Quantum
Hazard to Others
Posts: 300
Registered: 2-12-2003
Location: Nowhereville
Member Is Offline
Mood: Interested
|
|
How to purify a chemical to analytical grade
This is of course all thinking as I don't have the money to buy such purification equipment nor any chemicals I wish to purify to such a high
standard.
My question is what equipment would one need to purify a somewhat unstable bioactive chemical to medical grade(for ingestion) to say 99.99% clean all
one isomer ext. The starting product would be somewhat dirty - perhaps not even clean crystals but just a gunk depending on the chemists skill.
The chemist might have say about a gram and want to be able to purify it batch or all at once with such equipment. It would later be split into say
100 microgram units so a machine that can only handle chunks of microgram mass ( say for MS) would not be good.
After all its not much point to make such a chemical if one can not purify it.
[Edited on 6-6-2005 by Quantum]
What if, what is isn\'t true?
|
|
|
vulture
Forum Gatekeeper
Posts: 3330
Registered: 25-5-2002
Location: France
Member Is Offline
Mood: No Mood
|
|
The problem is that the purification process itselfs inserts further impurities. Glassware that's not 100% clean, contaminated solvents, etc.
Impurities are best excluded from the start as every purification step is just a compromise unless done with very pure reagents and you'll lose
massive amounts of yield.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
|
|
|
unionised
International Hazard
Posts: 5102
Registered: 1-11-2003
Location: UK
Member Is Offline
Mood: No Mood
|
|
It rather depends on what you want to purify and what the impurities are. For some materials a couple of recrystalisations will get to 99.99%
For some mixtures your only hope is something like preparative HPLC or CG.
In general, working with small quantities is fiddly, and so it's less efficient.
|
|
|
chloric1
International Hazard
Posts: 1070
Registered: 8-10-2003
Location: GroupVII of the periodic table
Member Is Offline
Mood: Stoichiometrically Balanced
|
|
| Quote: | Originally posted by vulture
The problem is that the purification process itselfs inserts further impurities. Glassware that's not 100% clean, contaminated solvents, etc.
Impurities are best excluded from the start as every purification step is just a compromise unless done with very pure reagents and you'll lose
massive amounts of yield. |
Vulture you couldn't be more right. But consider high purity chemicals come from somewhere. On that note Quantum you should investigate
thoroughly the properties of the compound you are interested and become an authority on that compound and related products.
Most manufacturers specialize. Maybe company A is great at making reagent grade Hydrobromic acid so they carry this expertise toward compounds like
ammonium bromide, cupric bromide, ethyl bromide, etc etc. Get the idea? Why not apply the same philosophy to hobbyist chemistry?
[Edited on 6/6/2005 by chloric1]
Fellow molecular manipulator
|
|
|
Quantum
Hazard to Others
Posts: 300
Registered: 2-12-2003
Location: Nowhereville
Member Is Offline
Mood: Interested
|
|
Hmm. I have done research and flash or gravity chromotography is a good choice. I have got a supplier(UGT) that sells the columns for not to much.
I read about them and how to use them and such and it seems your 'efluent' drips out the bottom with the compound inside it. The question is
how do you know when to catch the drips that have just what you want in them?
I have ordered a Organic Lab Manuel so soon all these stupid questions I have will be answered I guess.
Who here has column chromotography?
What if, what is isn\'t true?
|
|
|
Lambda
National Hazard
Posts: 566
Registered: 15-4-2005
Location: Netherlands
Member Is Offline
Mood: Euforic Online
|
|
Stupid questions ?????
| Quote: | Originally posted by Quantum
I have ordered a Organic Lab Manuel so soon all these stupid questions I have will be answered I guess. |
Quantum, nothing is as stupid as not to ask in the first place. It is easy to stay ignorant, as most people are, for they rather avoid the
"shame" of asking.
Please check these books out on eMule, they may be of great benefit to you, and they are free !!!!
Purification of Laboratory Chemicals (Fifth Edition).pdf (20.15 mb)
http://rapidshare.de/files/2375720/Purification_of_Laborator...
Purification of Laboratory Chemicals_4th ed.pdf (37.29 mb)
http://rapidshare.de/files/2369172/Purification_of_Laborator...
Academic Press, Encyclopedia of Biological Chemistry Vol. 1 (2004); BM OCR 7.0-2.5.pdf (23.21 mb)
http://rapidshare.de/files/2350280/Academic_Press__Encyclope...
Academic Press, Encyclopedia of Biological Chemistry Vol. 2 (2004); BM OCR 7.0-2.5.pdf (19.43 mb)
http://rapidshare.de/files/2349890/Academic_Press__Encyclope...
Academic Press, Encyclopedia of Biological Chemistry Vol. 3 (2004); BM OCR 7.0-2.5.pdf (18.99 mb)
http://rapidshare.de/files/2350280/Academic_Press__Encyclope...
"The Total Bio-Chemical Laboratory Manual" is also available.
Allso search "chromatography", "Biological", "Bio-Chemical", "Purification" and "Chemistry".
| Quote: | Knowlege is to know that a bee can sting, wisdome is to know how to avoid the sting !
|
[Edited on 14-6-2005 by Lambda]
|
|
|
Taaie-Neuskoek
Hazard to Others
Posts: 222
Registered: 14-5-2004
Location: Zermany
Member Is Offline
Mood: Botanical!
|
|
| Quote: |
I read about them and how to use them and such and it seems your 'efluent' drips out the bottom with the compound inside it. The question is
how do you know when to catch the drips that have just what you want in them?
|
If you compound is invisible, so it doesn't have a colour, TLC might be an option.
