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DIY Thin Layer Chromatography Options
 
endlessness
#21 Posted : 5/30/2011 4:11:53 PM

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Here im attaching a paper on TLC:

1978 MAJAK et al, TLC luminescence of gramine and
related indole alkaloids in Phalaris arundinacea
 

Explore our global analysis service for precise testing of your extracts and other substances.
 
Dr_Sister
#22 Posted : 5/30/2011 4:18:13 PM

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Aha! Far out, thanks endlessness! Very happy
 
Mydriasis
#23 Posted : 5/30/2011 9:30:08 PM
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http://www.google.com/ur...3D_CIJYf89A&cad=rja

Here's something on TLC and Van Urks with a mention of gramine.

If anyone ever gets a grass extract there are a few ideas we have come up with in chat, that should really be tried out(no column involved).
It's been fun. Thanks for all the wisdom.
 
Tsehakla
#24 Posted : 5/30/2011 11:01:41 PM

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burnt wrote:
While I'd certainly encourage do it yourself TLC just one note. Silica dust is toxic. It will get in your body and stay there. Its kind of like breathing asbestos. So just make sure to wear mask when making your own TLC plates or cutting up TLC plates. Also work in an area you can easily clean etc usual lab stuff.

That is somewhat overstated.

Asbestos causes a type of cancer, crystalline silica dust can cause silicosis (essentially lesions), amorphous silica (which is what Silica gel is) dust may not clear out of the lungs but is otherwise not toxic.

Of course wearing a mask is always a good idea, but if you grind your silica gel wet you shouldn't raise any dust and wearing a mask when cutting up the occasional TLC plate is likely overkill.

OTOH, the blue or green bits of silica gel are another story, they most likely contain cobalt(II) chloride and that stuff is toxic (maybe even carcinogenic).

I only mention this because I've run into some pretty irrational fear of silica gel over the years.
Two things to keep in mind:
1) It is all lies.
2) There is no privacy on the Internet.
 
Dr_Sister
#25 Posted : 5/31/2011 1:55:05 PM

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Mydriasis - that is an awesome reference, more than Sister had hoped for. Thank you! Cool
 
tryptographer
#26 Posted : 10/24/2011 9:47:55 PM

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This is a great thread, thanks Benzyme and all others!

Wow, loads of high quality information to digest and hopefully put into practice - there goes my free time Pleased
 
Dozuki
#27 Posted : 11/8/2011 3:58:20 AM

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The best solvent system that I've run has been IPA:NH4OH:H2O (9:1:1 - 91%:10%:100%), for acidic conditions try: IPA:AcOH:H2O (9:1:1 - 91%:30%:100%) All easily aquired solvents. I've run 10+ solvent systems from both the literature and suggested from other ppl that use harder to get solvents (n-Butanol, etc.) but these have worked the best for me.

As for Visualization, Xanthydrol has been the best of the 3 I've used, the other 2 are Ehlrich's and vanillin. All of them work better when heated. A small toaster oven is perfect for this, and can easily be had at a thrift store. Vanillin can be extracted from imitation vanilla extract. There are videos on you tube on how to this. Look at the solubility of vanillin, and you can probably find a suitable extraction solvent other than diethyl ether (what the you tube video I saw suggests).

As for re-agent sprayers, look at the local home improvement stores for the paint sprayers with the little aerosol can that screws onto the glass jar to hold paint. These are the same things that are sold at Chromatographic supply places and are probably much cheaper. After use, spray water through them to clear out any chemicals, especially acids and they can be use again. If you don't, they become one time use products and very expensive. It would also be totally feasible to use an air brush for this, tho much more expensive.

Vanillin Reagent:

1> 15g Vanillin : 250ml EtOH : 2.5ml H2SO4
2> 6% Vanillin : 1% H2SO4 : in EtOH

Heat to ~ 120 for 5 Minutes. (typically used for essential oils)

Xanthydrol:

100mg Xanthydrol : 94ml EtOH : 5ml HCl

Some of the Phalaris literature uses Phosphoric Acid instead of HCl, I can dig it up if anyone wants...
DMT - PURPLE
5-MEO - Blue
Gramine - Pink

Also, Marquis reagent might be useful as there is lots of info on color reactions with various compounds:

1>37% Formaldehyde : H2SO4 (conc.) [1:15]
2>Mix 10ml conc. H2SO4 with 8-10 drops of ~ 40% formaldehyde solution

These should be made up fresh and don't necessarily need heat.

 
nen888
#28 Posted : 11/8/2011 4:43:37 AM
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..excellent info. again thanks Dozuki... (& benzyme and all)
 
benzyme
#29 Posted : 11/19/2011 12:22:29 AM

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"Nothing is true, everything is permitted." ~ hassan i sabbah
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InMotion
#30 Posted : 6/10/2012 2:39:36 AM
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If you are anything like me you know preparing plates is a serious pain in the genitalia.

"I got somethin fo your candy", J.roc

*ends incoherent sales pitch*

Taken from -
Author: Weygand and Hilgetag, Title: Preparative Organic Chemistry
InMotion attached the following image(s):
tlc_tool.png (481kb) downloaded 152 time(s).
 
Parshvik Chintan
#31 Posted : 6/29/2013 8:31:04 AM

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whew! i can finally comprehend TLC (seriously i was beginning to feel dense).
awesome thread.
thanks benz for the pdf, and everyone else for contributing.
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ๆจน
 
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