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Bot0nist
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[*] posted on 3-3-2012 at 16:27


The link works for me.

pid222835
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  • posted on 24-9-2011 at 02:15 PM Reply With Quote
    Black Pepper to Piperine 91%IPA small scale


    This little extraction was a lot of fun. I learned a great deal about recrystallizations, which is a very valuable skill. It was also challenging and results in a beautiful crystalline and harmless end product.

    I have some pictures of the process and some good notes, but I will try again on a larger scale and take pictures at every step to post with a writeup.


    Here is how it happened.

    Materials:
    500ml RBF
    30cm Fredrick's reflux condenser
    assorted beakers
    filters
    eye droppers
    Bottle of 91% IPA
    Fresh ground black pepper

    __________________________________________

    EDIT: Blogfast25, it is because my browser shows 50 posts per page. If yours is default, then it will be on a higher numbered page.

    http://www.sciencemadness.org/talk/viewthread.php?tid=10676&...2#pid222835

    Since it isn't page 2 on your browser, it doesn't link to the right post. This will start you at the first post it seems, even though the pid is correct. My writeup is one of the last posts in that thread. The title is Black Pepper to Piperine 91%IPA small scale


    [Edited on 4-3-2012 by Bot0nist]




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    [*] posted on 4-3-2012 at 14:10


    I see, thanks!



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    [*] posted on 4-3-2012 at 16:19


    Quote: Originally posted by Bot0nist  
    Got to love the needles. Here is piperine (&chavicine?) that was extracted from black pepper with IPA being recrystallized from 10ml of etOH/IPA mix. Slowly cooled overnight. One of my favorite things is watching a recrystallization come to fruit. Ever so satisfying...


    Exactly! :D
    It's the feeling of purifying something, isolating something nice from some gunk. Awesome feeling.
    I really like the tower-like crystal going out of focus. Could you take a better photo of it, if the sample is still intact? :)


    Quote: Originally posted by mr.crow  
    Solid benzene looks like ice in a soda


    Kind of, yes. The whole bottle was one block of solid hydrocarbon, so I warmed it with my hands and soon the top melted and made a little pool.
    It crystalized a bunch of mostly hexagonal prisms extending from the walls towards the center of the bottle. It reminded me of a beehive. I couldn't take a nice, wide shot photo because the label was in the way.

    Also, my triethanolamine went solid overnight because I used to keep it in my sleeping room, and now it's in the cold lab. So I took a photo of it, too.
    Quick question - if we define the regional room temperature, and there's something that melts at that very temperature, do we call it a solid or a liquid? Because that's TEOA's case, more or less.




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    [*] posted on 11-3-2012 at 06:36


    Copper(II) acetoxybenzoate:
    Copper_aspirinate_2.jpg - 398kBcu2(asp)4_crystals_small.jpg - 172kB

    [Edited on 7/6/13 by bfesser]




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    [*] posted on 11-3-2012 at 13:46


    I noticed the pictures of sodium chlorate crystals earlier and remebered that I had a very large crystal that I had made a while ago. When i left a beaker of concentrated sodium chlorate solution on my shelf in my lab for a couple of months.

    Its a shame that when i took it out of solution and put it in a zip lock bag, it obviously wasnt sealed and developed some cavenous holes.

    (i tried to put up some photos, but they didnt make it.. I'll try and put them up later)

    [Edited on 11-3-2012 by vaslop]

    [Edited on 11-3-2012 by vaslop]

    rps20120311_222603-1.jpg - 31kB rps20120311_223445_488.jpg - 55kB

    [Edited on 11-3-2012 by vaslop]
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    [*] posted on 11-3-2012 at 16:12


    Quote: Originally posted by Endimion17  
    Quote: Originally posted by Bot0nist  
    Got to love the needles. Here is piperine (&chavicine?) that was extracted from black pepper with IPA being recrystallized from 10ml of etOH/IPA mix. Slowly cooled overnight. One of my favorite things is watching a recrystallization come to fruit. Ever so satisfying...


    Exactly! :D
    It's the feeling of purifying something, isolating something nice from some gunk. Awesome feeling.
    I really like the tower-like crystal going out of focus. Could you take a better photo of it, if the sample is still intact? :)


    I tried, My camera doesn't have a very good macro mode, and I am having trouble getting it to focus on the tower-like structure. I dumped it out to get a more contrasting backdrop. I will try to get a better camera this summer.





    NewPiperine.jpg - 188kB




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    [*] posted on 12-3-2012 at 10:18


    Just some caffeine extracted from coffee, having crystallized from an vaporised solution of Dichloromethane

    100_0223.JPG - 378kB
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    13-3-2012 at 05:10
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    [*] posted on 13-3-2012 at 08:02


    Quote: Originally posted by Vlassis  
    Just some caffeine extracted from coffee, having crystallized from an vaporised solution of Dichloromethane



    How many grams did you obtain from this?

    I'm doing a similar thing, and curious to see how I fair.
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    [*] posted on 18-3-2012 at 15:08


    Having eventually got my head round dowloading the photos, I thought this should be in the pretty picture section!
    Ampoules of crystalline Na & K - for sale (they are over 50 years old)! See under shiney K & Na thread.

