Smut Clyde

Epileptic spasms of tics and glitches in Krautrock diffractograms

Smut Clyde chases free radicals in a German-run lab in China

Professor Florian Stadler is a German materials scientist and nanotechnologist in China. He is very concerned with the lax research integrity attitude there. Luckily, his lab is a paradigm of good publication ethics. Oh wait. Smut Clyde wants you to meet Prof Stadler’s most productive postdoc, Dr Amit Kumar.

In September 2021, a reader reached out to me:

I have read your article concerning Chinese paper mills with great interest and a clear feeling of despise for those practices. Having been professor in China for the last 7 years, I have to say that I am not the least surprised that such a thing exists…

It was Prof. Dr. Florian Stadler, distinguished professor for materials science at Shenzhen University, who arrived there in 2014 after a previous faculty stint in Korea, postdoc stints in Japan and Belgium, and a PhD graduation at the University Erlangen-Nürnberg in Germany. Professor Stadler works in the area of polymer chemistry, nanoparticle synthesis, water purification and sensors, fields indeed polluted by papermills and other kind of research fraud.

How good to meet a decent and very concerned German researcher in a country where science fraud is so pervasive! Dr Stadler wanted to talk to me about

  • Coercive citations
  • Hijacked journals
  • Authors being asked by the referees to write the referee report for them
  • Highly unbalanced citations…”

And other abuses of peer review, authorship and publication ethics. Yet we never got to talk about that, but in June 2022 I reached out to Prof Stadler with the message that his papers were being flagged on PubPeer. It’s almost 30 publications now, and not all were penned by his postdoc Amit Kumar.

But you have to read Smut Clyde’s exposé first before you learn how Prof Stadler decided to heroically crack down on research misconduct in his own papers.


Welease Woger!

By Smut Clyde

Suppose that you have engineered an advanced nanotech material that breaks down water pollutants and purifies industrial effluent by converting the energy of sunlight into free radicals. ‘Free Radicals’ is not the Len Lye movie, nor even a 1970s demand for the liberation of political activists (not even Wodewick, the notorious wobber and wapist). Rather, as any fule kno, free radicals are incomplete molecules bearing an unpaired valence electron, and because every unpaired electron aspires to become a molecular bond, they are helpfully reactive in that purifying role.

Like atomic nuclei, unpaired electrons have ‘spin’, and like nuclei they can be persuaded to flip between -½ and +½ spin states by the right combination of microwave radiation and magnetic field, so smart people invented a method of electron spin resonance to measure their presence and sample their local quantum environments, analogous to NMR. Rather than varying the microwave frequency and looking for spikes in absorption when it aligns with the magnetic field and resonance occurs, ESR data are collected by holding frequency constant and varying the field strength, but it still seems reasonable to call the result a ‘spectrum’.

Prof Callaghan did not cover ESR in his NMR quantum-theory course some 40-odd years ago so I am only repeating what I learned from a crash course at the University of W*k*pedia. Even so I am fairly sure that the baseline, noise-dominated segments of these plots shouldn’t duplicate themselves at different scales or after vertical or horizontal flips. They should look more like ‘noise’ and less like someone trained a neural network on cursive handwriting exercises. In short, if authors are going to hand-draw their ESR plots then some more time looking at actual ESR outputs might be a good idea.

Wide spectral degradation of Norfloxacin by Ag@BiPO4/BiOBr/BiFeO3 nano-assembly: Elucidating the photocatalytic mechanism under different light sources” (Kumar et al 2019)
Construction of dual Z-scheme g-C3N4/Bi4Ti3O12/Bi4O5I2 heterojunction for visible and solar powered coupled photocatalytic antibiotic degradation and hydrogen production: Boosting via I−/I3− and Bi3+/Bi5+ redox mediators (Kumar et al 2021)

Regular visitors to PubPeer should be familiar with the Brokenspectra of fake, Frankensteinian spectra and collaged X-ray diffractograms. In contrast, fake ESR are a new outlet for artistic creativity. So far they are confined to the prodigious output of Amit Kumar and his Highly Cited Colleagues.

I know nothing about Dr Kumar, except that after four years as Assistant Professor at Shoolini University (India) he was recruited to the Stadler Laboratory (at Shenzhen University, China), which is Professor Florian Stadler‘s manor.*

He works there on various advanced-material projects, with the general paper-production strategy of “synthesise something, think of a possible application, and pretend that the application led to the synthesis” – not just the water purification side of the street.

