{{A/B extraction w/ MHRB.}}

Materials:
100g MHRB, powdered (roughly 140ml, unpacked)
HCl (Muriatic Acid)
NaOH (Lye)
DCM for NP solvent
Plenty of distilled H2O

Tools:
Hot Plate/ Stirrer- a true beauty
Buchner funnel w/ aspirator pump (102 & 410 qualitative paper) w/500ml filtering flask
2 Flasks- One 500ml and One 1000ml
1 beaker- 500ml
1 Sep funnel- 1000ml glass stopper
Distillation setup for distilling DCM w/ 1000ml FB boiling flask
Hannah Instruments pH meter
...not too much else

*General Chem knowledge and passion, here.
-If one were at the step of distilling the DCM, is the following were one would proceed?/;

1)[X1]Taking 100g of MHRB and adding 500 ml of aqueous HCl to acidify to pH 3, THREE times over (filtering with 102 grade filter paper through Buchner each time.
2) Defatting with 10% by volume DCM in sep funnel-
---a)pouring off DCM from funnel, while keeping aqueous solution in funnel, and then
3)[X2]Basifying with NaOH to pH 12-13 (adding basic solution, without removing acid solution from funnel)
4)[X3]Adding 10% by volume DCM directly to seperatory funnel and pouring of DCM (bottom layer)
---a)discarding the remaining solution
---b)saving the dcm layer poured off
5)[X4]Placing DCM in freezer at lowest possible temp to precipitate.
---a)removing next day to filter through 410 grade filter paper through Buchner
---b)removing precipitate from filter paper

Questions include:
[X1]: What is the route of deciding how much aqueous solution to use when acidifying? And what is this process doing to the DMT salt (found in the MHRB)?
[X2]: How much NaOH is to be added to aqueous solution? Proper route to go about calculating true neutralization between acid and base? (calculating molarity and/or/from pH?) And, again, what is this processing doing to the DMT, chemically speaking? (No laymens terms, please)
[X3]: Is 10% per volume of DCM solvent going to be enough for defatting and also for extracting?
[X4]: Best way to go about purifying from precipitate out of DCM? Is a Buchner funnel going to be of good use here?

I have tried to organize this as much as possible and have done much homework on what needs to be done. I am trying my best not to half-ass anything and to enjoy my time spent while making a good product to stand in the court of the gods once more. Hyperspace is not feared, but respected.
Thanks in advance to those who provide advice.
Respect to those who seek knowledge with me.
And bliss comes to those who read all the way through this.

Thanks,
Ananda

To answer question 2, when the solution turns black you know you're based.

This walkthrough is recipe for disaster and dismay. Is it inspired by the infamous old QT tek? if yes, please revise EVERYHING, since its the crappiest tek around. Go for vovin's or marsofold if you want a good old A/B.

You cannot freeze-precipitate spice out of dcm. You can salt it out of dcm though. And you really do not need defats, seriously. You're also better off boiling the bark in acidic solution 3-4 times than just soaking it in water.

Re to questions:
1. experience ;300-1000ml of total acidic extract will be enough to take out of 100g of rootbark (that is, after 3-4 boils, filtering and their reduction. 300ml may be too gooey to worj with with properly and issues with layer separation may arise.

2. Hard to know "true neutralisation". You need to neutralise all the acid you used for the brew plus all the additional acids that got extracted from mhrb. But nuetralisation means pH=7, so you also need to add base beyond 7 to basify. pH 12-13 is good. At basic solution what happens to dmt is that in basic solution the scarcity of protons and the overabundance of hydroxyls drives hydroxyls to react with protonated (ionised) dmt thus forming dmt freebase and water. I't all a matter of equilibria.

3. yes.

4. salt out dcm and do a mini-a/b

Dude.... Do a simple noman tek your first time around. I dont know why people love to pick the complicated teks first extraction. If something messes up with your 100 steps to follow, then you will come here asking what went wrong.... A simple STB noman tek is all you need.. Water, lye, mhrb and naphtha... Simple stuff man! 50g of mhrb for the first extraction...
Please rethink your complicated first timer tek and do yourself and everyone here a favour! STB = excellent starter tek

Inspired- yes, this was the first tek I looked at, about two years ago.
No defatting- even though Vovin's says to do so?
Why can you not freeze-precipitate from DCM?
Sorry to whom I annoy, buy I'm sticking with this route, and will tweak it as need be.

Since you want to stick to an A/B, here are my general thoughts:

First, start with 50g to get your feet wet and to keep the volume of liquids down.

Always add acids and bases to H2O and not the other way around.

Defatting might not be a bad idea if you are going to use DCM as it is a more efficient extraction solvent.

Don't basify in the separatory funnel, this is an exothermic reaction and will build a lot of pressure in the funnel. You might also run out of room if you are adding aqueous base, which is recommended for control of pH. It will also make it difficult to check the pH with a meter.

Freeze precipitation (a re-crystallization procedure) doesn't work with DCM because it is an efficient solvent for DMT which stays in solution as the temperature drops. You are going to have to evaporate the DCM to get the alkaloids out of solution. It's because of this that I say a defat might not be a bad idea.

In place of crystallizing, one would be able to distill off the dcm (~40*C) to reuse, leaving the remaining crystals in the glass, which could then be purified using a non-polar solvent with a lower pka? Naptha would be used here.

^^
well, in theory yes, but in practice things may not go as expected. The advice is to keep everything simple in a 1st time extraction (that means, stick to a tried and tested tek to see how things behave), i see here that you want to try 1 million of different things in one extraction, sure the enthusiasm is admirable but trying 1 million of new different things is not a great idea.

Also, non-polar solvents do not have a pKa.

Apologies I meant log p- have been reading up on pka and xlogp.
Why is it that it will not precipitate out of dcm, but will out of naptha? Because naptha has a log p twice as high as dmt, and dcm is so close?

Well, logP is good for guesstimating solvent - solute relations but in practice things can be more complicated and/or not as predicted. Anyway, as dozuki said you can freeze-precipitate (or crystalise for that matter) with solvents where a substance is soluble in it at a warm temperature but not too soluble at a colder temperature. dmt is soluble in naphtha but not soluble in cold naphtha. but for dcm it is just too soluble to precipitate it out. Sure it dmt will precipitate out of dcm if the dmt concentration is high enough, the volume of dcm low enough and the temperature cold enough but that's not too practical.