Pages:
1
2 |
DraconicAcid
International Hazard
Posts: 4339
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Online
Mood: Semi-victorious.
|
|
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]
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
|
|
Brain&Force
Hazard to Lanthanides
Posts: 1302
Registered: 13-11-2013
Location: UW-Madison
Member Is Offline
Mood: Incommensurately modulated
|
|
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)!
At the end of the day, simulating atoms doesn't beat working with the real things...
|
|
Praxichys
International Hazard
Posts: 1063
Registered: 31-7-2013
Location: Detroit, Michigan, USA
Member Is Offline
Mood: Coprecipitated
|
|
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."
|
|
unionised
International Hazard
Posts: 5127
Registered: 1-11-2003
Location: UK
Member Is Offline
Mood: No Mood
|
|
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.
|
|
phlogiston
International Hazard
Posts: 1379
Registered: 26-4-2008
Location: Neon Thorium Erbium Lanthanum Neodymium Sulphur
Member Is Offline
Mood: pyrophoric
|
|
Presmably in Nigeria they do not have the same access to resources or education.
Don't blame the authors, blame the poor peer review.
-----
"If a rocket goes up, who cares where it comes down, that's not my concern said Wernher von Braun" - Tom Lehrer
|
|
DraconicAcid
International Hazard
Posts: 4339
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Online
Mood: Semi-victorious.
|
|
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.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
|
|
kmno4
International Hazard
Posts: 1498
Registered: 1-6-2005
Location: Silly, stupid country
Member Is Offline
Mood: No Mood
|
|
Cited journals:
Hetero letters
Electrochem. J. of Chem.
Inorganic Chemical Acta
... and that is all about this "publication".
Слава Україні !
Героям слава !
|
|
The Volatile Chemist
International Hazard
Posts: 1981
Registered: 22-3-2014
Location: 'Stil' in the lab...
Member Is Offline
Mood: Copious
|
|
Sad. That wouldn't have passed our reviews in pre-pub., let alone ACS stuff. Blegh.
|
|
DraconicAcid
International Hazard
Posts: 4339
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Online
Mood: Semi-victorious.
|
|
I managed to get an email to the author, and a response. This could be an interesting conversation.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
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 .
Well done for taking time to email them though.
|
|
The Volatile Chemist
International Hazard
Posts: 1981
Registered: 22-3-2014
Location: 'Stil' in the lab...
Member Is Offline
Mood: Copious
|
|
Really, DA?
Post the conversation so far, I'm curious!
|
|
DraconicAcid
International Hazard
Posts: 4339
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Online
Mood: Semi-victorious.
|
|
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.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
|
|
phlogiston
International Hazard
Posts: 1379
Registered: 26-4-2008
Location: Neon Thorium Erbium Lanthanum Neodymium Sulphur
Member Is Offline
Mood: pyrophoric
|
|
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]
-----
"If a rocket goes up, who cares where it comes down, that's not my concern said Wernher von Braun" - Tom Lehrer
|
|
DraconicAcid
International Hazard
Posts: 4339
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Online
Mood: Semi-victorious.
|
|
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.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
|
|
DraconicAcid
International Hazard
Posts: 4339
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Online
Mood: Semi-victorious.
|
|
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.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
I wouldnt make a good scientist then, I hate criticism!
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 , 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
|
|
Metacelsus
International Hazard
Posts: 2539
Registered: 26-12-2012
Location: Boston, MA
Member Is Offline
Mood: Double, double, toil and trouble
|
|
What was it: anhydrous perchloric acid?
|
|
DraconicAcid
International Hazard
Posts: 4339
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Online
Mood: Semi-victorious.
|
|
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.....
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
Might be your website then, you do have a web site? Yeah I am sure so dont try and hide it lol
|
|
Brain&Force
Hazard to Lanthanides
Posts: 1302
Registered: 13-11-2013
Location: UW-Madison
Member Is Offline
Mood: Incommensurately modulated
|
|
He may be referencing NurdRage.
At the end of the day, simulating atoms doesn't beat working with the real things...
|
|
Amos
International Hazard
Posts: 1406
Registered: 25-3-2014
Location: Yes
Member Is Offline
Mood: No
|
|
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]
|
|
The Volatile Chemist
International Hazard
Posts: 1981
Registered: 22-3-2014
Location: 'Stil' in the lab...
Member Is Offline
Mood: Copious
|
|
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.
|
|
CuReUS
National Hazard
Posts: 928
Registered: 9-9-2014
Member Is Offline
Mood: No Mood
|
|
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
[Edited on 21-10-2014 by CuReUS]
|
|
Metacelsus
International Hazard
Posts: 2539
Registered: 26-12-2012
Location: Boston, MA
Member Is Offline
Mood: Double, double, toil and trouble
|
|
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.
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
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
|
|
Pages:
1
2 |