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Analytical Chemistry

New Frontiers in Analytical Chemistry

A reader sends this new literature citation along, from Organometallics. He directed my attention to the Supplementary Information file, page 12. And what do we find there?

. . .Solvent was then removed to leave a yellow residue in the vial, the remaining clear, yellow solution was concentrated to a volume of about 1ml, and diethyl ether was added in a dropwise manner to the stirred solution to precipitate a yellow solid. The vial was centrifuged so the supernatant solvent could be decanted off by Pasteur pipette. The yellow solid was washed twice more with ether and the dried completely under high vacuum to give 99mg (93% yield) of product.
Emma, please insert NMR data here! where are they? and for this compound, just make up an elemental analysis…

And don’t forget to proofread the manuscript, either, while you’re at it. Oops.
Update: I see that Chembark is on this one, and has gone as far as contacting the corresponding author, whose day has gotten quite a bit longer. . .

28 comments on “New Frontiers in Analytical Chemistry”

  1. Anonymous says:

    “We were just kidding…..”

  2. UKPI says:

    It’s been the talk of the town all morning on this side of the pond. ChemBark has a post up, followed by quite some discussion about elemental analysis.
    In all places I have worked, the EA submission forms requested the empirical formula (and solvents used) of the submitted compound. In my view this is asking for trouble as well; one should only indicate which elements to measure. Working out potential solvent impurities should be done once the data are there.

  3. Anonymous says:

    Hilarious! Thanks for the lunchtime chuckle

  4. Dr. Zoidberg says:

    Who should be more embarrassed by this, the authors or the reviewers/editor? Looking at the SI, that isn’t just a couple sentences nestled within a large body of text. They would stand out anyways because everything else has detailed NMR and this complex doesn’t. But these are even separated with spaces from the remainder of the text to make them stand out more. Apparently that wasn’t enough for people at multiple levels to catch.

  5. Anon says:

    Annoyed by people at Chembark trying to defend the author and going on about ‘native speaers’ etc…. In my opinion anyway, its pretty clear what this note was asking the student to do.

  6. samadamsthedog says:

    THis reminded me of “The Bedbug Letter” (http://www.snopes.com/business/consumer/bedbug.asp). That legend appears to be false, but toward the end of the article they cite a few examples which they term “almost the bedbug letter”. This fits nicely into that category, and I have duly made snopes.com aware.

  7. Hap says:

    @4: The reviewers ought to be embarrassed for not looking at the SI (or not looking hard enough), but they didn’t ask anyone to fake data, and that’s sure what it looks like the author did.
    I know EA has limited use, but you don’t fill in the blanks just because you don’t want to get one (or pay for one). And if your language or dialect may not be understood by other readers, you could get an editor or someone with a similar language background and better English to look it over first. (Also, I’m assuming the work was done in Switzerland, though I don’t know if the comment was written there or in Australia – if it had been written in Switzerland, the comment should have been written in relatively neutral English, to maximize the likelihood of being understood).

  8. Anonymous says:

    Most likely the student was not able to get the compound clean enough for NMR.

  9. sepisp says:

    I’ve always wondered why everyone insists on a complete collection of useless analytical data, because it’s a lot of work for no apparent benefit. But now I get it. You’re not supposed to actually *measure* them. The classical “if you don’t know who the idiot is, it’s you”.

  10. Puff the Mutant Dragon says:

    OMG!!!! that is freaking hillarious

  11. Project Osprey says:

    @2
    Empirical formula etc can be requested for accuracy reasons. If your expecting a species to be present, but only in low w/w concentrations then you need to prepare a larger sample.
    For combustion analysis, you’ll also want to know how much S and F are present for opperational reasons.

  12. Former Med Chemist says:

    Nothing new here – just less discrete. One of my former coworkers spoke of the days when grad students ran their own elemental analysis. When it didn’t come out, the PI would say “you should run this again”. And did you hear the one about putting your hand in the IR beam?

  13. Am I Lloyd says:

    I actually feel bad about this guy since he doesn’t seem to be a large-scale fabricator like Bengu Sezen and does seem to have been diligent in providing data about the other compounds. And yet this is the kind of thing that can end his career.

