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REVIEW 4 major objections 5 minor 15 references

Quantifying sulfur speciation in magmatic-hydrothermal fluids

T0 review · 4 major / 5 minor · reviewed 2026-08-07 · deepseek-v4-flash

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Pith's one-line read A reply to a recent geoscience report argues that the claimed dominance of hydrosulfide in magmatic fluids stems from a misassigned Raman band and inconsistent thermodynamic data, leaving the published properties of hydrosulfide and the…

desk verdict A pointed, partly circular comment that exposes a real contradiction in F&Z's model but leans on an extrapolated Raman reassignment. read the letter →

arxiv 2506.08598 v1 pith:2NGDLVO6 submitted 2025-06-10 physics.geo-ph physics.chem-ph

Gleb S. Pokrovski (GET) This is my paper
classification physics.geo-phphysics.chem-ph
keywords sulfurspeciationmagmatic-hydrothermalfluidsRamanspectroscopytrisulfurradicalionhydrosulfidefluidinclusionsthermodynamicmodelingporphyryoredeposits
verification ladder T0 review T1 audit T2 compute T3 formal

The pith

A machine-rendered reading of the paper's core claim, the machinery that carries it, and where it could break.

The reading

This paper is a comment on a recent study that used Raman spectroscopy on synthetic quartz-hosted fluid inclusions to report that hydrosulfide ($HS^-$) and dissolved $SO_2$, not trisulfur radical ions, dominate sulfur in hot magmatic fluids. The comment claims that the study's conclusions collapse under re-examination: its own model actually predicts negligible $HS^-$ and abundant $[S_3^\bullet]^-$, contradicting its Raman interpretation, and the 2570 cm$^{-1}$ band assigned to $HS^-$ is more plausibly an intrinsic asymmetric feature of the $H_2S$ stretching band. After correcting the model for inconsistent thermodynamic reference data, omitted alkali ion pairs, and the experimentally known $H_2S/SO_2$ redox transition, the predicted $[S_3^\bullet]^-$ abundance falls below the detection limit of non-resonant Raman. The matter matters because sulfur speciation sets how sulfur and gold partition into ore-forming fluids in the Earth's crust.

What carries the argument

The argument is carried by three equilibria and one spectroscopic line-shape observation. Reaction (1), $H_2S(aq) = HS^- + H^+$, is the acid dissociation constant $K_1$; the recent study's $HS^-/H_2S$ ratios imply a shift of at least eight orders of magnitude in $K_1$, a red flag that the band assignment, not the constant, is wrong. Reaction (2), $2H_2S + SO_4^{2-} + H^+ = [S_3^\bullet]^- + 0.75O_2(g) + 2.5H_2O$, is the formal equilibrium from which the trisulfur ion's thermodynamic properties were originally derived, and the author shows the criticized model perturbs it by using a different $H_2S(aq)$ Gibbs-energy source and by omitting alkali ion pairs. Reaction (3), $H_2S + 1.5O_2 = SO_2 + H_2O$, fixes the $H_2S/SO_2$ redox transition, which the criticized model places about two log units of fugacity too high. On the spectral side, the key object is the intrinsic asymmetry of the $H_2S$ $\nu_1$ Raman band, produced by hot bands in the gas-like high-temperature fluid and by hydrogen-bond dynamics in solution; its low-wavenumber shoulder sits almost exactly where a true $HS^-$ stretch would appear.

What would settle it

Measure Raman spectra of $H_2S$-bearing aqueous solutions at 875 °C and 2 kbar as pH is stepped across the $H_2S/HS^-$ pKa window while total sulfur is held fixed; if the 2570 cm$^{-1}$ feature grows with $HS^-$ abundance rather than remaining proportional to $H_2S$ concentration, the central spectral reassignment is wrong.