So you eluate every 5 minutes in a different vial, do TLC on all of them, and then look in which vail(s) your compound is.
Before you indest anything, I would search someone with some spare time and an analytical instrument to see what's actually in there...
Never argue with idiots, they drag you down their level and beat you with experience.
|
|
|
IrC
International Hazard
Posts: 2710
Registered: 7-3-2005
Location: Eureka
Member Is Offline
Mood: Discovering
|
|
Am I mistaken or is the link for Encyclopedia of Biological Chemistry Vol. 3 identical to the link for volume 1?
|
|
|
Lambda
National Hazard
Posts: 566
Registered: 15-4-2005
Location: Netherlands
Member Is Offline
Mood: Euforic Online
|
|
Volume 3 is wrong, and will be uploaded again
Sorry about this IrC. strang that it is only now noticed, for this file has been downloaded 9 times.
I don't seem to be able to edit my post, but this will be corrected as soon as I can find volume 3, and uploade it again.
Thank you for observing this error !
[Edited on 16-6-2005 by Lambda]
|
|
|
uber luminal
Hazard to Others
Posts: 124
Registered: 25-8-2004
Member Is Offline
Mood: No Mood
|
|
buying it pure might be cheaper.
|
|
|
Lambda
National Hazard
Posts: 566
Registered: 15-4-2005
Location: Netherlands
Member Is Offline
Mood: Euforic Online
|
|
ERRATA ! Academic Press, Encyclopedia of Biological Chemistry Vol. 3 (2004)
IrC had rightly remarked about the erroneouse link that I had given to:
Academic Press, Encyclopedia of Biological Chemistry Vol. 3 (2004)
I have uploaded this book again to Rapid Share.
Academic Press, Encyclopedia of Biological Chemistry Vol. 3 (2004); BM OCR 7.0-2.5.pdf (18.99 mb)
http://rapidshare.de/files/2475331/Academic_Press__Encyclope...
I apologise for this mistake.
|
|
|
Jettin4u
Harmless
Posts: 8
Registered: 1-7-2005
Member Is Offline
Mood: No Mood
|
|
When you are talking micrograms, tlc is not always the best bet, especially if it is hard to detect, if it has color it would make it somewhat more
easy. And usually crystalizations work better if you have more products because you would filter away your junk. Sounds like a tough one if you dont
have alot of the product. say 5grams at the least.
|
|
|
Beatnik
Harmless
Posts: 11
Registered: 21-3-2004
Member Is Offline
Mood: No Mood
|
|
Im trying to build a verticle zone melting/refinement device, As a alternative to recrystalisations. Along with a few other things.
Ive found that Analytical chem texts all have "sample preparation/purification" chapters, its worth looking into....
|
|
|
neutrino
International Hazard
Posts: 1583
Registered: 20-8-2004
Location: USA
Member Is Offline
Mood: oscillating
|
|
I was thinking that too, but I don't think an unstable chemical would survive too many meltings.
|
|
|
jqwhy
Harmless
Posts: 3
Registered: 14-12-2005
Member Is Offline
Mood: No Mood
|
|
the address is wrong or timeout
|
|
|
Darkblade48
Hazard to Others
Posts: 411
Registered: 27-3-2005
Location: Canada
Member Is Offline
Mood: No Mood
|
|
Well, it is over 5 months old...
|
|
|
andresderis
Harmless
Posts: 49
Registered: 24-8-2006
Location: santiago
Member Is Offline
Mood: No Mood
|
|
| Quote: | Originally posted by jqwhy
the address is wrong or timeout |
|
|
|
kazaa81
Hazard to Others
Posts: 368
Registered: 30-4-2004
Member Is Offline
Mood: ok
|
|
I'm sorry to bring up such an old thread but...
wouldn't be better to upload "Purification of Laboratory Chemicals (Fifth Edition)"
on another web hosting, instead of rapid sha re?
I couldn't find a working link about these books all trough the forum !
thank you
[Edited on by kazaa81]
|
|
|
hinz
Hazard to Others
Posts: 200
Registered: 29-10-2004
Member Is Offline
Mood: No Mood
|
|
Voilà ici:
http://www.megaupload.com/de/?d=MPCOHWJE
|
|
|
kazaa81
Hazard to Others
Posts: 368
Registered: 30-4-2004
Member Is Offline
Mood: ok
|
|
thank you!
is it just me, or that wasn't OCRed ?
being tired of rapidshare and/or megaupload for obvious reasons,
I've uploaded it on uploading.com
http://www.uploading.com/files/W1NJMAO4/Purification_of_Labo...
|
|
|
Sauron
International Hazard
Posts: 5351
Registered: 22-12-2006
Location: Barad-Dur, Mordor
Member Is Offline
Mood: metastable
|
|
If you mean ACS AR grade then you need the large and costly ACS book of specifications to start with. These are unique for every listed substance.
One of the major purification techniques is chromatography, so you are likely looking at prep scale ion chromatography, size exclusion, gel
filtration, HPLC, etc. Ion exchange resins.
In many instances, unless you are equipped to do the job already, there will be no cost effective way to get to AR grade that will compete with buying
the requisite compound in that grade. It's a matter of economy of scale. The capital expense might be the same to make 25 g or a ton, you see.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