  14. Pedro says:

    Have you taken a look at the photos available at the author’s lab website?
    http://dortagroup.scb.uwa.edu.au/Photos.html
    It seems so weird and random… The guy just stands in the background with a sleeveless tshirt holding a beer…

  15. Geir K.-A. says:

    @7 The reviewers don’t necessarily see the final, uploaded version of the SI. As pointed out at ChemBark, maybe the reviewers even requested NMR and EA for this particular compound and are without blame. The authors should definitely have caught this themselves during proofreading, though…

  16. Hap says:

    Probably – they might have caught the hole in the data but the request wouldn’t have been there. Sorry.

  17. Djerassi Unchained says:

    @14 The PI is no longer in Switzerland. He is at Univ. of Western Australia. The photos showing him in a sleeveless t-shirt correspond to formal attire in Perth.

  18. RMartin says:

    I really don´t see the problem here. Supporting Informations are not part of the review process. I don´t see signs of scientific fraud. Calm down guys.
    BTW the prep seems to make sense. Those complexes do crystallize very easily and I would also do it like this. Pouring diethyl ether to the crude and crush this stuff out.
    Just my 2 cents – from a highly experienced organic chemist.

  19. Djerassi Unchained says:

    @18 “Supporting Informations are not part of the review process”
    Please let me know the journals for which you provide peer review, so that I can avoid sending my manuscripts there. As I reviewer, I spend a substantial portion of my effort making sure the science is right in the Supporting Information. It is our job to ensure new compounds are properly evaluated with regard to identity and purity. Most often, the only way to confirm these details is to scour the SI.

  20. a. nonymaus says:

    I’m inclined to side with the comments on Chembark and here about non-native uses of the verb “to make”. Meanwhile, there is something very interesting about the SI compound numbering that suggests that this was in response to a reviewer request and didn’t get sent out for re-review. The compound in question is #14. The next compound in the SI is #154, followed by #165, et seq. So, what we are probably seeing is an original manuscript that got sent out for review and one of the reviewers wanted more about the un-numbered intermediate in Scheme 5 of the article. So, the appropriate reviewer comments are sent back with a “publish after minor revisions”. The authors grunt and strain and send off this intermediate draft of the SI without correcting compound numbering, tabulating the NMR data, or making up a sample for elemental analysis. It, and the revised manuscript without renumbering of Scheme 5 are sent off without any further review by the reviewers until they see it and can say, “…Some one had blunder’d” and all the world wonder’d.

  21. anon says:

    The SI id definitely part of the review process.
    The quote the angewandte journal “The scientific quality of the Supporting Information and the preparation of the text and graphics should be of the same standard as that in the actual publication.”

  22. Yancey Ward says:

    I knew a guy in graduate school that made up the NMR data, too, along with whiting out “solvent peaks”. Guy worked for a world famous natural products guy. Can be quite sure he wasn’t making up the entire synthesis.

  23. Yancey Ward says:

    “Can’t be quite sure”, that is.

  24. Ghost of Woodward says:

    @18 really as an experienced organic chemist, I don’t know what you look at especially at the synthesis details in the supp info.If you just take chemists at their word where is the due diligence required in a peer preview process. If you are reviewing papers let me know, my next paper is going to be “new drug for complete cure of HIV” without any supp info. Take it from me….it works!

  25. lzhi says:

    “make up an elemental analysis” could mean “do an EA” or it could mean “fake an EA”.
    “just make up” seems unlikely to intend the former. Or have EA’s become trivial in terms of analytical time & technique?

  26. DavidA says:

    If nothing else, this paper should make its way up the rankings on the Organometallics “Most Read Articles” tab ! As the old saying goes – there’s no such thing as bad publicity…..

  27. souls_at_zero says:

    @17
    “The photos showing him in a sleeveless t-shirt correspond to formal attire in Perth.”
    Haha, classic! So true. That picture took me right back there.. brick house, sand, and heat.

  28. Anonymous says:

    For the record, an editorial review of this case has been published.
    http://pubs.acs.org/doi/abs/10.1021/om401186q

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