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Extended reading notes

Core claim

The core claim is that none of the recent study's observations justifies overturning the published thermodynamic properties of $HS^-$, $H_2S$, and $[S_3^\bullet]^-$. The author reproduces the study's speciation calculations and notes that they produce an internally contradictory picture: the thermochemical model returns almost no $HS^-$ and up to mole fraction 0.1 of $[S_3^\bullet]^-$, while the Raman spectra were interpreted with the opposite ordering. Reproducing the reported $HS^-/H_2S$ ratio of about two would require increasing the $H_2S$ acid dissociation constant by at least eight orders of magnitude, which is chemically implausible and would, by charge balance, force the unphysical dominance of the gold cation $Au^+$ in solution. The alleged $HS^-$ Raman band near 2570 cm$^{-1}$ is instead explained as the asymmetric $\nu_1$ band of $H_2S$, broadened by hot bands and hydrogen-bond dynamics. Applied consistently with the thermodynamic framework from which the trisulfur radical ion properties were derived, the same data give $[S_3^\bullet]^-$ mole fractions of at most 0.0004, consistent with its absence from the non-resonant Raman spectra.

Load-bearing premise

The load-bearing assumption is that the 2570 cm$^{-1}$ feature in the criticized experiments is an intrinsic asymmetric band of $H_2S(aq)$ rather than a genuine $HS^-$ vibration, an assignment extrapolated to 875 °C and 2 kbar from lower-temperature and gas-phase spectra.

Editorial extensions

If this is right

  • The recent study's conclusion that $HS^-$ outnumbers $H_2S$ in arc magmatic fluids is not supported once the 2570 cm$^{-1}$ band is read as an $H_2S$ feature.
  • At the study's own experimental conditions, the corrected thermodynamic model places $[S_3^\bullet]^-$ mole fractions at 0.0004 or less, so its non-detection by non-resonant Raman is expected rather than anomalous.
  • Published thermodynamic properties of $HS^-$, $H_2S(aq)$, and $[S_3^\bullet]^-$ and their metal complexes remain the working basis for modeling sulfur and gold transport.
  • A hydrosulfide-dominated fluid of the kind claimed would impose a charge balance that makes $Au^+$ dominant, an unphysical result for gold speciation in these fluids.
  • In natural fluids that gain cations by reacting with granitic rocks, the corrected model still yields $[S_3^\bullet]^-$ mole fractions near 0.1 during cooling, so the trisulfur radical ion remains relevant to porphyry ore formation.

Reading between the lines

Editorial extensions of the paper, not claims the author makes directly.

  • If the asymmetry argument generalizes, other high-temperature Raman identifications of $HS^-$ as a single 2570 cm$^{-1}$ peak should be re-checked, especially in dense aqueous fluids.
  • The thermodynamic cross-check demonstrated here—testing whether a proposed speciation model stays within the same $H_2S(aq)$ reference-data family as the radical-ion equilibrium—could be applied to future studies of trace sulfur species.
  • A direct experimental test suggested by the paper's logic would be to vary the cation-anion balance in synthetic inclusions at 875 °C and 2 kbar; the corrected model predicts that $[S_3^\bullet]^-$ becomes significant only when extra alkali or alkaline-earth cations are available.
  • The paper does not itself supply new measurements of $[S_3^\bullet]^-$ at magmatic conditions, so the rebuttal is only as strong as the correctness of its spectral reassignment and its chosen thermodynamic reference data.
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Editorial analysis

A structured set of objections, weighed in public.

Desk editor's note, referee report, and a circularity audit.

Referee Report

4 major / 5 minor

Summary. This manuscript is a comment arising on Farsang and Zajacz (Nature Geoscience, 2025), in which Pokrovski challenges their Raman-based sulfur speciation in magmatic-hydrothermal fluids and their conclusion that published thermodynamic data for HS- and [S3•]- are incorrect. The author reproduces the original thermochemical model, showing that at F&Z's conditions it yields negligible HS- and abundant [S3•]-—opposite to F&Z's interpretation. He attributes the 2570 cm-1 Raman band to the asymmetric H2S ν1 feature rather than HS-, applies three corrections (dissociation constant K1, trisulfur equilibrium K2, and H2S/SO2 equilibrium K3) to bring the model into consistency with experiment, and concludes that F&Z provide no grounds to question the existing thermodynamic data. The manuscript includes one main figure, supplementary figures, and a numerical data file.

