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DBL%20Hendrix%20small.png College chemistry, 1983

Derek Lowe The 2002 Model

Dbl%20new%20portrait%20B%26W.png After 10 years of blogging. . .

Derek Lowe, an Arkansan by birth, got his BA from Hendrix College and his PhD in organic chemistry from Duke before spending time in Germany on a Humboldt Fellowship on his post-doc. He's worked for several major pharmaceutical companies since 1989 on drug discovery projects against schizophrenia, Alzheimer's, diabetes, osteoporosis and other diseases. To contact Derek email him directly: derekb.lowe@gmail.com Twitter: Dereklowe

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August 8, 2013

Make Up the Elemental Analysis: An Update

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Posted by Derek

Chemistry Blog has more on the incident picked up first at ChemBark and noted here yesterday. This rapidly-becoming-famous case has the Supporting Information file of a paper published at Organometallics seemingly instructing a co-author to "make up" an elemental analysis to put in the manuscript.

Now the editor of the journal (John Gladysz of Texas A&M) has responded to Chemistry Blog as follows:

Wednesday 07 August
Dear Friends of Organometallics,

Chemical Abstracts alerted us to the statement you mention,which was overlooked during the peer review process, on Monday 05 August. At that time, the manuscript was pulled from the print publication queue. The author has explained to us that the statement pertains to a compound that was ”downgraded” from something being isolated to a proposed intermediate. Hence, we have left the ASAP manuscript on the web for now. We are requiring that the author submit originals of the microanalysis data before putting the manuscript back in the print publication queue. Many readers have commented that the statement reflects poorly on the moral or ethical character of the author, but the broad “retribution” that some would seek is not our purview. As Editors, our “powers” are limited to appropriate precautionary measures involving future submissions by such authors to Organometallics, the details of which would be confidential (ACS Ethical Guidelines, http://pubs.acs.org/page/policy/ethics/index.html). Our decision to keep the supporting information on the web, at least for the time being, is one of transparency and honesty toward the chemical community. Other stakeholders can contemplate a fuller range of responses. Some unedited opinions from the community are available in the comments section of a blog posting: http://blog.chembark.com/2013/08/06/a-disturbing-note-in-a-recent-si-file/#comments

If you have any criticisms of the actions described above, please do not hesitate to share them with me. Thanks much for being a reader of Organometallics, and best wishes. . .

This is the first report of the corresponding author, Reto Dorta, responding about this issue (several other people have tried to contact him, with no apparent success). So much for the theory, advanced by several people in the comments section at ChemBark, that "make up" was being used in the British-English sense of "prepare". Gladysz's letter gets across his feelings about the matter pretty clearly, I'd say.

Comments (31) + TrackBacks (0) | Category: The Dark Side | The Scientific Literature


COMMENTS

1. David on August 8, 2013 10:14 AM writes...

I'm British and see no reason to use 'make up' to mean prepare in this case. It is true that 'make up' is sometimes used to mean 'prepare', but only in the sense of "I made up an NMR sample, by putting a solution in a tube". No-one 'makes up' data in the sense of 'preparing' an SI in British English, the only connotation in British English of 'making up' data is to invent it!

The kicker is the wording used by the author in the SI. If they had meant prepare, why not say "insert the NMR and EA data"? Why have two sentences to say the same thing? 'Make up' means 'invent' in this case.

This is indefensible, especially from a language argument.

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2. Anonymous on August 8, 2013 10:48 AM writes...

Yup, another "British-English" here and I 100% agree with David's comments

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3. Winnie bluesky on August 8, 2013 10:58 AM writes...

Even as a non-native but living in the UK, there is nothing one makes up in the lab except a solution in a volumetric flask (and that is making it up TO a certain volume) by diluting the stock...

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4. Oops... on August 8, 2013 10:59 AM writes...

I wonder if Prof. Gladysz will share the microanalysis data results with the rest of us too?

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5. Giles on August 8, 2013 1:27 PM writes...

Another Brit agreeing that making something up almost invariably means faking it.

On the other hand, one of the funniest sketches in a UK comedy program called Brass Eye in the 90s involved persuading various unwitting celebrities to speak out against a non-existent drug called "Cake", which they were told was a "made-up" drug -- that is, it was synthetic. Questions were asked in Parliament... presumably "made-up" in the sense of synthetic was believable enough to the celebs that they were willing to use it in that sense and didn't immediately realise they were being trolled.

