Marine and Petroleum Geology 91 (2018) 338–349

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Marine and Petroleum Geology

journal homepage: www.elsevier.com/locate/marpetgeo

Research paper

Thermal maturity assessment study of the late Pliensbachian-early Toarcian T

organic-rich sediments in southern France: Grands Causses, Quercy and
Pyrenean basins
Carolina Fonsecaa,c,∗, Joalice Oliveira Mendonçab, João Graciano Mendonça Filhob,
Carine Lézinc, Luis V. Duartea
a
MARE - Marine and Environmental Sciences Centre, Faculty of Sciences and Technology, Department of Earth Sciences, University of Coimbra, Rua Sílvio Lima, 3030-
790 Coimbra, Portugal
b
Laboratório de Palinofácies e Fácies Orgânica (LAFO), Departamento de Geologia, Instituto de Geociências, Universidade Federal do Rio de Janeiro, Av. Athos da
Silveira, 274, prédio do CCMN, sala J1020, Campus Ilha do Fundão, Cidade Universitária, CEP 21.949-900, Rio de Janeiro, RJ, Brazil
c
Géosciences Environnement Toulouse (GET), Observatoire Midi Pyrénées, Université de Toulouse, CNRS, IRD, 14 avenue E. Belin, F-31400 Toulouse, France

A R T I C L E I N F O A B S T R A C T

Keywords: Thermal maturity of late Pliensbachian-early Toarcian organic-rich sediments in the Grands Causses (Suèges
Thermal maturity section), Quercy (Caylus section) and Pyrenean (Pont de Suert section) basins was determined through multiple
Hydroid reflectance parameters, including Spore Coloration Index (SCI), hydroid random reflectance (HRr) and spectral fluorescence
Spectral fluorescence of Tasmanites algae (λmax). The main objective of this study is to test the effectiveness and make comparisons of
Spore coloration index
organic matter thermal maturity in these three sections by different techniques and particularly hydroid re-
Lower jurassic
flectance.
Southern France
For the Suèges section SCI presented a value of 3.5–4.0. HRr ranges between 0.36% and 0.47%, which cor-
responds to 0.45%–0.52% VReq, and shows a good correlation with SCI values. Spectral fluorescence analysis
presents a λmax of 560 nm for most samples. The fluorescence spectral maximum seems to be redshifted in
comparison to other thermal maturity parameters.
The Caylus section exhibited SCI of 3.5–4.0. HRr ranges between 0.32% and 0.50% corresponding to
0.42%–0.54% VReq. Spectral fluorescence analysis points out a λmax of 560 nm, displaying a good correlation
with SCI. When Req values determined through SCI are compared with equivalent vitrinite reflectance values
determined through λmax, a redshift of the fluorescence spectrum maximum is detected.
For the Pont de Suert section SCI ranges between 8.0-8.5 and 8.5–9.0. HRr varies between 0.85% and 1.18%
which corresponds to 0.76%–0.98% VReq. Even though there are lower values than those obtained by SCI, VReq
is reliable and acceptable to determine the thermal evolution stage. Furthermore, HRr values also present a good
correlation with SCI.
These data indicate that the majority of the samples from the Suèges and Caylus sections are in the immature
to early mature evolution stages and Pont de Suert section samples are in late mature to early overmature
evolution stages for liquid hydrocarbons generation, supporting a very similar thermal evolution for the Grands
Causses and Quercy basins and an entirely different thermal history for the Pyrenean Basin. This is in accordance
with the similar tectonic and sedimentary context of the Quercy and Grands Causses basins. The Pont de Suert
section, located near the collision front of the Pyrenees mountains, records a more complex sedimentary and
tectonic history. In addition, this study presents the first reflectance data for Jurassic hydroids, which show a
good correlation with other rank parameters.

1. Introduction matter (OM) goes through a physiochemical transformation that is

controlled firstly by biological activity followed by thermodynamic
During the geological history of sedimentary basins, the organic factors (Tissot and Welte, 1984). These progressive and almost

∗
Corresponding author. MARE - Marine and Environmental Sciences Centre, Faculty of Sciences and Technology, Department of Earth Sciences, University of Coimbra, Rua Sílvio
Lima, 3030-790 Coimbra, Portugal.
E-mail address: [email protected] (C. Fonseca).

https://doi.org/10.1016/j.marpetgeo.2018.01.017
Received 21 September 2017; Received in revised form 3 January 2018; Accepted 12 January 2018
Available online 17 January 2018
0264-8172/ © 2018 Elsevier Ltd. All rights reserved.
C. Fonseca et al. Marine and Petroleum Geology 91 (2018) 338–349

