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Thread: The Black Pepper Tincture Thread, Free Medicine :)

  1. #81
    Join Date
    Aug 2017
    Location
    USA
    Posts
    284

    Piperine Filtration Day! And that means pictures :P

    So my black pepper tincture was produced in two fractions, as mentioned above. I'll refer to these as the dross fraction (the first part that I siphoned off) and the "good" fraction for reference.

    The dross fraction was crystallized out using a preparation of salt water, because it was being fussy. This got everything out, and the picture doesn't really do it justice. It's looks green, but it has the right smell, so the filter paper caught a mixture of piperine and tar, but the solution clarified a lot after sitting for 24-48 hours (I did it twice by splitting the dross fraction into 2 separate containers for repeatability, salted one out, then poured the remaining clear fluid into the other. The salt is obviously staying with the fluid)




    The good stuff was in a separate flask, and the little crystals were fixing themselves to the glass. But after a good bit of agitation, most of them came loose. Enough that I didn't feel like scraping out the rest anyway. The filtrate was still super duper cloudy, which means more suspended piperine that is too small to get caught:




    The filter paper looked like this after opening. This solution has been sitting in a dark place for about a week to bring these about, nothing added after the distilled water:




    Here's a picture of the clear salted out dross filtrate on the left, and the "good stuff" filtrate on the right. In the middle is the rest of the dross waiting for filtering.




    I'm still not sure about salting out my good stuff. Next step is distilling the original solvent off the dross fraction, to see what happens. I might split the "good" filtrate into two equal parts and add some NaCl to one, just to see what drops out and how it compares to the dross fraction. I'm suspecting that if you start by adding a little water, let settle, and siphon the lower layer off, you will get a better piperine extract from the rest, that the gum falls out of solution very quickly, but I could be horribly wrong. I suppose we shall find out. The other question is the method of getting out the stuff that doesn't readily crystallize. Salt vs distillation.

    Either way. I haven't weighed my "good" crystals (retrieved from a sealed flask after a week of sitting in the dark), but it was a good heaping tablespoon worth. In both cases, removal from the filter paper while it was still wet was super easy. I spread the paper on a plate, and scraped them free with a butter knife, and there was enough that I didn't worry about the fiddly bits that got away. I'm really happy with how this went, the good fraction produced crystals of amazing brightness. They're small, but they have a great color like the ones on wiki.

  2. #82
    Join Date
    Aug 2017
    Location
    USA
    Posts
    284

    Back to my main focus experiment

    quintessence from decoction.

    I so far have not been successful (I don't think). Things at the final stages keep revealing an off putting odor, but one thing in particular remains sweet.

    To catch up, I got the common white salt from the ashes, and the red wine from the rest of the water. The "wine" I've been working with so far was not allowed to rest and ferment of it's own devices, and it can be separated in many ways, but you will notice after refluxing that the fluid becomes thick, almost slimy. This is the portion the next phase of my experiment will focus on.

    The solid mass is separated and burned to a calx, making our common alkali salt.

    In general though, the reddish liquid, however I extract it, drops a brownish earth. This isn't easily filtered out, but it can be mostly separated through decanting, and then filtering the last bit of solution with only a little of the "earth" remaining. This is dried to a red earth and saved. The remaining fluid is dried to a gum. <not sure separating these two is necessary>

    The red earth and/or the gum (I'm not sure which because I mixed them back together, I suspect the gum) contains inside it an oil, even when evaporated to dryness and calcined to over 150C. This oil can extracted via tincture, which then must be put through it's own series of purifications. I think this oil is the key, at least so far it's the only thing that doesn't stink of lysol when mixed.

    The white salt and the yellow or red oil are mixed in the proper proportions, and can be further purified through washing with distilled water to the point of purity, leaving a wonderful and precious something upon evaporation.

    So ends the theory. The next phase will be repeating this entire process with a red liquor that has putrified to a sharp vinegar and dropped it's red earth. The salts are already mostly prepared, and I start again. I'm worried that I don't have very much left, but perhaps enough to give my speculation above an honest run without killing the necessary ingredients for the final preparation.

    A note, the putrefication occurred BEFORE I separated the solids from the refluxed soup. The wine separated too early (what's left of it) has contracted a white hairy mold. Reflux, find the gellateanous goop, and bottle it up tight while it's still hot. That will (I think) allow it to putrefy to sharpness. The bottle was also placed near my heater, so it's been kept warm most of the time, but cooled down when nothing was happening in my heating pot.

    I'm pretty sure of the process at this point, so I'm going to go at it again and see if I get enough of the little oil to make something. I won't be doing any of my normal fractioning this time, it's all or nothing. If it proves interesting, then I'll repeat this whole thing again with another plant material, for validation of the process. It's been fun, and if nothing else, I learned a few tricks along the way for purification of products.

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