Now I am used to scientists wanting people to read their publications. So it came as a surprise to follow the links from Dr Kumar’s academic webpage to the ResearchGate and Google Scholar link-farm records of his productivity, and find that both had recently dissolved back into the quantum flux.

http://stadler-lab.org/profile/amit-kumar/

I can only speculate that the deletions were motivated by the hope of deflecting critical attention from the vast, cool, unsympathetic intellects that contribute to PubPeer. Just taking a stab of faith here, or a leap in the dark or something like that. For Dr Kumar has attracted rather a lot of that attention, beginning with Thallarcha lechrioleuca. He boasted of his status as Highly-Cited Researcher, and to the average PubPeer contributor this is like boasting about the size and suddenness of your unexplained income in front of the Audit Department of the IRS, or like boasting to a bull about the redness of your rags.

This provides a kind of natural experiment to test the value of Highly Cited as an index of research quality. Let’s begin with X-Ray Photoelectron Spectroscopy.

XPS measures the absorption of x-rays when they have just enough energy to knock an electron out of an orbital… x-rays with too little energy don’t interact with the electron at all, but the change of interaction also falls off when the x-rays have too much energy. An XRS plot might be a big-picture survey, showing several of these electron-emission lines. Conversely, the equipment might zoom in for a high-resolution expansion of the fine structure within a single line, so the results can be fitted as a sum of contributions from components that are slightly shifted in binding energy by the chemical environment of the molecule. This is clever stuff and I am forever awed by the exquisite precision for tuning the energy of an x-ray beam. It may be that the expense of the experiments is prohibitive, so Kumar &co present the same data in multiple papers, fitted with different components or basis functions.

Quaternary magnetic BiOCl/g-C3N4/Cu2O/Fe3O4 nano-junction for visible light and solar powered degradation of sulfamethoxazole from aqueous environment (Kumar et al 2018)
Environmental Pollution Remediation via Photocatalytic Degradation of Sulfamethoxazole from Waste Water Using Sustainable Ag2S/Bi2S3/g-C3N4 Nano-Hybrids (Kumar et al 2022); and Construction of dual Z-scheme g-C3N4/Bi4Ti3O12/Bi4O5I2 heterojunction for visible and solar powered coupled photocatalytic antibiotic degradation and hydrogen production: Boosting via I−/I3− and Bi3+/Bi5+ redox mediators (Kumar et al 2021)

You might think that if the baseline separating the absorption spikes in one of these survey scans consists of repeated segments of noise, then the whole experiment never happened. I could not possibly comment.

Silicate glass matrix@Cu2O/Cu2V2O7 p-n heterojunction for enhanced visible light photo-degradation of sulfamethoxazole: High charge separation and interfacial transfer (Kumar et al 2021)
Environmental Pollution Remediation via Photocatalytic Degradation of Sulfamethoxazole from Waste Water Using Sustainable Ag2S/Bi2S3/g-C3N4 Nano-Hybrids (Kumar et al 2022)

When x-rays are not being absorbed by a material, they’re reflecting off it, assuming that they encounter a crystal at the right angle for the x-ray wavelength to match the spacing between crystal layers. This is where we come under the rubric of x-ray diffraction. Within this domain, suspicions are quickly aroused by a diffractogram where a stretch of small-angle baseline is all glitchy and stitched together from copy-paste, with a longer extended glitch in the intermediate angular range. It turns out to be g-C3N4, which is (I think) a form of altered carbon modified graphene… definitely not an amorphous material, but not entirely morphous either.

If its artificial origins were not concerning enough, the artefact appears repeatedly in the Kumar oeuvre, presumably from samples of g-C3N4 synthesised afresh for different projects.

Constructing Z-scheme LaTiO2N/g-C3N4@Fe3O4 magnetic nano heterojunctions with promoted charge separation for visible and solar removal of indomethacin (Kumar et al 2020)
Construction of dual Z-scheme g-C3N4/Bi4Ti3O12/Bi4O5I2 heterojunction for visible and solar powered coupled photocatalytic antibiotic degradation and hydrogen production: Boosting via I−/I3− and Bi3+/Bi5+ redox mediators (Kumar et al 2021)
High-Performance Photocatalytic Hydrogen Production and Degradation of Levofloxacin by Wide Spectrum-Responsive Ag/Fe3O4 Bridged SrTiO3/g-C3N4 Plasmonic Nanojunctions: Joint Effect of Ag and Fe3O4 (Kumar et al 2018)
CeO2/g-C3N4/V2O5 ternary nano hetero-structures decorated with CQDs for enhanced photo-reduction capabilities under different light sources: Dual Z-scheme mechanism (Kumar et al 2020)

Then there are modified, embellished versions, created to demonstrate the successful synthesis of more complex materials, where “synthesis” consisted of replacing parts of the fake diffractogram with epileptic spasms of tics and glitches, retaining more or less of the original, and reminding me for some reason of the more technical sequencer-driven Krautrock musicians. These exercises in collage are not limited to g-C3N4 variants.