Fig. 1. Paleogeographic map of early Jurassic with location of studied basins (modified from Lézin et al., 2013; van de Schootbrugge et al., 2005): (A) Simplified geological map of the
Grands Causses Basin and location of the studied Suèges section (Fonseca et al., 2017); (B) Simplified geological map of the Quercy Basin and location of the studied Caylus section
(Fonseca et al., 2017); (C) Simplified geological map of the Pyrenean Basin and location of the studied Pont de Suert section (modified from Riera et al., 2009; Sellés and Vila, 2015). IM:
Iberian Meseta; AM: Amorican Massif; CM: Central Massif; LBM: London-Brabant Massif; BM: Bohemian Massif.

continuous changes in the chemical and physical properties of the se- Ordovician, 1 Silurian and 1 Jurassic). Kozlowski (1959) described 15
dimentary OM reflect and are an indicator of the thermal and burial genera and 22 species of polypoid forms of Ordovician Hydroids with
history of the basins (Tissot and Welte, 1984). To quantify thermal chitin skeletons and doubted Eisenack's (1935, 1934, 1932) conclusions
maturity of sedimentary rocks, several optical parameters were devel- due to sample fragmentation. Bertrand (1987), based on Kozlowski's
oped during the years, being vitrinite and huminite reflectance the most (1959) descriptions, presented the first reflectance measurements on
commonly used. However, when absent, other organic particles of Ordovician Hydroids.
different origins (e.g. solid bitumen, zooclasts) can be used as alter- Hydroid remains were described as being consistently observed in
native to assess thermal maturity (Hartkopf-Fröder et al., 2015). polished blocks of Ordovician to Devonian marine sedimentary rocks
Animal-derived organic particles are often reported as minor com- (Bertrand and Malo, 2012; Héroux et al., 2000). Nevertheless, these
ponents of the sedimentary OM. These components can be classified as remains are usually less often recorded compared to graptolites, chit-
belonging to: (i) the Zoomorph Subgroup, when composed by discrete inozoans or scolecodonts (e.g. Bertrand, 1987; Héroux et al., 2000),
unitary animal-derived particles, whether whole or fragmented, in- possibly due to identification issues. Bertrand (1991, 1990) and
cluding foraminiferal test-linings, chitinozoans, and scolecodonts; and, Bertrand and Malo (2012) suggested that hydroids can be a major
(ii) the Zooclast Group, which comprises unknown organic, structured, constituent of the zooclast/zoomorph fraction in proximal marine se-
fragmentary particles (clasts), with an angular outline (the most dimentary settings, although hydroid reflectance has been used only as
common varieties include graptolites, conchostraceans and other crus- a supplementary maturity parameter, compared to reflectance of
tacean fragments, arthropod exoskeletal debris, organic linings from graptolites, chitinozoans and scolecodonts, which are more often em-
some bivalve shells, tintinnids, and insect cuticle fragments) (Mendonça ployed to determine the equivalent vitrinite reflectance (e.g. Bertrand,
Filho et al., 2014c, 2012; Tyson, 1995). 1990, 1987; Bertrand and Malo, 2012, 2005; Bertrand et al., 2003;
Mendonça Filho et al. (2016) described for the first time the oc- Héroux et al., 2000, 1996). Hartkopf-Fröder et al. (2015) suggested that
currence, in dispersed OM, of Cnidarians (Phylum Cnidaria), Class this may be due to lower abundance of hydroids compared to other
Hydrozoa (Hydrozoans), and Hydroida Order (Hydroids); namely its zooclasts and zoomorphs. Mendonça Filho et al. (2016) suggested that
free-swimming medusoid forms. Recently, Mendonça Filho and hydroid fragments have probably been classified as undifferentiated
Gonçalves (2017) included these animal components in the classifica- zooclasts due to lack of knowledge and experience in their identifica-
tion system of the individual palynological components from the Zoo- tion. Nevertheless, hydroid reflectance has been used in a few previous
morph Subgroup, together with cuticles of ostracods, within the Zoo- maturation studies of Ordovician and Silurian sedimentary rocks
clast Group, and Fonseca et al. (2017) presented the first (Bertrand, 1993, 1990, 1987; Héroux and Chagnon, 1994; Héroux et al.,
paleoenvironmental application of Hydroids in a palynofacies based 2000, 1996; Bertrand et al., 2003; Bertrand and Malo, 2012, 2005).
study of the Toarcian Oceanic Anoxic Event organic record of the The description of the first occurrence of components from the
Grands Causses and Quercy basins (southern France). In literature, the Phylum Cnidaria, Class Hydrozoa, Order Hydroida in the record of
fossil record of these organisms is mostly restricted to forms with a particulate OM of the late Pliensbachian – earliest middle Toarcian
carbonate skeleton. Nonetheless, Eisenack (1935, 1934, 1932) defined sedimentary successions of the Grands Causses and Quercy basins in
4 genera of Hydrozoa polypoid forms with chitin skeletons (2 from the southern France was made by Fonseca et al. (2017). This opens the

