• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Reply to thread

Your outline scheme looks about right. I think we can probably get away with using a bit less lime, more like 50g, as there's no way 2 equivalents of lime will react with 1 equivalent of bark, even taking into account the polybasicity of tannin acids. [As an aside, a useful metric here would be the basicity per Dalton (or something like that) to get a better idea of how many neutralisation equivalents a given mass of tannin might require.]


You can fine-tune the amount of lime for your particular batch by doing a preliminary test with a measured, small (test tube sized...) quantity, or by mixing up a lime/vodka paste of, say, half a gram of lime and estimating how much of the extract it decolorises. Preparation of the extract proceeded smoothly in the microwave on low/medium for about 20 - 30 minutes, using powdered bark material - the main thing is to avoid boiling the solvent, and if using a microwave I would particularly recommend covering the  container with laboratory film or saran wrap. Shredded bark will certainly require longer, so powder your bark if at all possible.


Since our goal is slightly different, we only need to optimise dissolving the alkaloids rather than the tannins. I would still recommend doing three solvent runs on a given portion of of bark, using fresh solvent each time. In absence of vacuum filtration apparatus, the simplest way of separating the calcium tannate from the clarified solution is to dump it all into a funnel plugged with a piece of cotton wool. Circular make-up removal pads prove to be quite convenient for this since they can be gently but firmly pushed into the neck of the funnel and the ~felty-woven structure of the pad proves to be more effective at catching fine articles than the more random structure of a simple ball of cotton wool.


Once all the liquid has drained through, it's possible to wash the solid material with a bit more vodka to recover trapped alkaloids that remain in the vodka moistening the calcium tannate powder. Be aware that, without suction, this filtration can take a day or two each time on account of the fine particle size of the Ca tannate.


At this point, one way of removing excess water, in part resulting from the reaction of lime with tannin acids, is to put the solution into a very cold freezer. At around -30°C the whole solution will freeze solid, but at around -22 to -24°C ice crystals will separate. It's probably most straightforward to separate the alcoholic solution from the ice with the aid of a Pasteur pipette, although with a little ingenuity one could take advantage of the aforementioned freeze/thaw possibilities and set a frozen solid beaker upside down in a funnel in the freezer (if you have sufficient room and can rely on it remaining undisturbed) and then 'turn down the cold' so that the alcohol is released and the ice remains trapped in the funnel. Obviously, the funnel should be stood securely in a suitable receptacle, and it 's probably wise to enclose the apparatus in a sealed container to prevent ice formation from moisture in the air.


So, that's one way of separating off a good proportion of the excess water without using a ton of sodium carbonate - the "freeze-dried" solvent can be finished with a more frugal portion of anhydrous SC, and if using IPA it would be worth attempting a fumarate precipitation at that point.


In summary, less time, less lime, filter, freeze, and do as you please :)


Back
Top Bottom