My STB has nevered turned into that gook. And has never been yellow... Except maybe on the 5th pull, left in for 3 days or so.. then it looks like a dehydrated person peed in my mimosa.

Its strange you have the browning issue. I experienced this on my first "A/B" extraction as well. I had cooked my mhrb in acetic acid for 2 days on low with a crockpot (dunno just heard it somewhere), I decanted/filtered/basified, then added my first pull (total time was like 1-1.5h). once the first was done, I added my second, It turned close to a burgundy brownish within 2 hrs... I thought I had the "Brown Death" as was so put by acolon. I performed a quick a/b and the stuff dropped right out.

Indeed - seems to be the same phenomena. So it occurred with heptane AND naptha. The mystery deepens...

JBArk

PROGRESS UPDATE:

STB

5 STB pulls completed. Yield: 0.819 G from pulls 1, 2 & 3 of both jars. Pulls 4 & 5 from both jars was a goopy, resiny, unmeasurable mess that i estimate to be about 200mg. I am going to clean & re-x both piles separately before weighing in fully. I shall also use the freeze precip naptha to try another pull from the jars, evapping down to half and freeze precipping again to see if there is anything left in the bark. Final results within a fortnight or sooner.

"A/B"

Due to the red/burgundy naptha phenomena in one of the jars, I did 2 pulls from both jars, and 1 from the unaffected jar in the first freeze precip, for a total of 2.5 pulls, or half what I will end up doing. I pulled them out this morning and have never seen so much spice! Pics to follow later in the day.

For the affected jar, I pulled the red/burgundy naptha off and placed aside. Another pull (#4) was started with fresh ROOM TEMP naptha. Once again, the naptha pulled a lot of red, but a lot less than in the previous pull. So heating the naptha does not appear to be the problem, unless it changed the A/B MHRB solution permanently.

After a day and a half, a light sediment has accumulated on the bottom of the initial red/burgundy naptha. I will do one final pull on this jar (#5), then do a small A/B before cleaning and re-xing everything.

Pulls 4 & 5 from the unaffected jar also remain to be freeze precipped.


Cheers,
JBArk

PROGRESS REPORT

"A/B"

Curiouser and curiouser... The first 3 pics Are just the floaties from 2 pulls from both jars, and 1 from the unaffected jar. I have never had floaties before! I filtered them, as you can see from the coffee filter. They weighed in at 112 mg! The pyrex dish (no pics) had a condensation problem that turned the crystals to goo, so I put the naptha back in and added pulls 4 & 5 from the unaffected jar and put it back in the freezer. (I know this is getting complicated - that's why I am giving a step by step. Basically, minus the floaties, what I have in the freezer now is all 5 pulls from the "good" jar, and 2 pulls from the other, before it was affected...)

The floaties are to date the cleanest looking whitest crystals I have seen!!

The last pic is, from left to right, pull 3, pull 4, and pull 5 (still in the mason jar). Strangely, after 2 "affected pulls" pulls, the 5th pull reverted to a normal colour with the return of a slight emulsion! My plan is to put the red/burgundy pulls aside to do a "small A/B" after which I will pull remove 5th pull and mix it with the others and freeze precip it all (assuming the emulsion settles; if not I may be forced to roll the dice and add more lye to break it...)

Stay tuned!

JBArk

I'm having that burgundy nnaptha problem as well with 5 lbs of fucking rootbark. Talk about the biggest headache- 3 recrystalizations and little benefit. Freeze precip yields brownish gunk with crystal on top. When drained of naptha and air dried- the crystals and gunk turn into liquid.

Postulations:
Reaction took place at too hot temp (jugs were barely holdable after lye was added, SUPER hot)
Not enough h2o in the mix. (I'm using around 3 quarts distilled h2o and slightly less than 1qt of naptha per 1lb rootbark in a 1gallon jug)

I have NEVER had this happen before- my spice has always been fluffy and delicious every time.



How would one do an A/B on the naptha? Would the following be adequate?
1. Add Muratic Acid (35%) dropwise to h2o (10 drops? not sure about amount here)
2. Mix naptha and dilute acid to form DMT HCl which migrates to h2o layer
3. Decant naptha (necessary??)
4. Basify h2o with lye (amount??)
5. Mix basic h2o with naptha, shake and decant
6. Freeze precip naptha.

Re-x does not work very well when there are a lot of impurities.



Exactly what SWIM had.



Better get yourself a pH meter or some pH paper. Otherwise it will be guesswork every time. You don't even know your starting pH, do you?



Yes. This will be your defat stage. But keep it just in case.

At this stage swim would let the acidified aqueous solution sit for a day in a fridge, then decant and filter it from any solids.



Same as 1.

PROGRESS REPORT

STB
I re-xed everything with heated bestine/heptane (819mg + approx 200mg goo - call it an even gram...) and freeze precipped for 36 hours for a surprising reduction to 719 mg of yellowish spice. Must have been a lot of crud in the original pulls...

FINAL STB TALLY AFTER RE-X: 719mg

(*will try another pull just to see)

PROGRESS REPORT

"A/B"

Removed the pyrex from the freezer and poured off the naptha (collecting the floaties), turned the pyrex upside down and propped it up). Surprisingly, it still dried rather goopy. I scraped it up and weighed it:

1.651g!!!

It was all the material from all the pulls not including:

-the most recent 0.069g floaties

-the final pulls from the "affected" jar (red/burgundy naptha - see above posts)

I will re-x this material next (including the 0.069g floaties), then attempt the "mini A/B" on the "Affected" naptha. I was thinking though - most of the colour has precipitated out, so if I decanted, freeze precipped then re-xed, this material, would I need to bother doing a "mini A/B"?

Cheers,

JBArk

PROGRESS REPORT

"A/B"

So after 1 week, the red has pretty much completely settled out of the red/brown/burgundy naptha!! So instead aof a mini A/B, what I will do is to evap down to half, then freeze precip and then re-x. I feel confident this will clean it up.

In the meantime, I re-xed all the other pulls (minus 112mg of runoff floaties) and scraped the martini glass for a total of 1.255g!!

So with the floaties: 1.255g + 0.112g = 1.367g - and there are still 3 pulls to go!! (from only 1 jar, the "affected " jar, so really only 1.5 pulls...)

This is almost 2X the yield of the STB, and there's more to come...

Grand total, evaluation, conclusion, pros and cons of each tek to follow.

JBArk

LAST PROGRESS REPORT

"A/B"

The pics below show all the material from the "affected" pulls (originally the red/burgundy naptha before the red sediment dropped - the naptha was crystal clear at that point, but it took a week!) Instead of re-xing the last 70 mg i am going to save it for changa or enhanced leaf. This puts the total "A/B" yield to 1.437g!

A conclusion with data and pros and cons to follow.

One last note: I have taken all the post freeze precip naptha from the "A/B" and the STB, repulled from their respective soups and will freeze precip this after evapping down, just to see if I missed anything. I doubt it, but it will be interesting to see... An addendum will follow the conclusion if anything precips out.

JBArk

Jbark, amazing work!

And you have upheld my belief that A/B is superior to the quick and "easy" STB!!!

Even if that hadn't been the case, excellent work. You my friend are a massive asset to our community!

Thanks Acolon_5!! It's been so long since anyone responded to this thread i was contemplating checking myself in for insistent-talking-to-myself syndrome! I have been out of town or i would have posted the conclusion already... Stay tuned for the final tally and the pros and cons of each tek.

Cheers and thanks for the interest!

JBArk

I hate to be the guy who’s always going against the grain, but a lot is in technique rather than A/B versus STB.

Two different people can perform an A/B on the exact same material and one of the two usually gets much better results. How you perform each step, and your attentiveness to detail makes a big difference. How you mix the solvents in an A/B makes a big difference. The times of soaking makes a difference. As do many other things.

In an STB, the soaking time can make a huge difference, how it’s mixed, and how the material was pretreated can make a huge difference. For example, if you do an STB on cactus using very finely powdered cacti, the results are many times better than if the cactus was poorly ground.

Not really sure what you are saying here ron69 - are you imtimating that side by side comparisons are pointless? Your dimissive criteria could be used to discredit ANY labwork ever done...!!! I am not in a scientific profession, but i have a good handle of scientific methodology and did my utmost to maintain rigorous standards of work and process. Your points about materials are well taken, and are clearly the reasons i used the sqme bark, the same lye and the same NPS in both teks. I would be very open to an elaboration of your points, but I must confess your post as it stands doesn't make much sense and makes me question your motives. Surely i am wrong on this point and look forward to an articulation of your stance.

Cheers,
JBArk

So here's the final tally:

“A/B”

Theoretical time for extraction: 4 days acid soak + 4 days (1 to mix lye and start pulls, 1 extra for last pull, 2 for freeze precip) + 1day for re-xing = 9 days

Real Time for extraction: 16 days (7 days for red naptha to clear)

Lye used: approx 100g (+ approximately 100g that was likely unnecessary, but was used ineffectually to clear up the “red” naptha phenomenon. See pros & cons below)

Yield: 1.437g
Yield %: 1.4%


PROS & CONS:

pros
- yield!
- Lower lye quantity used
- Re-xing not necessarily essential (had I not re-xed, I would have had 300mg more DMT!)

Cons
- Requires more time and more steps
- Experienced a strange red naptha problem that took a week to solve (perhaps from heating the naptha, which i felt was unnecessary from the outset, and only did to be as faithful to the published tek as possible)


STB

Theoretical time for extraction: 2 days (1 for mixing and 1 for last pulls and freeze precipping) + 1 for re-xing = 3 days

Real Time for extraction: 3 days

Yield: 0.719g
Yield %: 0.7%

Lye used: approx 175g


PROS & CONS:

Pros
- speed. 3 days from MHRB to re-xed spice
- less steps and no acid

Cons
- yield. The yield was exactly half the yield of the A/B...
- much more lye used
- re-xing, or at least cleaning, seems to be a necessary step given the resulting spice and the large quantities of lye used


CONCLUSION

An interesting experiment, but ideally i would like to give the STB another go with the same bark to see if the yield is in fact that much lower, or if something was lacking in my technique, despite endeavours to keep everything as controlled, and equal as possible. After this, despite the cons, I tend to prefer the A/B; it seems somehow more complete, and while some argue that the acid step is unnecessary, it appears to be the only variable to account for the yield disparity. The “red” naptha phenomenon in the A/B extraction was strange, and may be from the heating of the naptha, but subsequent unheated pulls were a little funky too. I would like to get to the bottom of this, as it seems to happen fairly frequently based on others’ posts in various parts of this forum.

Also I should not for those who haven't followed the whole thread that there was some contention about Panoramix's tek being considered a true A/B, due to, among other things, the absence of a filtering and discarding of the bark before basifying. I stuck with calling it an A/B because nowhere in the wiki is an A/B defined as requiring this filtration. you decide...

Thanks for following along, and I hope this is helpful to someone somewhere!! I will try another side by side in a few months – in the meantime I am preparing an easy to follow A/B tech of my own (JBArk’s BARK EX TEK!) – nothing new, just easier to follow (IMHO) and organized in a way that in-depth information on procedures and chemistry is available to read, but may be skipped by more experienced extractors. Stay Tuned!

JBArk

EDIT: keep in mind these results are not NECESSARILY typical of A/B or STB extraction: do your own tests and contribute to the knowledge!!

Good work JBark- thanks for your efforts.

I agree with you- A/B does seem more 'complete' a process, somehow.But I wouldnt dismiss 69rons comments out of hand as I tend to agree the outcome can depend on how much attention to detail is paid at each step.

Indeed this is true. But by posting such a comment is he insinuating:

A - that tek comparisons are pointless
B - that no lab processes or tests are valid
C - that MY method is suspect

By default it must be one of these, or why post at all? We are all aware of the fallibility of the process, but from there to a conclusion that processes are pointless is too large a leap for me. I guess for anyone out there who agrees with Ron, the only solution is to ignore this thread and do your own comparisons!! I personally would like to encourage everyone to do similar side by sides, for reasons stated above.

JBArk

For a number of reasons I do not think your results should be considered as a basis for general conclusions. That's what 69ron was saying.

E.g. when I was experimenting with STB, several times my yield was ~2% (1.5% after re-xing). I did not run an A/B on that batch but I doubt I could have gotten 4% yield with any tek.

Also most people agree that an essential part of an A/B is filtering and discarding solids after the "A" stage. So, Panoramix's tek is sort of enchanced STB, rather than a proper A/B. Therefore we can only talk about comparing these two teks (Panoramix's and STB).

For any far reaching conclusions your result should be repeatable by anybody anywhere under the same conditions. Otherwise they could be experimenter-specific. Only if you run a few dozen Panoramix's and STB extractions and average your results you can generalize.

Just a quick fyi jbark re: Naphtha

There is another solvent option for Canadians - Recochem Camping Fuel

You can find it at Acklands

had to put in my 2 cents

i use stb with xylene or dlimo - fasa or fasi
i never get less than 2% freebase after the first 3 pulls and stop after 4-5 pulls and 2.4% or so - sometimes u get lucky and get more.

a/b with mhrb for me is just a hassle and the end result after heptane cleanup is about the same - just more work and more time/dirty pots.