Controlled synthesis of porous Zn/Fe based layered double hydroxides: Synthesis mechanism, and ciprofloxacin adsorption (Sharma et al 2021)

There is much more like that, but I’m bored now. Also I need to save space for some bactericidal disk assays, where the cleared roundels in a Petri dish – centred on little wells – show whether the catalyst has broken down an unwanted antibiotic, so there is none to diffuse out from a well and prevent the bacterial growth in the agar. The plates would be more convincing without the heavy-handed Photoshop, is all.

Fe3O4/ZnO/Si3N4 nanocomposite based photocatalyst for the degradation of dyes from aqueous solution (Sharma et al 2020)
Utilizing recycled LiFePO4 from batteries in combination with B@C3N4 and CuFe2O4 as sustainable nano-junctions for high performance degradation of atenolol (Kumar et al 2018)

Still with “Utilizing recycled LiFePO4 from batteries…”, Fig 7d displays a related form of fabrication, in which the absence of toxins in pollutant-laden water (after treating it with the photocatalyst) is demonstrated by exposing it to a cell-culture of peripheral blood lymphocytes. The Clone-Tool Fairy waved her magic wand over the microscope photographs.

Utilizing recycled LiFePO4 from batteries in combination with B@C3N4 and CuFe2O4 as sustainable nano-junctions for high performance degradation of atenolol (Kumar et al 2018, again)

A slightly later paper reveals a less processed version of the left-hand image:

(left) Quaternary magnetic BiOCl/g-C3N4/Cu2O/Fe3O4 nano-junction for visible light and solar powered degradation of sulfamethoxazole from aqueous environment (Kumar et al 2018)

The right-hand panel (“ATL by-products treated cells”) is particularly versatile. it became “Untreated Human PBL cells” in Fig 14c-d (where the areas of copy-paste fiddle-faddle are left as an exercise for the reader):

Biochar-templated g-C3N4/Bi2O2CO3/CoFe2O4 nano-assembly for visible and solar assisted photo-degradation of paraquat, nitrophenol reduction and CO2 conversion (Kumar et al 2018)

The ellipses are to assist comparison with these cookie-cut versions:

Visible photodegradation of ibuprofen and 2,4-D in simulated waste water using sustainable metal free-hybrids based on carbon nitride and biochar (Kumar et al 2019)

With alternative aliases, the images demonstrate how another of Kumar’s miracle materials – a “Pectin / guar-gum / zinc oxide nanocomposite”, perhaps – can stimulate the activity of lymphocytes and thereby cure cancer. Cancer-cure flim-flam is never far away.

Pectin-guar gum-zinc oxide nanocomposite enhances human lymphocytes cytotoxicity towards lung and breast carcinomas (Hira et al 2018); and Carbon quantum dots and reduced graphene oxide modified self-assembled S@C3N4/B@C3N4 metal-free nano-photocatalyst for high performance degradation of chloramphenicol (Kumar et al 2020)

Kumar’s general work paradigm seems to consist of farting around in the laboratory and sending the contents of his alembic off to the electron-microscope technicians for some imagery; then retrofitting a story about possible applications for the new material… making stuff up about its properties, with hand-drawn figures and XRD collage to fit the story. At least the SEM and TEM images appear to be genuine, but I am unconvinced that any of these syntheses could ever be replicated.

Artist’s impression of Professor Amit Kumar at work

This is all unfortunate for Prof Stadler, and if I were in his position I would be asking myself some hard questions… like “Should I have signed these papers as senior co-author?” and “Was I an effective mentor, neither negligent nor over-intrusive?” and “Is it Beer O’Clock yet?” and “What is this ‘kibosh’ and why do people keep putting it on things they don’t like?”

I want to stress that the Kumar shenanigans began while he was still Assistant-Professing at Shoolini University. They merely became more frequent in his later career, after he shifted to publishing in Elsevier journals, though I am not saying that peer-review standards are negotiable there. So despite this similarity of these two diffractograms (modulo a vertical compression), they characterise two different materials.

Polyacrylamide/Ni0.02Zn0.98O Nanocomposite with High Solar Light Photocatalytic Activity and Efficient Adsorption Capacity for Toxic Dye Removal (Kumar et al 2014) and A multifunctional nanocomposite pectin thorium(IV) tungstomolybdate for heavy metal separation and photoremediation of malachite green (Sharma et al 2016)

The malarkey is not limited to Kumar, and we find problems in papers from his broader Shoolini circle with no Kumar involvement. I feel for this electron-emission spectrum, where one element’s emission line was brutally shorn off leaving only a flat-topped stump, while another has been duplicated.