Significance. If fully valid, the comment would re-establish the Pokrovski-Dubessy thermodynamic framework for [S3•]- and HS- and would identify an internal inconsistency in F&Z's modeling versus their spectroscopic interpretation. The manuscript's strengths are that the model reproduction is explicit, the internal contradiction is sharply demonstrated, and the quantitative corrections are individually sourced. The main weaknesses are that the Raman reassignment is extrapolated to conditions beyond its empirical calibration and that the preferred model partly relies on the very thermodynamic properties under dispute; hence the categorical conclusion exceeds what the evidence currently supports.

major comments (4)
  1. [Fig. S2 and main text (2570 cm-1 band)] The attribution of the 2570 cm-1 band to the asymmetric H2S ν1 feature, rather than HS-, is the load-bearing empirical step in the comment, but it is justified by gas-phase spectra and aqueous spectra up to about 500°C, whereas F&Z's measurements were made at 875°C, 2 kbar in dense NaCl-bearing supercritical fluids. At these conditions the H2S band shape, width, and temperature dependence are not directly calibrated, and the high water density and salt content may alter the hydrogen-bond dynamics on which the asymmetry argument rests. If a real HS- contribution exists at 875°C and 2 kbar, then the thermodynamic inconsistency alone does not refute F&Z's spectroscopic detection. Please provide direct evidence at or near the experimental conditions, or explicitly restrict the conclusion to the calibrated range.
  2. [Fig. 1c] The preferred model in Fig. 1c uses the [S3•]- thermodynamic properties from Pokrovski and Dubessy (2015) to show that [S3•]- should be undetectable in F&Z's experiments. Because the validity of those properties is the very point contested by F&Z, this particular model-based prediction is circular if used as independent evidence. The internal-inconsistency argument and the use of F&Z's own H2S/SO2 transition are independent, but the categorical conclusion that F&Z provide no grounds to question the thermodynamic data should not rest on Fig. 1c alone. Please separate the circular from the non-circular strands and state what survives if the disputed [S3•]- data are set aside.
  3. [Paragraph 2 (constant HS-/H2S ratio)] The argument that a constant HS-/H2S ratio over the fO2 range NNO-0.9 to NNO+2.6 cannot be matched with a single K1 value is not self-evident: for two S(-2) species, the ratio [HS-]/[H2S] is controlled by pH and K1 and is not directly a function of fO2, so a constant ratio could reflect pH buffering rather than an inconsistent model. Please provide the pH or buffering assumptions used in the calculation, or drop this argument from the list of inconsistencies.
  4. [Conclusions (last two paragraphs)] The statements that reaction (1) is 'generally insignificant at shallow-crust magmatic contexts' and that F&Z's compositions 'cannot be used to infer its abundance in nature' go beyond what the calculations show. The calculations are for a specific NaCl-dominated fluid at 875°C and 2 kbar, and the author's own Fig. 2 demonstrates that fluid-rock interaction can change sulfur speciation dramatically at lower temperatures. Please soften these categorical conclusions or support them with calculations spanning the compositional and P-T range of shallow-crust magmatic systems.
minor comments (5)
  1. [References] The second entry in the reference list is numbered 3 (Pokrovski and Dubrovinsky) and the following entry is also numbered 3 (Pokrovski and Dubessy); renumber sequentially throughout.
  2. [Fig. 1c caption] The H2S(aq) thermodynamic properties are said to come from ref. 9, but the text and the reference list identify refs. 11 and 12 as the H2S sources; correct this citation.
  3. [Main text, third paragraph] The phrase '250(!) times smaller' is informal for a journal report; replace with 'a factor of 250 smaller'.
  4. [Main text, last paragraph] The statement that 'the signal arising from the HSO4- moiety was not detected' and the inferred detection limit of ~0.01 mole fraction should be justified with a quantitative detection-limit estimate, not an extrapolation from a single non-detection.
  5. [Fig. 2 caption] The notation 'Σ stands for the sum of sulfate, hydrosulfate and hydrosulfide forms' should list explicitly which species are summed, including ion pairs, to avoid ambiguity.

