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DraconicAcid
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[*] posted on 1-10-2014 at 08:49
A Lousy Paper


Doing a bit of googling for salicylate complexes brings me this paper:

http://iosrjournals.org/iosr-jac/papers/vol7-issue4/Version-...

They make metal salicylates by refluxing the acid with a transition metal salt for two hours in mixed-water/ethanol, and filtering off the precipitate. They characterize the salicylates by IR, UV/Vis, mp, and conductivity measurements, and report that they are all either M(sal)2 or M(sal)3 (where "sal" = the salicylate dianion, with both the phenolic and carboxylic acid protons removed). They also seem to think that the phenolic hydrogen will ionize without the addition of another base.

It does not occur to them that a divalent metal will either coordinate 1 dianionic "sal" ligand, or two monoanionic "Hsal" ligands to make an electrically-neutral product.

They do not seem to realize that the replacement of ligands on Cr(III) and Co(III) is very slow, and do not test for the presence of chlorine in the products (despite making them from the chlorides).

They do not notice that the spectra of the products they get from Co(II) and Co(III) are very similar (and would probably look identical if shown on the same scale). Their melting points and colours are similar, and I'd guess that one is simply a less-pure form of the other.

[Edited on 1-10-2014 by DraconicAcid]




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Brain&Force
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[*] posted on 1-10-2014 at 09:54


Who made those graphs? All of them are scaled differently. I could have written a better paper by myself (and I don't even have a lab notebook)!



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[*] posted on 1-10-2014 at 10:26


They would have done well to roast the salicylates until they were metals or oxides, and use the mass loss to empirically determine the true ratio of salicylate to metal in each sample.

If the mass loss had ambiguity, I would take each precipitate and reflux it with dry toluene using a dean-stark trap with K2CO3 in it to suck up any leftover acids and water that might be part of the crystallization. Filter, wash with more toluene, dry in vacuo, try again.

What the heck is with the MP of Co(sal)3? It is listed as "13-215."




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unionised
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[*] posted on 1-10-2014 at 11:07


Well, OK, it's a lousy paper.
What do you expect from a journal that's a short step away from vanity publishing?
Incidentally, their UV/vis spectra are all pretty meaningless too.
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[*] posted on 1-10-2014 at 11:31


Presmably in Nigeria they do not have the same access to resources or education.

Don't blame the authors, blame the poor peer review.




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DraconicAcid
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[*] posted on 1-10-2014 at 12:15


Quote: Originally posted by Praxichys  
What the heck is with the MP of Co(sal)3? It is listed as "13-215."


I assumed that was a typo for 213-215 oC.

But, yeah, it's basically a vanity publisher with no peer review, so we can't expect much better. But I've had first-year students from Nigeria who could have spotted these mistakes.




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[*] posted on 1-10-2014 at 14:55



Cited journals:

Hetero letters
Electrochem. J. of Chem.
Inorganic Chemical Acta

... and that is all about this "publication".




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[*] posted on 7-10-2014 at 12:40


Sad. That wouldn't have passed our reviews in pre-pub., let alone ACS stuff. Blegh.



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DraconicAcid
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[*] posted on 13-10-2014 at 13:16


I managed to get an email to the author, and a response. This could be an interesting conversation.



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[*] posted on 13-10-2014 at 13:28


This is why its not always a good idea for noob like me TUTFSE! How would I know it was shite?
thats why I ask basic stuff :D.
Well done for taking time to email them though.
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[*] posted on 14-10-2014 at 15:05


Really, DA?
Post the conversation so far, I'm curious!




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[*] posted on 14-10-2014 at 15:18


Quote: Originally posted by The Volatile Chemist  
Really, DA?
Post the conversation so far, I'm curious!


So far, he's just confirmed that I've contacted the correct person.

I won't reproduce the conversation here (that would be a breach of ethics), but I'll let you know how it goes. I'm hoping to give him enough constructive criticism that he revisits these complexes and fixes his errors- my goal is not to simply insult him or make fun of him.




