Characterisation of the plutonium isotopic composition of a sediment core from Palomares, Spain, by low-energy AMS and alpha-spectrometry

E. Chamizo; J.A. Sanchez-Cabeza; J.L. Mas; J. Merino; M.C. Jim\'enez-Ramos; M. Garc\'ia-Le\'on; P. Masqu\'e; R. Garc\'ia-Tenorio; S.M. Enamorado

REVIEW 3 major objections 5 minor 19 references

Characterisation of the plutonium isotopic composition of a sediment core from Palomares, Spain, by low-energy AMS and alpha-spectrometry

T0 review · 3 major / 5 minor · reviewed 2026-08-10 · deepseek-v4-flash

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Pith's one-line read Measured plutonium isotope ratios in a seafloor core off Palomares show that weapon-grade plutonium from the 1966 accident makes up about 84% of the core's plutonium activity, confirming that the land contamination reached the marine…

desk verdict A useful capability milestone and a new environmental Pu dataset, but the AMS 240Pu/239Pu accuracy lacks a direct standard check, so the qualitative finding is solid while the source-apportionment percentages carry more uncertainty than the paper lets on. read the letter →

arxiv 2501.13998 v1 pith:EBRGLC6A submitted 2025-01-23 physics.ins-det physics.ao-ph

E. Chamizo , M.C. Jiménez-Ramos , S.M. Enamorado , M. García-León , R. García-Tenorio , J.L. Mas , P. Masqué , J. Merino

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J.A. Sanchez-Cabeza

This is my paper · ORCID

classification physics.ins-detphysics.ao-ph PACS 29.30.Aj29.20.Ba89.60.Gg

keywords acceleratormassspectrometryplutoniumisotopes240Pu/239PuratioPalomaresaccidentsedimentcorealpha-spectrometryglobalfalloutsourceapportionment

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 reports the first environmental plutonium measurements made at 670 kV on a compact accelerator mass spectrometry (AMS) system, and it uses them to trace the legacy of the 1966 Palomares nuclear accident into the sea. The key observation is the $^{240}\mathrm{Pu}/^{239}\mathrm{Pu}$ atomic ratio in a 20 cm sediment core from the Aguas submarine canyon: the ratios lie below the $\sim 15\%$ expected for local global fallout, often below $11\%$, and approach the $5.8\%$ fingerprint of the weapon-grade plutonium released in the accident. A two-source mixing model between Palomares plutonium and global fallout attributes roughly $84\%$ of the core's total plutonium activity to the accident, with layer-by-layer accident fractions mostly between $40\%$ and $95\%$. Because twin aliquots measured by $\alpha$-spectrometry agree with the AMS activity concentrations across a wide range, the paper takes this as validation that the low-energy AMS technique can support environmental plutonium studies. The result is a demonstration that the land contamination did not stay on land: weapon-grade plutonium has been transported into the marine environment.

What carries the argument

The central object is the $^{240}\mathrm{Pu}/^{239}\mathrm{Pu}$ atomic ratio, a source fingerprint that is about $5.8\%$ for the Palomares weapons plutonium and about $15\%$ for local global fallout. It is measured by low-energy AMS: a compact 1 MV accelerator run at 670 kV, with $^{242}\mathrm{Pu}$ as the internal spike, plutonium injected as $\mathrm{PuO}^-$, stripped to $\mathrm{Pu}^{3+}$, and counted isotope-by-isotope in a gas ionisation detector. The second piece of machinery is the two-source mixing model, which solves each measured ratio for the accident-derived fraction of plutonium activity once the two endmember ratios are fixed. Agreement between duplicate aliquots and between AMS and $\alpha$-spectrometry on total $^{239+240}\mathrm{Pu}$ activity is the evidence that the ratios feeding that model are reliable.

What would settle it

Analyse the same core slices for $^{241}\mathrm{Pu}/^{239}\mathrm{Pu}$ (or its decay product $^{241}\mathrm{Am}$) while remeasuring $^{240}\mathrm{Pu}/^{239}\mathrm{Pu}$ by an independent mass-spectrometry method: the two-source model predicts each slice should fall on the mixing line between the $5.8\%$ Palomares endmember and the $\sim 15\%$ fallout endmember, so a slice off that line, or a ratio the independent method does not reproduce, would expose a third source or a systematic AMS bias and invalidate the $84\%$ estimate.

Watch

Extended reading notes

Core claim

The paper establishes that plutonium can be measured in environmental sediments at 670 kV on a compact AMS system, and it uses that capability to show that weapon-grade plutonium from the 1966 Palomares accident has reached the marine environment. In the URE sediment core from the Aguas submarine canyon, every measured $^{240}\mathrm{Pu}/^{239}\mathrm{Pu}$ atomic ratio falls below the $\sim 15\%$ local fallout value, most lie below $11\%$, and the lowest approach the $5.8\%$ characteristic of the Palomares weapons material. A two-source mixing model assigns $40\%$–$95\%$ of the plutonium activity in most layers, about $16\%$ in the deepest layer, and roughly $84\%$ of the total core inventory to the accident. Twin aliquots measured by $\alpha$-spectrometry agree with the AMS $^{239+240}\mathrm{Pu}$ activity concentrations over a wide range, which the authors present as validation of the AMS technique; the depth profile itself is homogenised by mixing and punctuated by probable hot particles, so it cannot support a deposition chronology.

Load-bearing premise

The apportionment rests on two linked assumptions: that every plutonium atom in the core is a mixture of only the Palomares $5.8\%$ endmember and a $\sim 15\%$ local fallout endmember, and that the AMS-measured $^{240}\mathrm{Pu}/^{239}\mathrm{Pu}$ ratios are accurate, since the $\alpha$-spectrometry comparison validates total activity concentrations but not the ratio itself.

Editorial extensions

If this is right

Environmental plutonium surveys can now be done on a compact low-energy AMS system, with $^{240}\mathrm{Pu}/^{239}\mathrm{Pu}$ ratios available at sample sizes where alpha-spectrometry can only give a combined activity concentration.
The Palomares accident's marine footprint is established: sediment accumulating in the Aguas submarine canyon carries a majority of accident-derived plutonium, so land-to-sea transport is a confirmed pathway.
Isotopic fingerprinting makes the accident traceable: any future sample from the area with a $^{240}\mathrm{Pu}/^{239}\mathrm{Pu}$ ratio below the local fallout value can be attributed partly to Palomares material, regardless of the total plutonium level.
The homogenised depth profile and hot-particle layers mean this core cannot be used to date the 1966 accident or reconstruct a fallout chronology; its value is source identification and inventory, not stratigraphy.

Reading between the lines

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

Extension: measuring $^{241}\mathrm{Pu}/^{239}\mathrm{Pu}$ in these slices would test the binary-mixing assumption directly; any sample that departs from the $5.8\%$-to-$15\%$ mixing line would uncover a third plutonium source and shift the $84\%$ estimate.
Extension: the authors identify probable hot particles but do not image them; single-particle analysis of the 2 cm and 5–6 cm layers could show whether the weapon-grade signal arrived as intact fuel fragments or as a dispersed, leached component.
Extension: the same 670 kV AMS capability could measure other actinides, such as $^{236}\mathrm{U}$, in the same aliquots, giving the land-to-sea transport story a test that does not depend on plutonium chemistry alone.
Extension: the $84\%$ figure is an inventory for this single core; converting it into a regional statement about how much Palomares plutonium now resides on the Mediterranean shelf would require additional cores and a sediment budget.

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Editorial analysis

A structured set of objections, weighed in public.

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

Desk Editor's Note

read the letter

Quick take: this is a competent applied paper with a genuine new dataset and a useful capability milestone. The first environmental Pu AMS results from CNA's 1 MV system are a real step, and the depth-resolved 240Pu/239Pu profile for a Palomares marine core is new. The AS-AMS agreement for total 239+240Pu activity (slope 0.984±0.034, r2=0.98) is solid and properly validated. I give credit where it is earned: the radiochemistry is careful, the mixing model is standard, and the hot-particle heterogeneity in the duplicate aliquots is acknowledged rather than hidden.

The qualitative conclusion, that weapon-grade Pu from the 1966 accident reached the marine environment, is well supported by the consistently low ratios (6.2–13.2%) and is consistent with earlier alpha-spectrometry work on coastal samples. I would not want to argue the accident signal is absent.

Where the paper is soft: there is no certified reference material with independently known 240Pu/239Pu reported for the AMS measurements. The alpha-spectrometry comparison only validates gross activity; it is blind to a possible mass-dependent transmission bias in the AMS system. That is a genuine gap. In practice, a 15% fallout ratio would need to be depressed by a third to mimic the core's top-layer values, which would be a large bias, but the paper gives no direct evidence of accuracy. The Pwg percentages inherit this uncertainty as well as uncertainty in the fallout endmember, which is extrapolated from Seville soils rather than measured locally. These are concrete, addressable limitations, not fatal flaws.

If this is going to peer review, I would send it out and ask the authors to add a reference ratio measurement (e.g., NIST SRM 947 or IRMM-085), ideally a cross-check by ICP-MS on a subset of samples, and a sensitivity analysis on the fallout endmember. The dataset is worth having, and the methodological lessons are directly useful to the AMS community.

Referee Report

3 major / 5 minor

Summary. The paper reports the first plutonium AMS measurements made on the 1 MV compact AMS system at the Centro Nacional de Aceleradores (CNA) using a 670 kV terminal voltage, applied to a 20 cm sediment core (URE) from the Aguas submarine canyon near Palomares, Spain. The authors measure 239+240Pu activity concentrations by both AMS and alpha-spectrometry on twin aliquots and find good agreement (slope 0.984±0.034, r²=0.9828), which they use to validate the AMS technique for total plutonium. The central scientific claim is that the measured 240Pu/239Pu atomic ratios, which average below 11%, are significantly lower than the ~15% expected for global fallout in the region, and thus confirm the presence of weapon-grade plutonium released during the 1966 Palomares accident. Using a two-source mixing model with a 5.8% weapon-grade endmember and a ~15% fallout endmember, the authors estimate that 40-95% of the plutonium in individual core sections, and about 84% of the total core inventory, originates from the accident. The deepest layer (URE-17) is an exception, with a ratio of 13.2±1.1% that yields only a 15.7% accident contribution.

Significance. If the reported isotope ratios are accurate, this is a valuable confirmation that weapon-grade plutonium from the 1966 Palomares accident has been transported to the marine environment, and it demonstrates the feasibility of low-energy AMS for plutonium isotope ratio measurements at environmental levels. The alpha-spectrometry comparison is a genuine independent check for total 239+240Pu activity, and the wide dynamic range of the agreement is a concrete strength. However, the central conclusion rests on the accuracy of the AMS 240Pu/239Pu ratios, and the paper provides no validation of this ratio accuracy against a certified reference material or a second mass-spectrometric technique. The quantitative source apportionment also depends on an extrapolated fallout endmember. These issues are addressable and do not invalidate the qualitative detection, but they must be resolved before the claims as stated can be accepted.

major comments (3)

[§2 (AMS method) and §3 (Table 1, Fig. 2)] The validation of the AMS technique is based entirely on the comparison with alpha-spectrometry for total 239+240Pu activity (Fig. 2). This comparison is, as the authors state, a check of chemical yield and gross activity, but it is blind to the 240Pu/239Pu ratio that drives the central conclusion. No measurement of a certified reference material with independently known 240Pu/239Pu ratio (e.g., NIST SRM 947 or IRMM-085) is reported, nor is any cross-check against ICP-MS or another mass-spectrometry method. The stated 2% instrumental precision is a measure of repeatability, not accuracy, and does not constrain a possible mass-dependent bias in the sequential-injection, stripping, or detector energy-window stages of the 670 kV AMS system. Such a bias could shift all measured ratios systematically low and produce the same pattern as the presence of weapon-grade plutonium. I request that the authors report the results of a certified reference material measurement or a direct method intercomparison on at least a subset of samples, and temper the claim of definitive applicability accordingly.
[§3 (two-source mixing model, Table 1)] The Pwg percentages are computed from a two-source mixing model referenced to [9], but the equation is not given in the paper, so the reader cannot reproduce the values or propagate the endmember uncertainties. The assumed endmembers are 5.8% for Palomares weapon-grade plutonium (Ref. [1]) and about 15% for local global fallout, the latter extrapolated from Seville soils [11]. Neither endmember is measured in this sediment core. The qualitative conclusion that the core contains non-fallout plutonium is robust because most measured ratios (6-10%) are far below any reasonable fallout value, but the quantitative claim that the accident contributes 40-95% of the activity in individual layers and 84% of the total core inventory is directly conditional on these endmembers. Please state the mixing formula explicitly and provide a sensitivity analysis (e.g., Pwg for fallout ratios of 13% and 18%), or soften the quantitative claims accordingly.
[§3 (Table 1, Fig. 3; URE-17)] The statement that 'in all samples this ratio is lower than that expected for fallout plutonium' is not well supported by the deepest sample URE-17, whose measured ratio is 13.2 ± 1.1%. This is within about 1.6σ of the assumed local fallout value of 15%, so the deepest layer does not, by itself, provide significant evidence of a non-fallout source. The aggregate claim, 'on average levels lower than 11%', is supported by the data, but the whole-core claim should be qualified to acknowledge that the lowermost section is statistically compatible with fallout.

minor comments (5)

[§1 (Introduction)] Line 3 of the Introduction: 'another are of investigation' should be 'another area of investigation'. The sentence beginning 'The first Pu AMS results on Palomares samples were obtained in 2006' would be clearer as 'The first Pu AMS results for Palomares samples were obtained in 2006'.
[Table 1] Table 1 does not include rows for some core slices (URE-11 and URE-16, corresponding to approximately 10.5-11.5 cm and 16.5-17.5 cm depth intervals), and the text does not explain why these samples are missing. Please indicate whether these sections were not measured, lost, or omitted for another reason.
[Abstract and §2] The abstract's phrase 'first Pu AMS results for environmental samples' could be misread as the first such results worldwide; clarify that they are the first from the CNA 1 MV AMS system, as stated in the Introduction.
[Fig. 2] The regression line in Fig. 2 is reported with slope and intercept, but no confidence bands for the fit are shown. Adding them would make the validation plot more informative.
[Table 1 notes] The entries marked with * for 238Pu/(239+240)Pu are said to be unmeasurable due to traces of 228Th [14]; a brief sentence explaining the interference would help the reader understand the otherwise unexplained missing entries.

Circularity Check

0 steps flagged · score 1.0 of 10

No significant circularity. The measured 240Pu/239Pu ratios are new data, not fitted to the conclusions; the AS cross-check and two-source model are independent, and the only self-citation (local fallout estimate from Ref [11]) is not load-bearing for the central qualitative claim.

full rationale

The paper's central inference that weapon-grade plutonium from the 1966 accident reached the marine environment rests on the measured 240Pu/239Pu atomic ratios in Table 1 and Fig. 3, which are independent observations, not quantities defined by the accident ratio or by the mixing model. The accident endmember (5.8%) and Northern-Hemisphere fallout value (~18%) come from external references [1] and [9]; the local fallout estimate (~15%) is extrapolated from the authors' earlier soil study [11], a self-citation, but it is an empirical input rather than a fitted parameter, and the qualitative conclusion (ratios below 11%, i.e., below fallout) would survive even if [11] were disregarded. The alpha-spectrometry comparison in Fig. 2 is an independent cross-check of total 239+240Pu activity, not of the isotope ratio; the lack of a certified ratio standard or a second mass-spectrometric method is a genuine accuracy/calibration limitation, but it does not make the derivation circular, because the ratio measurements are not constructed from their own conclusion. The two-source mixing model of Ref [9] is an external standard method; the reported Pwg percentages are functions of the measured ratios and stated endmembers, with no parameter fitted to the same data that is then presented as a prediction. No equation or argument reduces to its inputs by construction, so no circular step can be exhibited.

Assumptions & free parameters 2 free parameters · 3 assumptions · 0 invented entities

No parameters were fitted to the data in this paper. The mixing model takes two endmember ratios from prior literature (Ref [1] and Ref [11]) that the reader must accept as inputs, and the AMS isotope-ratio accuracy is assumed because the alpha-spectrometry validation only covers total activity. These assumptions, together with the two-source model, carry the central source-apportionment claim.

free parameters (2)

Palomares weapon-grade 240Pu/239Pu ratio = 0.058 (5.8%)
Used as one endmember in the two-source mixing model to compute Pwg percentages. Taken from Ref [1] and assumed constant for all samples, not measured in this study.
Local global fallout 240Pu/239Pu ratio = ~0.15 (~15%)
Used as the other endmember in the mixing model. Extrapolated from Seville soil measurements in Ref [11], not measured in the core; Pwg values are sensitive to this choice.

assumptions (3)

domain assumption The sediment plutonium is a binary mixture of Palomares weapon-grade plutonium and global fallout.
Invoked in Section 3 to compute Pwg from the two-source mixing model of Ref [9]; no test for additional sources such as Chernobyl or Saharan dust is presented.
domain assumption The 240Pu/239Pu ratio of Palomares weapon-grade plutonium is 5.8% and the local fallout ratio is about 15%.
Endmember values are taken from Ref [1] and extrapolated from Ref [11]; they are not measured in the core and their uncertainties are not propagated.
domain assumption The CNA AMS produces unbiased 240Pu/239Pu ratios at environmental levels.
The alpha-spectrometry comparison validates total 239+240Pu activity, not the isotope ratio used for source identification; accuracy of the ratio is assumed from the instrument's prior characterization.

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Cite this review

Pith. "Pith review of Characterisation of the plutonium isotopic composition of a sediment core from Palomares, Spain, by low-energy AMS and alpha-spectrometry." pith.science (2026). https://pith.science/paper/EBRGLC6A

@misc{pith2026250113998,
  author       = {Pith},
  title        = {Pith review of: Characterisation of the plutonium isotopic composition of a sediment core from Palomares, Spain, by low-energy AMS and alpha-spectrometry},
  year         = {2026},
  howpublished = {\url{https://pith.science/paper/EBRGLC6A}},
  note         = {Machine review of arXiv:2501.13998}
}

read the original abstract

The measurement of plutonium isotopes, 239Pu and 240Pu, at 670 kV on the compact accelerator mass spectrometry (AMS) system at the Centro Nacional de Aceleradores (CNA) in Seville, Spain, is now a reality. In this work, we present first Pu AMS results for environmental samples: a sediment core collected in a submarine canyon in the Mediterranean coast of the Spanish region of Palomares, affected by a nuclear accident in 1966. From the study of the 240Pu/239Pu atomic ratio profile, showing on average levels lower than 11%, we confirm that the weapon-grade plutonium released on land during the accident, with a characteristic 240Pu/239Pu atomic ratio of 5.8%, has found its way into the marine environment. A two-plutonium sources mixture model (Palomares and fallout) is used to elucidate the percentage of the plutonium coming from the accident. As a validation exercise of the Pu AMS measuring technique and in order to obtain the 238Pu/(239+240)Pu activity ratios, samples were also studied by alpha-spectrometry (AS). The obtained AS 239+240Pu activity concentration results fit in with the AMS ones in a wide dynamic range, thus validating the AMS technique.

Figures

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Works this paper leans on

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Pith tools

Reviewed August 10, 2026 · model on record in the stance chip above.

[1] [9]

Krey, E.P

P.W. Krey, E.P. Hardy, C. Pachucki, F. Rourke, J. Coluzza, W.K. Benson, IAEA - SM-199/39 (1976) 671

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A. Espinosa, “ Comportamiento ambiental de las partículas de combustible nuclear (fundamentalmente Pu) tras un accidente nuclear en un ecosistema de tipo mediterráneo”, PhD Dissertation, University of Extremadura, 2002

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Chamizo, M

E. Chamizo, M. García -León, H.-A. Synal, M. Suter, L. Wacker, Nucl. Instr. and Meth. B, 249 (2006) 768

work page 2006

[4] [2]

Jiménez-Ramos, R

M.C. Jiménez-Ramos, R. García -Tenorio, I. Vioque, G. Manjón, M. García -León, Environmental Pollution, 142 (2006) 487

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García López, M.C

J. García López, M.C. Jiménez-Ramos, M. García -León, R. García -Tenorio, Nucl. Instr. and Meth. B, 260 (2007) 343. 8

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Manjón, M

G. Manjón, M. García -León, S. Ballestra, J.J. López, J. Environ. Radioactivity, 28 (1995) 171

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