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Thread: Little white "something" in distillate.

  1. #1
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    Little white "something" in distillate.

    This is boggling my mind now. If this were an oil it should have been absorbed or floated to the top or something. It's also notoriously difficult to capture in a photograph, so bear with me on the camera photo, but if you look real close you can see this subtle swirly haze sitting in the bottom of my collection flask. I've been leaving it covered with a foil so light can't get to it. This came over with one of my piperine distillations (extraction of the eth from solution).



    I tried fiddling with the image to boost the contrast, but nothing worked well enough to make the little half-swirl any more noticeable, so this is the original from the camera, cropped and resized only. Thoughts?

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    Are you talking about the little tiny white dot looking things at the bottom of your flask?

    Do either of these edits show what you're referring to any better...?




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    It would be helpful to provide an outline of the process, or a summary of your lab notes. Otherwise, your guess is as good as mine.
    Art is Nature in the flask; Nature is a vial thing.

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    Quote Originally Posted by Schmuldvich View Post
    Are you talking about the little tiny white dot looking things at the bottom of your flask?

    Do either of these edits show what you're referring to any better...?
    I got similar images. The dots are off the black background that I needed to hi-light it. It's the little misty swirls that can be seen in all, they're much easier to notice in real life when held up to a light.

    It would be helpful to provide an outline of the process, or a summary of your lab notes. Otherwise, your guess is as good as mine.
    Kiorionis. Black pepper was tinctured, tincture was separated, water added ~2 parts to one, crystallized piperine was filtered off.
    The remaining solutions (I split them up for various things, such as adding more water or salting out) were distilled to recover the alc solvent for more experimenting with the crystals. This came over with the distillation. I think shiners might call this "tails," but I'm not sure what that consists of. I suspect some water came over with one of the distillations. I'm wondering what this substance might be if it's a common thing for watery organic solutions.

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    I see similar things during distillation, and if you evaporate it down it will first be watery with some oils, then phlegm, and finally a bit of volatile salts. The exact constituents will have to be analyzed in a lab to really know what they are.

    If you evaporate off the alcohol, you can check the pH to see if it’s alkaline or acidic, which might narrow it down more.
    Art is Nature in the flask; Nature is a vial thing.

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    DT could you isolate some of the milky substance using a pipette?

    Ghislain

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    Quote Originally Posted by Ghislain View Post
    DT could you isolate some of the milky substance using a pipette?

    Ghislain
    I'm not certain. I went to look again, and today it looks like floating heat waves. It persisted for about 3 days though, I was thinking about using a separating funnel. This distillate is being used to make a piperine tincture, and some of it was used already for purifying, because I found out that the sticky gum is a bit more soluble than the piperine itself. If I distill off the leftover gum solution, I might create more of it, but there isn't much and I'll need to mix with a little water to keep the precipitating gum from burning to the side of the flask.

    If I manage to isolate some, what would I do with it? PH test? I have a creeping suspicion that it will show back up if I distill again, either in the receiver or possibly left behind in the boiling flask.

    EDIT: unless I destroyed it with that bright light trying to get a photo.

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    I guess if you could isolate some you could test the disparity between the two.

    Ph test, evaporation, flamability, odour etc...

    Ghislain

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    does water work well for chromatography of alcohol solutions? I thought about this with a couple of things that I'm doing, most likely the current piperine final preparations... I suppose like anything else I'll try it and see. If I can repeat and get it back I'll take a closer look.

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    Quote Originally Posted by Dragon's Tail View Post
    does water work well for chromatography of alcohol solutions? I thought about this with a couple of things that I'm doing, most likely the current piperine final preparations... I suppose like anything else I'll try it and see. If I can repeat and get it back I'll take a closer look.
    I doubt it. Water will only take water soluble substances along. All nonpolar substances will be left behind. I recommend a mixture of ethanol or (better) acetone and ligroin. You will have to test the ratio of the mixture for even then you can get bad results in chromatography.

    Edit: Further the milky substance looks to me like some kind of solid matter. Chromatography won't be helpful in this case. But it could work identifying the yellow piperine if you can compare it with a reference solution of piperine in alcohol. Of course you have to be sure your reference really is piperine or you are lucky and find comparable data somewhere.

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