Rather NSFW (swearing) YouTube of the sketch here: http://www.youtube.com/watch?v=g0GxUxKZdHk

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6. Godfrey Bloom on August 8, 2013 1:33 PM writes...

Perhaps he was asking Emma to put on some make up before getting the analysis done.

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7. Anonymous on August 8, 2013 2:16 PM writes...

This is hilarious at first...until I read the paper and SI in details, and I just felt sad for all the authors involved.

The cmpd in question indeed was a never isolated proposed intermediate with only in situ HNMR (see below for quoted paragraph from the original article, page G). So there was, of course, no EA data. O what the heck just make up some numbers to shut up these stupid reviewers--the PI must have thought.

If he had just replied to the editor by stating the fact it probably wouldn't have affected its acceptance anyway.

BTW, the cmpd numbering in SI from 14 and on are quite messed up if you just look at Schemes 5 & 6. So sloppy work by both the authors and reviewers IMHO.

"When 5a was treated with only 1 equiv of AgBF4, unlike in the Pd case, a chloro-bridged complex was formed. No crystals could be grown to confirm the structure, but an in situ 1H NMR spectrum after the first step of the reaction to form 14
showed the ligand to be still symmetric...This intermediate then reacted cleanly with 1 equiv of Ag(acac) (acac = acetylacetonate)to give the monocationic complex 14..."

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8. road on August 8, 2013 2:36 PM writes...

@7 I sympathize, too, but once you start down the road of fabricating inconsequential data, it's a pretty slippery slope.

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9. The Iron Chemist on August 8, 2013 3:15 PM writes...

"The cmpd in question indeed was a never isolated proposed intermediate with only in situ HNMR (see below for quoted paragraph from the original article, page G). So there was, of course, no EA data. O what the heck just make up some numbers to shut up these stupid reviewers--the PI must have thought.

If he had just replied to the editor by stating the fact it probably wouldn't have affected its acceptance anyway."

Obtaining the elemental analysis for a compound that couldn't be isolated wouldn't be the strangest thing a referee's ever insisted upon as a pre-requisite for publication, I'm afraid.

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10. BTDT on August 8, 2013 7:57 PM writes...

I have (legitimately) included the following line in a number of experimentals that have been published over my career:
"The instability of intermediate X precluded obtaining satisfactory EA"
Mom was right - honesty is the best policy.

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11. samadamsthedog on August 8, 2013 8:48 PM writes...

Two things.

1. When I the story to several colleagues and friends, the saddest thing was that most of them said something like, "I'm not at all surprised."

2. A question. When you review an article, do you review the supplemental material? Personally, I look at it only if I need to in order to clarify my understanding of something in the article.

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12. Scientist on August 8, 2013 9:21 PM writes...

Yes, you review the SI! You review the whole paper. If you aren't reading the SI, you probably didn't read it closely enough. I sympathize with people who are too busy, but that's probably the point at which you should be passing along the papers to former grad students/current postdocs (or asking grad students with expertise to help out with the review).

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13. Anonymous on August 8, 2013 9:30 PM writes...

Are there any reviewers that would be tempted to let something like this slip by in order to publicly expose the attempted fraud? If you rejected the paper based on the note in the SI, would it be likely that the authors would "fix" the errant comment and publish elsewhere, being more diligent to cover up tracks in the future?

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14. Bender on August 9, 2013 12:30 AM writes...

Everybody knows that if you don't want to put the effort into proper SI you submit to Elsevier. That would've solved this whole debacle.

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15. LionKing on August 9, 2013 1:17 AM writes...

Slip of the tongue (or the keyboard). Nothing unusual in it happening ---It even happens to US presidents like W.
Do we know where the funding for this research came from, its monetary size, and if there was a reaction to the news by the funding agency?

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16. LionKing on August 9, 2013 1:22 AM writes...

Slip of the tongue (or the keyboard). Nothing unusual in it happening ---It even happens to US presidents like W.
Do we know where the funding for this research came from, its monetary size, and if there was a reaction to the news by the funding agency?

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17. Anon on August 9, 2013 3:40 AM writes...

Language-wise: Of course, the phrase used is only correct if they really meant "to invent" some data. However, I have no idea how fluent (and grammatically,... correct) the author is in english. I have heard the phrase more than once in the context of preparing a sample. I am German by the way.