    PICTNa&K.JPG - 77kB
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    [*] posted on 23-3-2012 at 07:01


    High purity rubidium in ampoule.
    Melted with a heatblower as close to Rb melting point as possible. This slow melting gives the surface this very nice "wave" look.
    This was the first test result


    And here a few of the ampoule. (definately one of my better samples in my element collection) :)







    [Edited on 23-3-2012 by Dennis SK]
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    [*] posted on 23-3-2012 at 13:32


    Some of you might already have seen some of my cesium pictures. But here's one anyway.

    Cesium 99,99%+ in ampoule.
    Grown with temp. control. Took alot of tries to get this result.
    I had absolutely no idea that cesium could make such crystals. So you could imagine the look on my face when I first succesfully made these :o



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    [*] posted on 23-3-2012 at 14:23


    Dennis, those pics are beautiful! I wish I had some ampoules like this, too xD

    offtopic: May I ask where r u from? :)




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    [*] posted on 23-3-2012 at 14:29


    Hello Adas,

    Sure, I'm from Denmark
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    [*] posted on 24-3-2012 at 04:41


    Rubidium ampoule. Now with Cesium ampoules also.

    Sorry for the picture spamming ;)


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    [*] posted on 24-3-2012 at 06:38


    Wonderful.



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    [*] posted on 24-3-2012 at 07:59


    All of that cesium reminds me of Greek mythology. Ichor, the blood of the gods, was said to be golden in color and very poisonous to humans. Cesium metal exactly fits that description! And the crystals of Cs are just great! :D
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    [*] posted on 24-3-2012 at 08:14


    But caesium isn't especially poisonous. It's pyrophoric.

    Dennis SK, great samples. There's a ton of money inside those ampoules...




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    [*] posted on 24-3-2012 at 08:29


    Well, if you eat it, it will probably do a lot of harm and corrode your mucosa very badly (not to mention the explosion). I meant cesium the metal, not the compounds.
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    [*] posted on 24-3-2012 at 08:40


    Quote: Originally posted by Bot0nist  


    I tried, My camera doesn't have a very good macro mode, and I am having trouble getting it to focus on the tower-like structure. I dumped it out to get a more contrasting backdrop. I will try to get a better camera this summer.


    Take another lenses from an old telescope or something similar and place it in front of your camera lenses, generally this allows you to make your own macro and has worked very well in the past for me to take pictures of small crystals.




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    [*] posted on 24-3-2012 at 08:58


    Quote: Originally posted by barley81  
    And the crystals of Cs are just great! :D


    They really are!
    I'll try to grow the same type of crystals with rubidium.
    But its alot harder to control crystal growth in rubidium, but I'll show you the results here if succesful.

    Rubidium has the "funny/interesting" fact that its slightly radioactive. The Rb in the ampoule above gives about 150k Bq, equal to about 4,2 americium fire detectors (calculated)
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    [*] posted on 24-3-2012 at 13:37


    HOLY JESUS!

    That must have been expensive. So beautiful




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    [*] posted on 25-3-2012 at 12:49


    Quote: Originally posted by Endimion17  

    Dennis SK, great samples. There's a ton of money inside those ampoules...


    They wasn't cheap thats for sure.
    But alkali metals have always been some of my favorite elements. So naturally I looked for the best samples I could possibly find.
    It took 5 years and so many inspections of Rb/Cs ampoules.
    Trust me, depending on source its relatively easy to find clean samples of Rb/Cs in ampoules below 10 gram. But to find large clean, particle free samples above 10g of especially Cs... Good luck! :)

    For info the purity are the following:
    Rb, Certified 99,95% minimum. But possibly even more pure.
    Cs, Certified 99,99% minumim.

    Glad you guys like the pictures. Once I get a better camera I will take high-end pictures.


    [Edited on 25-3-2012 by Dennis SK]
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    [*] posted on 25-3-2012 at 13:26


    Tried a bit of experimenting with Cobalt complexes, I attempted to make trans-dichlorobis(ethylenediamine) cobalt(III)chloride.

    The procedure I used instructed(as the before last step) to wash with 6M HCl and vacuum filter, repeating if required until the brown or blue crystals turn green. Mine came out of solution as dark red/orange crystals that did not change color at all despite 4x washes with 6M HCl


    Any ideas what happened? Regardless... Pretty pictures

    [Edit: Initially in the process, after adding the ethylenediamine to the CoCl2 solution, the instructions are to stir vigourously while heating in order to oxidize the Co(II) to Co(III). I wanted to see what would happen if I stirred slowly with a magnetic stirrer and bubble pure oxygen into the solution at the same time over the course of 40 minutes. I am thinking that maybe in doing this the complex was oxidized further?



    cobaltcomplex1.JPG - 157kB cobaltcomplex2.JPG - 95kB

    Also, some tris(ethylenediamine)nickel (II) chloride made this afternoon



    nickelcomplex.JPG - 138kB

    [Edited on 25-3-2012 by Mailinmypocket]
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    [*] posted on 25-3-2012 at 18:32


    oh that purple is such a pretty color! :)
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    [*] posted on 29-3-2012 at 05:51


    Quote: Originally posted by Mailinmypocket  
    trans-dichlorobis(ethylenediamine) cobalt(III)chloride.


    I've synthesized the same complex, but i've obtained a green solid :o
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