Can one long pull be enough

[Trickster]

SWIM's 1st exraction (Noman's tek) was very successful (640 mg of spice from 70 g of mhrb after 1 recrystallisation). He noticed that 1st 3 day's pull yielded almost 85% of the whole lot. The second pull gave about 12%. He did the 3rd and the 4th out of curiosity and got about 20 mg of dirty yellow powder.

Now he is doing his second extraction. Is it possible that a single superlong pull (5-7 days)will be enough? SWIM uses lab grade NaOH and n-heptane. He also heats the jar with the basified powder and heptane to 40-45C and shakes it vigorously very often.

 

[Entropymancer]

Is it possible that a single superlong pull (5-7 days)will be enough? SWIM uses lab grade NaOH and n-heptane.

No, a single long pull will always leave behind at least 10% of the goods; this is the nature of extractions.

You'll notice that your first pull got 85% of the spice, and the second pull got ~85% of what remained behind from the first pull. This indicates that based on the nature of DMT partitioning between these particular solvents, you're never going to get more than a 90% efficient extraction. For this reason, two pulls are necessary.

 

[EZ4U2Shoot]

SWIM's 1st exraction (Noman's tek) was very successful (640 mg of spice from 70 g of mhrb after 1 recrystallisation). He noticed that 1st 3 day's pull yielded almost 85% of the whole lot. The second pull gave about 12%. He did the 3rd and the 4th out of curiosity and got about 20 mg of dirty yellow powder.

Now he is doing his second extraction. Is it possible that a single superlong pull (5-7 days)will be enough? SWIM uses lab grade NaOH and n-heptane. He also heats the jar with the basified powder and heptane to 40-45C and shakes it vigorously very often.

I might add that if you use powdered bark from one of a few sources, no matter what you want to pull more. It took 2 weeks before Swim got everything out of his current batch. Now he is using touline and is planning to find out if he can catch jungle fever. Even if he can't he figures he got a pretty good deal his powder yielded around 1.4%+/-. So, Jungle Spice would be an added bonus.

 

[El Ka Bong]

wow .. if you go 'pulp-mill' on the MHRB for weeks, you can get 1.4% ?! do you need to heat ? wow !

 

[Trickster]

wow .. if you go 'pulp-mill' on the MHRB for weeks, you can get 1.4% ?! do you need to heat ? wow !

SWIM's stopped pulling because the 4th 3 weeks long pull yielded only 20 mg (3%).

SWIM's also seem to have screwed up re-x, because he lost almost 50% of the original yield. The only noticeable improvement was colour change from dirty yellow to light yellow. He never tried the original spice.

He just got afraid that 1.2g is wa-a-ay too much for 70 g of mhrb (premium purple or not).

BTW, what is "pulp-mill"?

 

[acolon_5]

It is ElKa's way of saying STB. Some members are very against STB because of the possiblity of lye making its way into the Naptha and ending up in the final product. It is possible that some of the loss was not in fact dmt but crud. There are a lot of arguments about STB vs A/B.

During the rextalization did you do let it sit at room temp or in the freezer? How much solvent did you use? SWIM uses maybe 50ml hot bestine for 1/2g.

SWIM usually uses bestine and only uses the smallest amount of hot bestine possible to dissolve everything. He then lets it sit, uncovered, in a safe place to a day or two. Bestine evaporates very quickly and the losses are very minimal. He will evap it down to a very small amount and then pour the remaining bestine into a recent pull and then sticks it all in the freezer. Again going for minimal loss.

Oh and to answer you original question, no 1 pull is never enough. SWIM can still get spice after 3-4 pulls. Doing cold pulls takes longer, but less oils (if any) get into the solvent.

 

[Trickster]

Acolon_5,

Thanks for your comments.

During the rextalization did you do let it sit at room temp or in the freezer? How much solvent did you use? SWIM uses maybe 50ml hot bestine for 1/2g.

SWIM let it sit for an hour under room temp then in a fridge and finally in a freezer for half a day. He used around 70 ml of n-heptane to dissolve 1.2 g of raw spice first time and around 30 ml this time.

SWIM usually uses bestine and only uses the smallest amount of hot bestine possible to dissolve everything. He then lets it sit, uncovered, in a safe place to a day or two.

SWIM usually puts the solvent into a water bath and uses a fan. Takes 5-15 min to evap 2/3rd of heptane. Then he lets it cool and keeps for an hour. Then he moves it to the fridge and later to the freezer.

He will evap it down to a very small amount and then pour the remaining bestine into a recent pull and then sticks it all in the freezer. Again going for minimal loss.

Why SWIY does not combine all pulls without evapping and then do it all at once?

Oh and to answer you original question, no 1 pull is never enough. SWIM can still get spice after 3-4 pulls. Doing cold pulls takes longer, but less oils (if any) get into the solvent.

That is understandable but SWIM thinks that each consecutive pull brings less spice that the previous one. So spending time and chemicals to squeeze that last few mgs is not really worth it.

SWIM just finished his 2nd extraction (125 g of mhrb Noman's tek).

First pull gave 1.15 g of yellowis flakes.

SWIM screwed up the second pull so he cannot tell how much he got. During evapping he left his makeshift water bath unattended for a few minutes and as heptane evapped the glass became lighter and the air stream from the fan toppled the glass. Most of the heptane spilled into the water. He took the bath off the plate and poured some fresh heptane in the water. The idea was to minimize mechanical losses. Some heptane was still in the glass, but there was a lot of water too. Carefully he separated heptane from water with a sep funnel. He was relieved to see that heptane was the same yellowish color as before the accident. But when he evapped it there was no spice whatsoever, only yellow oily goo.

Third 2 days long pull also yielded nothing but oil. This time SWIM collected most of heptane thanks to fellow spirits suggestions.

1.15 g from the first pull is slowly recrystallizing. Already there are some nice looking crystals. A few questions:

1. SWIM just bought a magnetic heater/stirrer. Is it worth trying another - 4th pull?
1. During the 3rd pull trying to get back as much heptane as possible SWIM added some salt (NaCl) to the aqueous mix. Did he ruined the mix? Is it still possible to try another pull or should he just discard the stuff?