Did he really order his student to fabricate data? Nobody knows for sure, but I am rather convinced he did. And I am by no means suprised. On the one hand, I have to agree with #9: Reviewers sometimes request the strangest things and are a) not easily convinced that they demand bulls*** and b) not the quickest to reply to your concerns in less than two weeks. If you want to just get the paper out...
On the other hand, how often do you see 100mg reactions yielding 90%+ that have a matching EA? I am sure, that in most cases either yield or EA is fake (including doing EA on a batch that yielded only 55%, but using the reaction that yielded a barely recognizeable 1H to give the yield).
And to all those that demand public decapitation of the suspect. I am willing to bet that at least 30% of any(!) audience at a conference would be headless, if that punishment were standard protocol...
And no, I never faked EA :-) I generally get around submitting 3-10 samples to barely trained and capeable technicians until one gives the correct values by blaming instability/hygroscopicity.

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18. Nodz on August 9, 2013 4:24 AM writes...

To me the damning word is "just".

"make up the EA" = some (not a lot, but some) doubt as to language/intent. Maybe its legit.

"just make up the EA" = sorry broseph, no doubt as to what is going on here. Busted!

And no, Im not surprised. Does anyone really doubt that there is a lot of HRMS or EA fudgery out there? I am surprised that he put the fake data request 1) in writing and 2) in the freakin manuscript!

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19. Anon on August 9, 2013 7:03 AM writes...

Nothing in science should be "made up", except buffers and solutions.

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20. Alex on August 9, 2013 2:17 PM writes...

This might come as a shock to some scientists out there, but A LOT of elemental analyses that are published are made up. Quite a few theoretical yields also are not what they should be (for example, the highest of all measured yields, and not an average). Pretty much most organic compounds you obtain are oils, and getting a good elemental from an oil in my experience is next to impossible. You will have an exemplary 1H NMR and 13C NMR, but rest assured your elemental will be way off in at least one element.

In my PhD days I avoided this burden by doing HRMS instead- getting a decent elemental analysis on ~100 new complex organometallic oils would have probably left me brain dead

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21. crankcase on August 9, 2013 4:39 PM writes...

Derek--let the B-team cover this one--they have it and the torches/pitchforks well in hand.

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22. jbosch on August 9, 2013 7:57 PM writes...

Well, it's a bit dicy.
As a German I would rather go by
"Mach's halt" as short for "Mach es halt", which can be translated into many variants, the worst such variant could include "make up that damn analysis ..." but more in the sense of do the experiment, why the hell did you not include this ? This is your oversight [add additional blaming words].
Does not necessarily speak for the PI as mentor but would fit into the mentality of some German/Austrian/Swiss PI's.

How about this phrase ?
"Make up that figure, where's the problem? You have all that data."

And what I wanted to say with this sentence was, assemble the pieces of data into a nice publishable figure with various panels. You have all that stuff dispersed over 10 slides in a Keynote presentation, summarize it and make it presentable.

In dubio pro reo.
I expect this to be a translation error and not an instruction to fabricate data.

Just think about this for a minute, if you ask somebody to fabricate the data you will be in trouble later. Most fabricated stuff comes from first authors or PI's where the first author does not know what the PI submitted. And to avoid this I guess many papers have included the group-emailing behavior to send out an email to all authors. Sure one could simply fake the email accounts of the co-authors.

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23. Morten G on August 10, 2013 5:39 PM writes...

I notice that the Organometallics are not at any fault (according to the statement from the Organometallics editor).

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24. ib1 on August 11, 2013 11:22 AM writes...