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[*] posted on 14-10-2014 at 16:41


He is probably just excited that someone read his paper and took up an interest in it, even if it is for a different reason than a shared interest in the scientific content.
Good scientist tend to take criticism pretty well, its part of the job (as is criticizing other scientists research/finding the weak spots).

[Edited on 15-10-2014 by phlogiston]




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[*] posted on 14-10-2014 at 17:47


Quote: Originally posted by phlogiston  
He is probably just excited that someone read his paper and took up an interest in it, even if it is for a different reason than a shared interest in the scientific content.
Good scientist tend to take criticism pretty well, its part of the job (as is criticizing other scientists research/finding the weak spots).


I hope he feels the same way as you. So far, he hasn't shown much excitement.




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[*] posted on 17-10-2014 at 15:27


I pointed out that his formulations (with doubly deprotonated salicylates) were certainly wrong, and he wrote back to agree, blame the MSc student, and apologize. I replied with a list of the other criticisms I had- we'll see what he says.



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[*] posted on 18-10-2014 at 09:33


I wouldnt make a good scientist then, I hate criticism! :D
I have seen your you tube channel Draconic Acid, it made me feel so very much better knowing that at my age you had similar disasters that I do lol.

Nitric acid and sodium bicarb in too small a vessel and too large a quantity WOOSH, also had some copper in, so a lovely blue fountain :D, I am still cleaning it all up!
Ruined the power supply as acid got in and the copper traces in parts are no more. I also had a run in with what I though was fuming nitric acid and turned out to be something else far more dangerous lol
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[*] posted on 18-10-2014 at 10:48


What was it: anhydrous perchloric acid?



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DraconicAcid
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[*] posted on 18-10-2014 at 12:01


Quote: Originally posted by Little_Ghost_again  

I have seen your you tube channel Draconic Acid, it made me feel so very much better knowing that at my age you had similar disasters that I do lol.


Which? What? I don't have a Youtube channel.....




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[*] posted on 18-10-2014 at 13:31


Might be your website then, you do have a web site? Yeah I am sure so dont try and hide it lol
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[*] posted on 18-10-2014 at 13:34


He may be referencing NurdRage.



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[*] posted on 19-10-2014 at 08:59


Quote: Originally posted by Little_Ghost_again  
Might be your website then, you do have a web site? Yeah I am sure so dont try and hide it lol


I think you mean Bromic Acid. HE has the list of childhood disasters that is commonly referenced on here, not DraconicAcid.

Here is what I think you're talking about : http://www.bromicacid.com/mistakes.htm

[Edited on 10-19-2014 by No Tears Only Dreams Now]




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[*] posted on 20-10-2014 at 16:28


Yea, bromic acid's a pretty cool guy, I don't see him around much anymore, too bad. He was one of the people who convinced me to join this site.



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[*] posted on 21-10-2014 at 04:09


Quote: Originally posted by Little_Ghost_again  
I also had a run in with what I though was fuming nitric acid and turned out to be something else far more dangerous lol

Quote: Originally posted by Cheddite Cheese  
What was it: anhydrous perchloric acid?


i think most probably he ended up collecting nitrogen dioxide(in the liquid state) in the condensing flask;)
if you use a very strong acid along with a nitrate salt ,that's what happens:D

[Edited on 21-10-2014 by CuReUS]
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[*] posted on 21-10-2014 at 07:18


Correction: if you do it at atmospheric pressure. Using a vacuum prevents decomposition. I have distilled nearly anhydrous nitric acid from sodium nitrate and Rooto concentrated sulfuric acid under vacuum without problems.



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[*] posted on 22-10-2014 at 16:38


No it turned out to be hydrofluric acid, or maybe olieum. Not sure which way around it was now because I ended up with both for a very short time, it all went a bit tits up. Dad ended up doing a hazmat on it and got it back to its correct home at the uni lab it came from.
Anyway las time I do iffy deals with lab cleaners
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