Circularity Check

2 steps flagged · score 4.0 of 10

Self-citation is load-bearing in the [S3•]− rebuttal, but the Raman reassignment and internal-consistency arguments give the central critique independent content.

  1. self citation load bearing [Main text, Fig. 1 caption (model c)]
    "A model consistent with i) thermodynamic framework within which the [S3•]− parameters have been derived in ref. 3, with H2S(aq) thermodynamic properties from ref.9, and including those of Na ion pairs (NaHSO40, NaSO4– and NaHS0) from ref.3; and ii) the experimental fO2 value of NNO+0.3 for the H2S/SO2 transition1 as per the reaction (3) equilibrium constant1 (equivalent to a correction of –50 kJ/mol for SO2(aq) Gibbs energy value of ref.9)."

    The model used to declare [S3•]− undetectable is constructed from the thermodynamic framework of the author's own 2015 paper (ref. 3), i.e., the very [S3•]− data whose validity Farsang and Zajacz disputed. The closing statement that the result is 'in perfect agreement with its thermodynamic properties reported by Pokrovski and Dubessy' is therefore agreement with the model's own input, not an independent confirmation. This makes the central vindication of the disputed [S3•]− thermodynamic data partly self-referential.

  2. self citation load bearing [Main text, paragraph beginning 'The related critical issue in ref.1 is about the significance of the [S3•]− ion...']
    "These independent data are all in mutual agreement, confirming the K2 value validity across the whole T-P range covered (25–500 °C, 1 bar–15 kbar), with no evidence of potential artefacts related to Raman signal absorption in coloured solutions10."

    The 'independent data' that 'confirm' K2 are the author's own prior Raman and UV-Vis studies (refs 2, 3, 9, with the thermodynamic derivation in ref. 3). Since the comment's purpose is to defend the validity of those same [S3•]− properties against Farsang and Zajacz's rebuttal, this confirmation is a self-citation chain rather than an external check. The methodological details mitigate the circularity, but the load-bearing validity claim reduces substantially to the author's prior work.

full rationale

The comment is not wholly circular: it offers independent content in (i) the internal inconsistency between F&Z's reported HS−/H2S ratios and their own adopted thermochemical model, (ii) the experimental fO2 constraint on the H2S/SO2 transition and the HSO4− non-detection argument, and (iii) the Raman reassignment of the 2570 cm−1 band using published H2S hot-band spectra and HSO4− asymmetry analogies. However, the paper's affirmative defense of the disputed [S3•]− data relies on its own 2011/2015 work as both input and confirmation: Fig. 1c constructs the 'corrected' speciation from the Pokrovski-Dubessy framework and then reports agreement with Pokrovski-Dubessy properties. This is a load-bearing self-citation, though not a strict tautology because the calculation also incorporates the experimental fO2 constraint and independent Raman/gas-phase evidence. Score 4: some self-citation with independent content in the central claim.

Assumptions & free parameters 3 free parameters · 4 assumptions · 0 invented entities

The central model depends on three hand-applied corrections and on the author's own S3- thermodynamic framework; no new entities are introduced.

free parameters (3)
  • K2 correction (trisulfur ion equilibrium constant) = -2.3 log units
    Applied to convert the S3- equilibrium constant to the H2S(aq) dataset of Schulte et al. (ref. 11) used in the author's own framework; this correction strongly lowers predicted S3- in Fig. 1c.
  • K3 correction (H2S/SO2 equilibrium constant) = +2 log units
    Applied so that the calculated H2S/SO2 transition matches the experimentally inferred fO2 of NNO+0.3 reported by Farsang and Zajacz; it shifts redox boundaries and lowers S3-.
  • K1 shift (H2S dissociation, hypothetical) = +8 log units
    Used only in Fig. 1b to show that matching the reported HS-/H2S ratio would require an implausibly large dissociation constant; not part of the author's preferred model.
assumptions (4)
  • domain assumption The thermodynamic properties of S3- from Pokrovski and Dubessy (2015) are correct.
    The predicted undetectability of S3- in Fig. 1c is computed within this framework; the comment assumes its validity while disputing Farsang and Zajacz's challenge to it. Invoked in the Fig. 1c caption and the paragraph on 'the [S3•]- thermodynamic framework3'.
  • domain assumption The H2S(aq) thermodynamic data of Schulte et al. (2001) are more reliable than those of Akinfiev and Diamond (2003) at magmatic temperatures.
    The -2.3 log unit correction to K2 depends on preferring ref. 11 over ref. 12; the paper notes the difference but does not independently justify the choice at 875 degrees Celsius.
  • domain assumption The 2570 cm-1 Raman feature in Farsang and Zajacz is an asymmetric H2S band, not HS-.
    This central reinterpretation is based on spectral analogies from gas-phase and lower-temperature aqueous measurements; no direct spectrum at the exact conditions of ref. 1 is shown.
  • standard math Standard thermodynamic relations (reaction quotients, charge balance) apply to the synthetic fluid inclusion compositions.
    Used throughout to translate Raman ratios into equilibrium constant shifts, and to argue that abundant HS- would force Au+ dominance.

