BLAB woes are over!

[corpus callosum]

Good day to all Nexians!

I am stupidly impressed with the BLAB tek; it was performed on 300g MHRB and has yielded a final total of 10.6g of crystalline material.The tek was inadvertently changed when the vinegar and water was added to the powder right at the start and allowed to sit for 5 days with alot of vigorous shaking whenever I passed the HDPE container by.The amounts of vinegar/water/lye/d-limo were all adjusted for the reduced weight used when compared to the tek itself.

After basification it was left to sit for 24 hours with more vigorous shaking as I passed the jug by.Two pulls with the d-limo were made on the first day of pulling;these were done 4 hours apart and again with alot of mixing.The last 3 pulls were done at 36 hour intervals with even more frequent mixing.

The d-limo was placed in the fridge and within an hour crystalline accretions could be seen adhering to the glass jars' wall.More and more was just being deposited and there was a layer of orange crystal material covering the whole of the bottom.


In essence, apart from the water and acetic acid being added together, the tek was followed perfectly but in a more slothful fashion.My conclusion is that the bark has alot of goodies in it which can be extracted by adopting an even more leisurely approach than the tek asks for.

BLAB/S(lothful)L(arge)AB tek is definitely the way forward8) 8) :d !!

 

[rOm]

Waow ! So much of a yield !

BLAB is my favorite tek at the moment.

 

[Eden]

3.5% yield is massive.

I was not aware freeze precipitation of limo was possible. Does its solubility really decrease that much with temp change?

I don't want to doubt, but 3.5% seems too good to be true. How clean is the resulting freebase from this freeze precip?

 

[SnozzleBerry]

Did you add fumarate? I see no mention of that. If you didn't I'm calling shenanigans, as Eden pointed out, freeze-precip of d-limo's just not gonna happen.

 

[corpus callosum]

Apologies for not making the OP clear enough Eden and Snozzleberry- the 10.6g is the fumarate salt and I plan to keep it this way for now.And I didnt attempt to freeze-precipitate for as you say,it just doesnt happen.

The tek seemed to emphasise that adding the FASI slower is better and this is what I did.The tek says 10mls of FASI should be added every 5 minutes or so until you no longer get a white cloudiness as it hits the d-limo.Being in a slothful frame of mind, I put the FASI in a separatory funnel and just left it to drip into the d-limo very slowly.After leaving it 5 minutes or so and then returning to it, it was still dripping in and causing whiteness to form.I gently swirled it every 10 minutes or so and the whole process before no more whiteness was seen must have taken 35-40 minutes.The drip-rate was very slow.

At this point I placed it in the refrigerator (not a freezer) simply to have it not sitting out.The yield has surprised me too and Im not complaining:d :d

The slight differences between the way I did it and the tek are:

1.Adding the acetic acid with distilled water to the bark rather than acetic acid soak for 3 days then adding base and water (NaOH is what I used ,as per the tek).This was discussed in the post entitled BLAB woes...


2.The soaking period was extended to 5 days rather than 3 and the pulling phases were done much more slowly than the tek suggested.Mixing the d-limo and basified black stuff as often as I remembered to with strict attention paid to avoiding shaking was my approach.

3.Lastly the FASI was added at a seriously retarded rate.

Im not sure that the refrigertion part had too much to do with things;I simply mentioned it to highlight how my approach differed to the tek.The tek advises letting it sit for 24 hours before proceeding and made no mention of using a fridge.

I used 250g MHRB from mimosahostilis.co.uk and 50g I had from a previous purchase from MHRB.org and using vovins tek on the latter I only got a yield of 0.8%.