak to absent. I suspect evapping to dryness is your best bet, even if you caught a good plant your yields are likely to be in the 10's of mg rather than the hundreds, which is good enough for such a ubiqitous and free plant, great to see somebody trying this outSmile
mistakes were made
 
endlessness
#4 Posted : 11/17/2009 11:31:15 PM

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edit: oops, read wrong..

yeah try to evap most of the naphtha and stick again in freezer, and if nothing comes next day then evap it all and see what comes up
 
furley
#5 Posted : 11/18/2009 12:14:06 AM
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Another idea if you don't want to evaporate some of the naptha down is to split it up between collection chambers in the freezer. I usually take 1 naptha pull and put it into 2 jars to freeze precip.
 
omega-scar
#6 Posted : 11/18/2009 7:48:30 AM

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fourthripley wrote:
Were your rhizomes straight from the ground or dried first, the dry weight is what you would calculate your % from, water weight will throw your estimates right out. I've never seen a % for this plant, Trouts notes list the dmt content as weak to absent. I suspect evapping to dryness is your best bet, even if you caught a good plant your yields are likely to be in the 10's of mg rather than the hundreds, which is good enough for such a ubiqitous and free plant, great to see somebody trying this outSmile

They were not dryied as SWIM would let a 'leaf' dry in order to smoke it, theese were long thick healthy roots have a wood-like hardness to them mostly, which in SWIM opinion should've taken half a year to dry, buy they were washed, peeled away from any papery-like-skin, and thoose looking 'best' were put it the freezer for about 1 week before the cutting and grindind took place, and during this week they were repeatedly taken out 3-4 times to defreeze and then put back in the freezer.
Just as a side note: This operation in itself was a tremendous work, harvesting those deep-down in the ground rhizomes, taking/peeling all the papery stuff around then, cleaning every tiny bit of dirt out of them, etc.
 
Noman
#7 Posted : 11/18/2009 8:03:47 AM

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What came out into that NP may never precip but still be loaded with alks - I'd evaporate it down completely.
 
biopsylo
#8 Posted : 11/18/2009 2:55:09 PM

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Does everybody think he had high enough ph before adding naptha?
he said he started with 3.5 L water-600ml of which was 9% acetic vinegar.
Then premixed 6 tablespoons naoh into 400ml of water.
would this be enough?

so the rhizomes he started with were fresh, so could be as much as 50-70% water by weight?
 
Infundibulum
#9 Posted : 11/18/2009 3:30:37 PM

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biopsylo wrote:
Does everybody think he had high enough ph before adding naptha?
he said he started with 3.5 L water-600ml of which was 9% acetic vinegar.
Then premixed 6 tablespoons naoh into 400ml of water.
would this be enough?

so the rhizomes he started with were fresh, so could be as much as 50-70% water by weight?

Good call here, nicely spotted! The solution is massively underbasified.

3.5l of 9% vinegar contain a total of 315g of acetic acid. All this amount of acid needs at around 210g of NaOH jsut to neutralise to pH 7! omega scar used around 90-100g of NaOH. His solution should still be pretty acidic.

He needs to add at least 150g NaOH jsut to neutralise and an additional 50-100g to decently basify it.

In short, omega scar you need to dump at least 250g of NaOH and repeat the pulls!

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endlessness
#10 Posted : 11/18/2009 8:16:10 PM

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inf, but he didnt have 3,5l of 9% vinegar, he had 3,2l water + 600ml 9%vinegar...

anyways, adding more base wont hurt Very happy
 
Infundibulum
#11 Posted : 11/18/2009 8:23:19 PM

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Ahem!Very happy

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
omega-scar
#12 Posted : 11/19/2009 9:10:30 AM

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endlessness got it right. SWIM started with 3200 ml water and 600 ml 9% acetic vinegar, and after discarding the plant-goo at the bottom of the jar, plus the other separations SWIM was left with around 3500-3600 ml of liquid.

Another thing, Infinidibulum sayd:
" 3.5l of 9% vinegar contain a total of 315g of acetic acid. All this amount of acid needs at around 210g of NaOH jsut to neutralise to pH 7! omega scar used around 90-100g of NaOH. His solution should still be pretty acidic. "
- Umm... SWIM did not use 90-100g, because SWIM remember very clearly that the whole package of drain-cleaning granules contained 80g , and after putting 6 tablespoons from it, there was still some of that 80g remaining, which SWIM threw out, because Marsofold's tek said 4 tablespoons and SWIM've already put six. So SWIM's solution got ~50-60 mg NaOH.

biopsylo: "so the rhizomes he started with were fresh, so could be as much as 50-70% water by weight?"
- They didn't seem watery to SWIM.... really. Well, it's safe to assume they also contain SOME water, but really they were more like "woody" than "grassy"... SWIMS kitchen blender witnessed this best, as SWIM almost broke it's motor in the grinding process.

So what is now to be done , in your opinion folks ? SWIM just make some more NaOH and simply pour over ? And continue just as he did before ?

 
Infundibulum
#13 Posted : 11/19/2009 11:53:31 AM

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Just add more NaOH (seriously do not believe the "you need to predissolved in water otherwise NaOH spikes will harm the spice" myth) and repeat the pulling. Adding much more NaOH will not harm at all.

There's one more thing flawed in the tek; SWIY defatted with the aromatics xylene/toluene, then basified and pulled with naphtha. If there were any traces of xylene/toluene during defatting (even in the form of a small emulsion) then these traces of xylene/toluene will be pulled with naphtha. So your final naphtha pull will have traces of xylene/toluene as well as (hopefully) spice, and SWIY won't be possibly able to freeze-precipitate it. Xylene/toluene dissolve spices very well and they may keep spice dissolved even in a frozen solution containing naphtha.



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biopsylo
#14 Posted : 11/26/2009 4:50:42 AM

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Hi Omega-scar:
just wondering if you have had any success with the common reed.
did you add more base?
or did you post results elsewhere?
im gonna grab a shovel....Razz
 
omega-scar
#15 Posted : 12/6/2009 2:11:22 PM

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Hello biopsylo. No, SWIM did not add any more base, just evaporated the remaining naphta, and that resulted in no crystals whatsoever. SWIM is going to order Mimosa Hostilis root bark from Heavenly products, and is planning to start a new extraction this month. Wish SWIM good luck, because SWIM is having difficulties finding the legal status of MHRB here in Romania. SWIM will do some mantras, not to get the package along with a couple of cops at his door Laughing Cheers.
 
endlessness
#16 Posted : 12/6/2009 2:40:41 PM

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well just in case better have the extraction equipment away until it arrives, and if anybody asks anything its to make dye Pleased
 
 
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