Sol–gel synthesis of polyacrylamide-stannic arsenate nanocomposite ion exchanger: binary separations and enhanced photo-catalytic activity (Ajay Kumar et al 2019)

From the same paper, some bonus x-ray diffraction, displaying more symmetry than one expects to encounter.

And here is the inevitable spreadsheet, for readers who wish to explore further.

Afterthought:

The techno nightmares of the XRD patterns reached a nadir in 2017.

Solar-driven photodegradation of 17-β-estradiol and ciprofloxacin from waste water and CO2 conversion using sustainable coal-char/polymeric-g-C3N4/RGO metal-free nano-hybrids (Kumar et al 2017)

* The sheltering aegis of a Shenzhen University affiliation extends to Dr Kumar’s Shoolini colleague, Gaurav Sharma (“highly cited researcher 2020 & 2021“). As well as faking papers, Dr Sharma’s hobbies include editing journals, reviewing for journals, counting his citations, and mentoring PhD students in How to Science.



LS again. I promised you Prof Stadler’s reaction to all this malfeasance which takes place in and with his name, so here it comes, from June 2022:

These allegations are pretty much the same that I got from RSC where somebody supplied a 115 page document accusing me of data manipulation, pretty much all focused on “too similar noise”. I don’t know who did that but somebody tries to tarnish my reputation. I checked some of the raw data (not for all) and found that my postdoc made a mistake about the x-axis. i.e. the 5 datasets in the figure did not have the same x-scaling (wavenumbers). This alone makes it extremely likely that she did not do any data manipulation, as interpolating at different x-values to yield faked y-values, would be plainly much harder than having the same x-values.

For the flagged papers, I need to go through the raw data and check them. That might take a while to get them and see whether there is a problem.”

There is so much to unpack. First of all, someone (definitely neither Smut Clyde nor Thallarcha lechrioleuca, but rather a Stadler lab member unhappy about all the research fraud) sent a 115 page report to the Royal Society for Chemistry detailing problems with cloned spectra fragments. So far, it seems RSC decided to do nothing.

Also, the RSC stuff isn’t even on PubPeer, except of this paper flagged by T. lechrioleuca, which might also hint which female postdoc Stadler is blaming while defending himself and Kumar, namely Mina Namvari:

Mina Namvari , Lei Du , Florian J. Stadler Graphene oxide-based silsesquioxane-crosslinked networks – synthesis and rheological behavior RSC Advances (2017) doi: 10.1039/c7ra02764h

Thallarcha lechrioleuca: “Fig.3 Raman spectra of GO-COOH and rGO-POSS are identical

And now a month has passed and Stadler still didn’t comment on PubPeer or replied to me, even to reminders. Maybe he found no problems.


Donate to Smut Clyde!

If you liked Smut Clyde’s work, you can leave here a small tip of 10 NZD (USD 7). Or several of small tips, just increase the amount as you like (2x=NZD 20; 5x=NZD 50). Your donation will go straight to Smut Clyde’s beer fund.

NZ$10.00

1 comment on “Epileptic spasms of tics and glitches in Krautrock diffractograms

  1. smut.clyde

    The plague of deleted ResearchGate pages continues to spread, with Gaurav Shamar’s page as the latest victim.

    Space did not permit any digressions about another of Dr Kumar’s colleagues, Mu. Naushad… a third alumnus of Shoolimi University, now ensconced at that hotbed of fraud and malfeasance, Kind Saud University, and occasionally collaborating with Stadler Lab. Shoolimi is evidently a private university, setting its own curriculum and standards, and we can only speculate about what they teach there.

    We learn from his Loop page that Dr Naushad has co-authored 350 papers, of which only a fraction have turned up on Pubpeer so far: https://pubpeer.com/search?q=mu+naushad.

    The capital-letters title “HIGHLY CITED RESEARCHER” turns up so often in his web presence that I am open to the possibility that it is not a boast but actually part of Dr Naushad’s name, bestowed upon him by pround parents with high expectations.

    Like

Leave a Reply

Fill in your details below or click an icon to log in:

WordPress.com Logo

You are commenting using your WordPress.com account. Log Out /  Change )

Twitter picture

You are commenting using your Twitter account. Log Out /  Change )

Facebook photo

You are commenting using your Facebook account. Log Out /  Change )

Connecting to %s

%d bloggers like this: