Supergene phases from ferruginous duricrusts: non-destructive microsampling and mineralogy prior to (U–Th) ∕ He geochronological analysis

<p>Interpreting the ages of supergene mineralogical phases in laterite is complex because they consist of polycrystalline mixtures of different phases at the microscopic scale that could be crystalized at different epochs. Among the geochronometers, the <span class="inline-formula"...

Full description

Bibliographic Details
Main Authors: K. P. P. Marques, T. Allard, C. Gautheron, B. Baptiste, R. Pinna-Jamme, G. Morin, L. Delbes, P. Vidal-Torrado
Format: Article
Language:English
Published: Copernicus Publications 2023-06-01
Series:European Journal of Mineralogy
Online Access:https://ejm.copernicus.org/articles/35/383/2023/ejm-35-383-2023.pdf
_version_ 1797804315710062592
author K. P. P. Marques
K. P. P. Marques
T. Allard
C. Gautheron
B. Baptiste
R. Pinna-Jamme
G. Morin
L. Delbes
P. Vidal-Torrado
author_facet K. P. P. Marques
K. P. P. Marques
T. Allard
C. Gautheron
B. Baptiste
R. Pinna-Jamme
G. Morin
L. Delbes
P. Vidal-Torrado
author_sort K. P. P. Marques
collection DOAJ
description <p>Interpreting the ages of supergene mineralogical phases in laterite is complex because they consist of polycrystalline mixtures of different phases at the microscopic scale that could be crystalized at different epochs. Among the geochronometers, the <span class="inline-formula"><math xmlns="http://www.w3.org/1998/Math/MathML" id="M2" display="inline" overflow="scroll" dspmath="mathml"><mrow class="chem"><mo>(</mo><mi mathvariant="normal">U</mi><mo>-</mo><mi mathvariant="normal">Th</mi><mo>)</mo><mo>/</mo><mi mathvariant="normal">He</mi></mrow></math><span><svg:svg xmlns:svg="http://www.w3.org/2000/svg" width="58pt" height="14pt" class="svg-formula" dspmath="mathimg" md5hash="f4b2fa0b999292f48cb1b1e04a07aa2a"><svg:image xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="ejm-35-383-2023-ie00003.svg" width="58pt" height="14pt" src="ejm-35-383-2023-ie00003.png"/></svg:svg></span></span> method on hematite and goethite is more often used, but ages can be difficult to interpret due to phases mixing. To resolve this issue, this study proposes a methodology for performing detailed mineralogical analysis of hematite and goethite single grains prior to their dating using the <span class="inline-formula"><math xmlns="http://www.w3.org/1998/Math/MathML" id="M3" display="inline" overflow="scroll" dspmath="mathml"><mrow class="chem"><mo>(</mo><mi mathvariant="normal">U</mi><mo>-</mo><mi mathvariant="normal">Th</mi><mo>)</mo><mo>/</mo><mi mathvariant="normal">He</mi></mrow></math><span><svg:svg xmlns:svg="http://www.w3.org/2000/svg" width="58pt" height="14pt" class="svg-formula" dspmath="mathimg" md5hash="26d53101b6c836ab0b6ef325d9bca65f"><svg:image xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="ejm-35-383-2023-ie00004.svg" width="58pt" height="14pt" src="ejm-35-383-2023-ie00004.png"/></svg:svg></span></span> method. Strictly non-destructive mineralogy of single grains is not achievable by classical tools, such as conventional powder XRD (X-ray diffraction; requiring at least some milligrams of powder) or SEM (scanning electron microscopy; that can contaminate the grain by coating or fixing). Therefore, we performed X-ray diffraction patterns of single grains using high-flux X-ray beams from both a rotating anode (XRD_rotat) laboratory diffractometer and a synchrotron beamline (XRD_synch) and compared the results in order to design a method based on XRD_rotat only. For this purpose, two samples from the pisolitic facies of a Brazilian ferruginous duricrust (Alto Paranaíba region, Minas Gerais State, Brazil) were chosen because they presented a usual heterogeneity. Rietveld refinements of the XRD patterns obtained from both XRD_rotat and XRD_synch yielded similar results for the weight percentage ratio of the main phases and mean coherent domain sizes and less similar results for Al substitution rates, thus validating the XRD_rotat approach. No beam damage was observed when increasing X-ray exposure time, neither on XRD patterns nor on <span class="inline-formula"><math xmlns="http://www.w3.org/1998/Math/MathML" id="M4" display="inline" overflow="scroll" dspmath="mathml"><mrow class="chem"><mo>(</mo><mi mathvariant="normal">U</mi><mo>-</mo><mi mathvariant="normal">Th</mi><mo>)</mo><mo>/</mo><mi mathvariant="normal">He</mi></mrow></math><span><svg:svg xmlns:svg="http://www.w3.org/2000/svg" width="58pt" height="14pt" class="svg-formula" dspmath="mathimg" md5hash="c9cf0718e10396f6e2182a01dacbca3e"><svg:image xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="ejm-35-383-2023-ie00005.svg" width="58pt" height="14pt" src="ejm-35-383-2023-ie00005.png"/></svg:svg></span></span> ages. Hence, sub-millimeter, undisturbed grains can be used to analyze the mineralogy of ferruginous duricrusts by XRD_rotat with a short exposure, and the same grains can subsequently be dated by <span class="inline-formula"><math xmlns="http://www.w3.org/1998/Math/MathML" id="M5" display="inline" overflow="scroll" dspmath="mathml"><mrow class="chem"><mo>(</mo><mi mathvariant="normal">U</mi><mo>-</mo><mi mathvariant="normal">Th</mi><mo>)</mo><mo>/</mo><mi mathvariant="normal">He</mi></mrow></math><span><svg:svg xmlns:svg="http://www.w3.org/2000/svg" width="58pt" height="14pt" class="svg-formula" dspmath="mathimg" md5hash="1b812d81e06111d524c50b551af57291"><svg:image xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="ejm-35-383-2023-ie00006.svg" width="58pt" height="14pt" src="ejm-35-383-2023-ie00006.png"/></svg:svg></span></span> geochronology analysis. The <span class="inline-formula"><math xmlns="http://www.w3.org/1998/Math/MathML" id="M6" display="inline" overflow="scroll" dspmath="mathml"><mrow class="chem"><mo>(</mo><mi mathvariant="normal">U</mi><mo>-</mo><mi mathvariant="normal">Th</mi><mo>)</mo><mo>/</mo><mi mathvariant="normal">He</mi></mrow></math><span><svg:svg xmlns:svg="http://www.w3.org/2000/svg" width="58pt" height="14pt" class="svg-formula" dspmath="mathimg" md5hash="9d21999f80ac3e5cb55b34a6e125d8e4"><svg:image xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="ejm-35-383-2023-ie00007.svg" width="58pt" height="14pt" src="ejm-35-383-2023-ie00007.png"/></svg:svg></span></span> dating of pisolitic core and cortex grains also provided meaningful ages: they revealed two evolution phases of the ferruginous duricrust, which occurred at or before the Oligocene for the pisolitic core and middle Miocene for the pisolitic cortex, agreeing with the previous model for the development of pisolites. The mineralogy of single grains selected for dating is helpful for discussing the crystallization ages, and the high-flux XRD approach may be applied to other supergene mineral parageneses used for absolute dating.</p>
first_indexed 2024-03-13T05:34:18Z
format Article
id doaj.art-2f3a972d248b4db0aeec9185d7e1fac1
institution Directory Open Access Journal
issn 0935-1221
1617-4011
language English
last_indexed 2024-03-13T05:34:18Z
publishDate 2023-06-01
publisher Copernicus Publications
record_format Article
series European Journal of Mineralogy
spelling doaj.art-2f3a972d248b4db0aeec9185d7e1fac12023-06-14T10:17:12ZengCopernicus PublicationsEuropean Journal of Mineralogy0935-12211617-40112023-06-013538339510.5194/ejm-35-383-2023Supergene phases from ferruginous duricrusts: non-destructive microsampling and mineralogy prior to (U–Th) ∕ He geochronological analysisK. P. P. Marques0K. P. P. Marques1T. Allard2C. Gautheron3B. Baptiste4R. Pinna-Jamme5G. Morin6L. Delbes7P. Vidal-Torrado8“Luiz de Queiroz” College of Agriculture, University of São Paulo, 13418-900, Piracicaba, São Paulo, BrazilInstitut de Minéralogie, de Physique des Matériaux et de Cosmochimie, UMR CNRS 7590, Sorbonne Université, IRD, MNHN, 75252, Paris CEDEX 05, FranceInstitut de Minéralogie, de Physique des Matériaux et de Cosmochimie, UMR CNRS 7590, Sorbonne Université, IRD, MNHN, 75252, Paris CEDEX 05, FranceUniversité Paris-Saclay, CNRS, GEOPS, 91405, Orsay, FranceInstitut de Minéralogie, de Physique des Matériaux et de Cosmochimie, UMR CNRS 7590, Sorbonne Université, IRD, MNHN, 75252, Paris CEDEX 05, FranceUniversité Paris-Saclay, CNRS, GEOPS, 91405, Orsay, FranceInstitut de Minéralogie, de Physique des Matériaux et de Cosmochimie, UMR CNRS 7590, Sorbonne Université, IRD, MNHN, 75252, Paris CEDEX 05, FranceInstitut de Minéralogie, de Physique des Matériaux et de Cosmochimie, UMR CNRS 7590, Sorbonne Université, IRD, MNHN, 75252, Paris CEDEX 05, France“Luiz de Queiroz” College of Agriculture, University of São Paulo, 13418-900, Piracicaba, São Paulo, Brazil<p>Interpreting the ages of supergene mineralogical phases in laterite is complex because they consist of polycrystalline mixtures of different phases at the microscopic scale that could be crystalized at different epochs. Among the geochronometers, the <span class="inline-formula"><math xmlns="http://www.w3.org/1998/Math/MathML" id="M2" display="inline" overflow="scroll" dspmath="mathml"><mrow class="chem"><mo>(</mo><mi mathvariant="normal">U</mi><mo>-</mo><mi mathvariant="normal">Th</mi><mo>)</mo><mo>/</mo><mi mathvariant="normal">He</mi></mrow></math><span><svg:svg xmlns:svg="http://www.w3.org/2000/svg" width="58pt" height="14pt" class="svg-formula" dspmath="mathimg" md5hash="f4b2fa0b999292f48cb1b1e04a07aa2a"><svg:image xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="ejm-35-383-2023-ie00003.svg" width="58pt" height="14pt" src="ejm-35-383-2023-ie00003.png"/></svg:svg></span></span> method on hematite and goethite is more often used, but ages can be difficult to interpret due to phases mixing. To resolve this issue, this study proposes a methodology for performing detailed mineralogical analysis of hematite and goethite single grains prior to their dating using the <span class="inline-formula"><math xmlns="http://www.w3.org/1998/Math/MathML" id="M3" display="inline" overflow="scroll" dspmath="mathml"><mrow class="chem"><mo>(</mo><mi mathvariant="normal">U</mi><mo>-</mo><mi mathvariant="normal">Th</mi><mo>)</mo><mo>/</mo><mi mathvariant="normal">He</mi></mrow></math><span><svg:svg xmlns:svg="http://www.w3.org/2000/svg" width="58pt" height="14pt" class="svg-formula" dspmath="mathimg" md5hash="26d53101b6c836ab0b6ef325d9bca65f"><svg:image xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="ejm-35-383-2023-ie00004.svg" width="58pt" height="14pt" src="ejm-35-383-2023-ie00004.png"/></svg:svg></span></span> method. Strictly non-destructive mineralogy of single grains is not achievable by classical tools, such as conventional powder XRD (X-ray diffraction; requiring at least some milligrams of powder) or SEM (scanning electron microscopy; that can contaminate the grain by coating or fixing). Therefore, we performed X-ray diffraction patterns of single grains using high-flux X-ray beams from both a rotating anode (XRD_rotat) laboratory diffractometer and a synchrotron beamline (XRD_synch) and compared the results in order to design a method based on XRD_rotat only. For this purpose, two samples from the pisolitic facies of a Brazilian ferruginous duricrust (Alto Paranaíba region, Minas Gerais State, Brazil) were chosen because they presented a usual heterogeneity. Rietveld refinements of the XRD patterns obtained from both XRD_rotat and XRD_synch yielded similar results for the weight percentage ratio of the main phases and mean coherent domain sizes and less similar results for Al substitution rates, thus validating the XRD_rotat approach. No beam damage was observed when increasing X-ray exposure time, neither on XRD patterns nor on <span class="inline-formula"><math xmlns="http://www.w3.org/1998/Math/MathML" id="M4" display="inline" overflow="scroll" dspmath="mathml"><mrow class="chem"><mo>(</mo><mi mathvariant="normal">U</mi><mo>-</mo><mi mathvariant="normal">Th</mi><mo>)</mo><mo>/</mo><mi mathvariant="normal">He</mi></mrow></math><span><svg:svg xmlns:svg="http://www.w3.org/2000/svg" width="58pt" height="14pt" class="svg-formula" dspmath="mathimg" md5hash="c9cf0718e10396f6e2182a01dacbca3e"><svg:image xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="ejm-35-383-2023-ie00005.svg" width="58pt" height="14pt" src="ejm-35-383-2023-ie00005.png"/></svg:svg></span></span> ages. Hence, sub-millimeter, undisturbed grains can be used to analyze the mineralogy of ferruginous duricrusts by XRD_rotat with a short exposure, and the same grains can subsequently be dated by <span class="inline-formula"><math xmlns="http://www.w3.org/1998/Math/MathML" id="M5" display="inline" overflow="scroll" dspmath="mathml"><mrow class="chem"><mo>(</mo><mi mathvariant="normal">U</mi><mo>-</mo><mi mathvariant="normal">Th</mi><mo>)</mo><mo>/</mo><mi mathvariant="normal">He</mi></mrow></math><span><svg:svg xmlns:svg="http://www.w3.org/2000/svg" width="58pt" height="14pt" class="svg-formula" dspmath="mathimg" md5hash="1b812d81e06111d524c50b551af57291"><svg:image xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="ejm-35-383-2023-ie00006.svg" width="58pt" height="14pt" src="ejm-35-383-2023-ie00006.png"/></svg:svg></span></span> geochronology analysis. The <span class="inline-formula"><math xmlns="http://www.w3.org/1998/Math/MathML" id="M6" display="inline" overflow="scroll" dspmath="mathml"><mrow class="chem"><mo>(</mo><mi mathvariant="normal">U</mi><mo>-</mo><mi mathvariant="normal">Th</mi><mo>)</mo><mo>/</mo><mi mathvariant="normal">He</mi></mrow></math><span><svg:svg xmlns:svg="http://www.w3.org/2000/svg" width="58pt" height="14pt" class="svg-formula" dspmath="mathimg" md5hash="9d21999f80ac3e5cb55b34a6e125d8e4"><svg:image xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="ejm-35-383-2023-ie00007.svg" width="58pt" height="14pt" src="ejm-35-383-2023-ie00007.png"/></svg:svg></span></span> dating of pisolitic core and cortex grains also provided meaningful ages: they revealed two evolution phases of the ferruginous duricrust, which occurred at or before the Oligocene for the pisolitic core and middle Miocene for the pisolitic cortex, agreeing with the previous model for the development of pisolites. The mineralogy of single grains selected for dating is helpful for discussing the crystallization ages, and the high-flux XRD approach may be applied to other supergene mineral parageneses used for absolute dating.</p>https://ejm.copernicus.org/articles/35/383/2023/ejm-35-383-2023.pdf
spellingShingle K. P. P. Marques
K. P. P. Marques
T. Allard
C. Gautheron
B. Baptiste
R. Pinna-Jamme
G. Morin
L. Delbes
P. Vidal-Torrado
Supergene phases from ferruginous duricrusts: non-destructive microsampling and mineralogy prior to (U–Th) ∕ He geochronological analysis
European Journal of Mineralogy
title Supergene phases from ferruginous duricrusts: non-destructive microsampling and mineralogy prior to (U–Th) ∕ He geochronological analysis
title_full Supergene phases from ferruginous duricrusts: non-destructive microsampling and mineralogy prior to (U–Th) ∕ He geochronological analysis
title_fullStr Supergene phases from ferruginous duricrusts: non-destructive microsampling and mineralogy prior to (U–Th) ∕ He geochronological analysis
title_full_unstemmed Supergene phases from ferruginous duricrusts: non-destructive microsampling and mineralogy prior to (U–Th) ∕ He geochronological analysis
title_short Supergene phases from ferruginous duricrusts: non-destructive microsampling and mineralogy prior to (U–Th) ∕ He geochronological analysis
title_sort supergene phases from ferruginous duricrusts non destructive microsampling and mineralogy prior to u th he geochronological analysis
url https://ejm.copernicus.org/articles/35/383/2023/ejm-35-383-2023.pdf
work_keys_str_mv AT kppmarques supergenephasesfromferruginousduricrustsnondestructivemicrosamplingandmineralogypriortouthhegeochronologicalanalysis
AT kppmarques supergenephasesfromferruginousduricrustsnondestructivemicrosamplingandmineralogypriortouthhegeochronologicalanalysis
AT tallard supergenephasesfromferruginousduricrustsnondestructivemicrosamplingandmineralogypriortouthhegeochronologicalanalysis
AT cgautheron supergenephasesfromferruginousduricrustsnondestructivemicrosamplingandmineralogypriortouthhegeochronologicalanalysis
AT bbaptiste supergenephasesfromferruginousduricrustsnondestructivemicrosamplingandmineralogypriortouthhegeochronologicalanalysis
AT rpinnajamme supergenephasesfromferruginousduricrustsnondestructivemicrosamplingandmineralogypriortouthhegeochronologicalanalysis
AT gmorin supergenephasesfromferruginousduricrustsnondestructivemicrosamplingandmineralogypriortouthhegeochronologicalanalysis
AT ldelbes supergenephasesfromferruginousduricrustsnondestructivemicrosamplingandmineralogypriortouthhegeochronologicalanalysis
AT pvidaltorrado supergenephasesfromferruginousduricrustsnondestructivemicrosamplingandmineralogypriortouthhegeochronologicalanalysis