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Cite this review

Pith. "Pith review of Quantifying sulfur speciation in magmatic-hydrothermal fluids." pith.science (2026). https://pith.science/paper/2NGDLVO6

@misc{pith2026250608598,
  author       = {Pith},
  title        = {Pith review of: Quantifying sulfur speciation in magmatic-hydrothermal fluids},
  year         = {2026},
  howpublished = {\url{https://pith.science/paper/2NGDLVO6}},
  note         = {Machine review of arXiv:2506.08598}
}
abstract

Quantitative knowledge of sulfur speciation in the fluid phase is key to understanding sulfur degassing from magmas and its transfer along with metals by fluids across the lithosphere. Farsang and Zajacz (1) recently reported new sulfur speciation data using Raman spectroscopy measurements on aqueous H$_2$SO$_4$-NaCl(-KCl) solutions trapped as synthetic fluid inclusions in quartz at 875$^\circ$C and 2 kbar under variable redox conditions. They interpreted the data by dominant SO$_{2(aq)}$ and HS$^-$, along with subordinate H$_2$S$_{(aq)}$, whereas the di-and trisulfur radical ions, $[S_3^\bullet]^-$ and $[S_2^\bullet]^-$, reported in aqueous fluids both in nature and experiment to at least 700 $^\circ$C and 15 kbar (2-5) , were undetectable in Raman nonresonant spectra 1 . On the basis of thermochemical calculations that returned negligible HS$^-$ and large $[S_3^\bullet]^-$ concentrations at their experimental conditions, the authors claimed that the published $[S_3^\bullet]^-$ and HS$^-$ thermodynamic data were incorrect and that the major species controlling both sulfur and gold transport in hydrothermal-magmatic fluids is the HS$^-$ anion. Here I demonstrate that their conclusions stem from the use of inconsistent thermodynamic data and incorrect Raman spectra assignments. Thus, ref. 1 provides no grounds for questioning the validity of the thermodynamic properties of HS$^-$ and $[S_3^\bullet]^-$ or of their metal complexes in the fluids of the Earth's crust.

Figures

Figures reproduced from arXiv: 2506.08598 by the authors.

Figure 1
Figure 1. Comparison of sulfur speciation models in the aqueous fluid phase at the conditions of Farsang and Zajacz study1 . Species concentrations are in mole fractions of total sulfur. Oxygen fugacity is relative to the nickel-nickel oxide conventional buffer (NNO), with an absolute log10fO2 value of –12.36. (a) The original model (equivalent to Fig. 2a and S4 of ref.1 ) reproduced using thermodynamic data of Table S5 in re… view at source ↗
Figure 2
Figure 2. Concentrations of sulfur species (expressed in mole fraction of total sulfur) calculated in an aqueous magmatic fluid of typical composition of ref.1 brought into equilibrium with a granitic rock. The fluid with an H2S/SO2 molal ratio of 2.6 (corresponding to the maximum of [S3 • ] − abundance in [PITH_FULL_IMAGE:figures/full_fig_p007_2.png] view at source ↗

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Works this paper leans on

15 extracted references · 15 canonical work pages

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