I feel for the authors, they are facing a not-so-fair worldwide barrage. The PI was implicitly saying that the Elemental Analysis does not bring any value to an experimental part; and he did not want to provoke a requirement from some over-the-top referee. I am seeing two big questions here:
1- Is the EA a must have? During my PhD, I have been really annoyed with the escalade in analytical data where a NMR and a MS were more than sufficient. Sometimes the IR gave me some crucial information. Ten years later, I still do not see any utility to the EA.
2- Is it to the referee to ask for an un-necessary analysis or for repeat of experiments? I too often to my taste have to challenge referees with their requirements, saying plainly that I dis-agree with their point. I may be pretentious, but I consider myself as the expert of my work and referees are here to judge if the work can be publish in the high impact-factor journal, maybe correct some English syntax, and if I am lucky possibly challenge me scientifically, so I can add value to the paper. At least, this is where I stand when I am asked to do that.
Let’s not give discredit to a group because of this sentence; if you look at the big picture, it is not a proof of dis-honesty. I personally do not consider this as an ethical issue. Don’t get me wrong, the PI asking for a student to make up an analysis is still a breach of trust (quite frankly if you want to cheat, make up the EA yourself), but it is not like they have done the same as the Diederik Stapel or JJ la Clair.
I would give them a break and a second chance. Let’s not kill a group because of that and only judge the scientific work.
I want to point out, I have no stake in the work published, do not know the authors and do not even work in organometallics chemistry.

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25. Mike on August 11, 2013 3:07 PM writes...

Sadly, I have seen repeated examples of this kind of behaviour: faking of EA data by inorganic chemists (two academics at a middle-sized uni in eastern europe). At one point, almost the whole faculty (inc. head of school) knew about it, but they have done nothing (except politely telling the offenders not to do this anymore and forcing the whistleblower to shut up)! One of this people moved to industry (to a senior position), the other will shortly be promoted to senior professorship.

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26. anon on August 11, 2013 3:44 PM writes...

This is an example of this kind of fakery that I remember from my previous-previous uni. One guy submitted a paper to Polyhedron with a solvated complex in the experimental part (but the fake EA was for the unsolvated one). One of the referees spotted the disrepancy, so the lead author resubmitted the corrected manuscript with a fake EA of the solvate (explaining that he repeated the analysis on a purified sample). Another example from the same uni: the manuscript about some inorganic complexes (with x-ray structures) was almost prepared for submission, just one of the collaborators was asked to run the NMR. He found out that the complex cocrystallized with HBr (stoichiometric amount of HBr seen on 1H-NMR) – which was neither present in the x-ray structure, nor in the fake EA. So the x-ray was re-solved with HBr in the unit cell, and the EA recalculated and everything got published. As far as I know, this practice ran for years. The problem is that there is no written evidence…

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27. simpl on August 12, 2013 5:16 AM writes...

EA used to be important in the golden age of chemistry, around the time of Berzelius.

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28. anon on August 12, 2013 12:56 PM writes...

@24: Sorry, no sympathy here.

If you don't think EA is necessary, and the reviewers do (and the editors don't overrule them), you complain to the editor, do the analyses anyway, or take the paper elsewhere (assuming other journals will take the paper without the missing EA, which is likely). If enough authors (who, in the most likely publication scenario, are paying the freight for a journal) don't want to do EA to get in a journal, they can go elsewhere, and the parent journal will have to decide how badly it needs EA to validate its contents. What you don't get to do is make up your own rules for publication. If you want the credit of being in journal X, then you have to play by their rules (because that's at least some of how they got the reputation they did). In addition, in the case or organometallic compounds, where NMR or HPLC analyses may not be applicable or give you a complete idea of purity or composition, EA seems like a good idea.

There have been complaints about excessive reviewer requests. I would be more likely to hold my ground on something where the work can be repeated only with difficulty or will take a lot of time to repeat. I don't know how long it would have taken to repeat this preparation, but I am not guessing enough to be worth faking it instead.

Making up data is probably one of the few deadly sins in science. Most people aren't going to do your experiments - all they have is your word and the data that they were done. Once they know that when things get inconvenient, you'll make stuff up (or order someone else to), it becomes for them to hard to know when you've told them everything and when you've taken unscientific license with your data.

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29. Paul on August 12, 2013 11:40 PM writes...

@24 Performing an EA analysis is part of ensuring that the compound is indeed what you claim. If you are using any element for which there is not a convenient NMR-active nucleus, then an EA is a must. Mass spec may show that you have what you want, but does a relatively poor job of showing other impurities (and their quantity). Many may claim that an EA is unnecessary (and trust me when I say that obtaining an EA on a pyrophoric liquid is a large headache!), but as somebody who has seen

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30. Perdurabo on August 19, 2013 2:43 PM writes...

I see this story has made Chemical & Engineering News today. Probably not the way the authors envisioned being reported

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31. Anonymous on February 26, 2014 10:29 PM writes...

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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