So after following some teks (Vovins A/B and Q21's dry tek #2) one decided to try something different... although its not really that different at all..

Its kinda like a BLAB, but shorter in duration (although one is obviously keeping EVERYTHING in case it doesnt work, but fingers crossed) .. here goes..

1) Acidify 100 g MHRB with 200 ml vinegar, warm in water bath for an hour while stirring periodically

2) Add ~250 g NaOH to 500 mL and add to mix, also add 400 mL unbasified water
-even with all that base pH was only ~12 (this could be a potential problem but a new pH meter is in store as the readings were never constant or consistent .. ie 12.2 to 11.5, from one to the next, even after calibrating in between)

3) Add 100 mL NP (one used naphtha)... mix
- this is where it went wrong... it simply wouldnt separate... heat, more lye=notta
- so after some research on here one discovered more WATER was needed... so the water was roughly doubled
- this worked wonders!! (Thank you everyone here for all your knowledge!!!) and it separated instantly

4) Repeat step 3
(only did NP pulls 2x.. gonna leave the rest for a day and pull again, maybe 2x.. but really wanted to see if this would work)

5) Perform Sodium Carb wash

6) Perform plain water wash
- when doing this wash should salt be added? (I think I read that here but cant remember if so, how much?)

7) Put in freezer and wait... will post results as they happen

Thoughts/comments on how to improve would be greatly appreciated (though it is mostly from teks found here)

And much thanks and appreciation must be given to everyone here for all their wonderful knowledge..it is so very helpful when one encounters the challenges these endeavors are sometimes filled with..

Again, THANK YOU EVERYONE

Edit: Sorry, just realized what board it was posted to .. please feel free to move it if necessary

The initial yield from the first two pulls was 1.28 g (after acetone evap) from 100 g MHRB or 1.28%
- this was accomplished in ~ < 3 hours (which is much less compared to an A/B)
- 1 hour vinegar soak, add lye and water, add NP, mix for 20 min & separate, repeat twice more, sod carb wash then water wash

Mind you the gooides were slightly yellow (presumably from oils) compared to the snow white crystals from A/B & Q21's Tek 2 produced. However, no suitable Hydrated lime can be found for Q21's tek, which also takes ~ 3 hours and yields similar results, so if in a pinch one can perform this procedure instead of an A/B and simply re x if looking for white crystals or simply enjoy the yellow goodness!

Will post results from 3 & 4 pulls later

After waiting for 24 hours 2 more pulls were done using the NP from the first two pulls...

After 24 hours in the freezer the 3 and 4rth pulls yielded a total of .36%

For a total of 1.64%

... not to bad at all

For a A/B I always use about 1g of lye for every 10mL-15mL of water. I never use more than 50g of lye for 500mL of water and it works fine for me.

For a STB I wouldn't use more lye by weight than amount of MHRB. So 100g lye to 100g MHRB. But I usually use about 75g lye to 100g MHRB and it seems to work fine.

Unfortunately, no, that isnt a typo.

One started low, with 50 g lye in 100 mLs water, added it to the mix and the pH wasnt high enough (cant remember exactly)

So another 50 g in 100 mL's was added and the pH was only about 11 (according to the pH meter).
(It should have been realized about this time that the pH was good, as the solution was black. But one figured the pH meter was right as it was only recently purchased for ~200)

But alas, this wasnt realized until shortly after... Another 100g's was added in 200 ml's to bring the pH to 12.2. One then cleaned and re calibrated the pH meter to double check the reading and it some how dropped down from 12.2 to 11.5.

So one figured everything was good and proceeded to add the NP solvent... After swirling a few times and placing in a water bath, after 20 mins it hadnt seperated at all. One then remembered reading somewhere on here if it wont separate add more lye (although that wasnt the problem in this case). So another 50 g in 100 mls was added, to no avail.

That whens some more reading was done and it was discovered, almost 2x as much water is needed with prepowdered bark. Not quite that much was added and voila! Separation!

Sorry, guess one should have been a little more clear in the initial post in regards to the amount of lye used and how/when. Looking back at it now, the way it is written, seems like an unholy amount for the amount of bark used. But it was quite late when that was typed... One apologizes for any confusion this may have caused..

So if one starts with an acid (in this case 200 ml vinegar), how much lye (in g's) is theoretically needed to bring to pH 13?

(if 1 g for 15 ml's as per MySmelf and ~ 2000 mls was used in total. 2000/15 = ~ 130 g's.. would that be right?.. A properly functioning pH meter is definitely in store!)

Edit: Please note the amount of lye used to basify is excessively high (for any type of tek...A/B, STB and hybrid STB teks such as this) and needn't be higher than 1 lye : 1 bark (even this may be considered too high for some). The reliance on the pH meter was too complete, common sense should have kicked in at some point, unfortunately it did not, fortunately nothing came of this mistake. Please remember to always use common sense, caution and wear the necessary protection when handling such materials.

100g mhrb powdered

100g lye beeds (food grade)

600ml Water

mix let sit for 30 min

12oz of CROWN naphtha

mix 30 min later pull and evap down to fill a couple shot glasses and throw in freezer....Pure white

2nd pull put 8oz of naphtha mix and let sit for a couple hours

pull and evap to fill shot glass and freeze.

No need for acid bath or wash. Pulls with Crown Naphtha have always been clear. Yields 1.2%

nice work tequila! although it seems like a lot of Naphtha is being wasted due to using excessive volumes and having to evap before freeze precip'ing.. why not try a more appropriate volume and reuse solvents? (mind you this may cause slight yellowing of final product after a few uses of the same solvent)

So a second take on this procedure was attempted changing a few variables...

1) mix 100 g MHRB with 250 mls vinegar, warm in water bath for 1 hour (bath at approx 40 C, down 10 C from last attempt)

2) mix 100 g lye with 500 ml water, let disolve, mix with bark/vinegar solution, add another 1250 ml water (to give a total of 20 ml water / 1 g bark...this was all that was needed to allow for distinct separation of bark solution and NP solvent), let stand for 10 min

**One didnt bother to use the pH meter as he doesnt think its working right anyways, just went with what was customary, but one believes the pH wasnt high enough as nasty emulsions formed when NP was mixed in... these went away for the 4/5 pulls after 30% more lye was added***

3) mix 1 ml Naphtha / 1 g bark (100 ml) in solution, mix for 15 let sit for 5.. separate...repeat once
**Note even with water bath emulsions took forever to settle after pouring into the sep funnel**

4) mix 0.5 ml Naphtha / 1 g bark (50 ml), mix for 15, let sit for 5, separate

5) prepare 25 ml water with a pinch of sodium carbonate.. warm.. mix with naphtha, separate

6) mix 25 ml warm water with naphtha, separate. repeat once more

7) place in freezer and wait...

after 24 hrs in freezer 0.4% very slightly yellow goodies were collected from the NP solvent

9) 2 more NP pulls were preformed after solution was allowed to sit for 24 hrs, using 0.5 ml / g of bark (50 ml).. (nasty emulsions still formed when separating NP solvent so an additional 30% lye was added (for a total of 1.3 lye : 1 g bark) and this quelled the emulsion problem)... and washed as above.. frozen and yielded an additional 0.52%, again, very slightly yellow goodies.. for a total of 0.92% from 100 g bark..

Conclusions
- 20 mls water / 1 g of PRE POWDERED bark (compared to 15 ml/g in first attempt) allowed for distinct separation of layers when NP solvent was mixed.. tho more might perhaps quell emulsions?? IDK

- 1 g lye : 1 g bark ratio didnt seem to be enough (one should have used the pH meter to give a rough estimate but didnt) to convert most to freebase immediately (as when 2.5 lye g : 1 g bark most of the gooides came out in the first 2 pulls, 1.28%. Compared to 0.4% for the first 3 pulls when a 1:1 ratio was used) but this was solved by performing 2 more pulls 24 hrs later, easily solved but not preferred... The 1:1 ratio also didnt seem to be enough in the sense that there were nasty emulsions upon attempted separation of the NP from the bark solution, this was solved by adding 30% more lye for the 4/5 pulls for a total of 1.3 g lye to 1 g bark.. Next time one will try 1.5 : 1 ratio in an attempt to reduce emulsions from the beginning

- reducing the temp of the water bath from 50 C (first attempt) to 40 C (second attempt) significantly reduced the "yellowness" of the final goodies..

Questions
- would more water help reduce emulsions? or is this a pH problem (exact pH was not known)?

- what is the optimal temperature for the water bath to be?... if there is such a thing


THANKS in advance for any advice, its much appreciated!! (and sorry for the lengthy post)