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C. Fonseca et al. Marine and Petroleum Geology 91 (2018) 338–349

Fig. 2. Stratigraphic logs of studied sections with sample location. (A) Suèges section (Fonseca et al., 2017); (B) Caylus section (Fonseca et al., 2017); (C) Pont de Suert section.

opportunity to pursue a thermal maturity study of the dispersed OM of first approach to the use of hydroids as a key thermal maturity para-
this time interval in different basins of southern France, especially fo- meter for OM of this age.
cused and based on the hydroid reflectance.
The Lower Jurassic sequence in southern France has been the main
2. Geological setting
focus of stratigraphic, sedimentological and geochemical studies for
decades (Cubaynes, 1986; Cubaynes et al., 1989; Emmanuel et al.,
The Jurassic paleogeography of southern France is characterized by
2006; Harazim et al., 2013; Trümpy, 1983, and references therein).
a number of interconnected shallow marine epicontinental basins bor-
However, no emphasis has been given to the study of the thermal
dered by the Central Massif to the north, and open and in connection
maturity of the OM present in the organic-rich carbonate Toarcian se-
with the Tethys Ocean towards the south. Shallow marine sedimenta-
dimentary rocks of the basins in this region. Therefore, this study aims:
tion occurred in each basin isolated from each other by paleo-highs
(i) to estimate and compare the OM thermal maturity, through organic
(Dumont, 1988; Lemoine and de Graciansky, 1988; Thierry et al.,
petrology techniques, of the upper Pliensbachian-lowermost middle
2000). In this geological framework are included the selected basins for
Toarcian sedimentary successions of the GCB, QB and PB; and, (ii) to
this study (Fig. 1): Grands Causses Basin (GCB), Quercy Basin (QB) and
assess the consistency of values obtained using different techniques
Pyrenean Basin (PB). From each basin was selected one reference sec-
(Spore Coloration Index, spectral fluorescence and hydroid reflectance).
tion, namely, Suèges (Fig. 1, A), Caylus (Fig. 1, B) and Pont de Suert
So far, no published data on reflectance of Jurassic hydroids are
(Fig. 1, C) sections, respectively.
available, and their use as a major index for the assessment of sedi-
In the Suèges section (Fig. 2, A), the studied chronological frame is
mentary OM maturity has not been attempted. This paper, then, is the
represented by organic-rich marls with intercalated limestone beds of

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C. Fonseca et al. Marine and Petroleum Geology 91 (2018) 338–349

Table 1 3. Materials and methodologies

Samples ordered by basin and lithostratigraphy as well as the lithological composition.
3.1. Materials
Sample ID Lithostratigraphy Lithological
description
For this research a set of 38 outcrop rock samples was selected.
Grands Causses Basin From the Suèges section (GCB) a set of 13 samples belonging to the
S69 Marnes de Fontaneilles Fm. Marl
Rivière-sur-Tarn Group was analyzed: three from the Marnes de
S64 Marnes de Fontaneilles Fm. Marl
S61 Marnes de Fontaneilles Fm. Marl Villeneuve Fm., seven from the Schistes Cartons Fm. and three from the
S55 Schistes Cartons Fm. Marl Marnes de Fontaneilles Fm. (Fig. 2, A; Table 1). In the Caylus section
S52 Schistes Cartons Fm. Black Shale (QB) 11 samples were collected and studied: four from the Barre à
S50 Schistes Cartons Fm. Black Shale Pecten Fm., six from the Schistes Cartons Mb. of the Penne Fm. and one
S22 Schistes Cartons Fm. Black Shale
from the Marnes et calcaires à Hildoceras Mb. of the Penne Fm. (Fig. 2,
S19 Schistes Cartons Fm. Black Shale
S17 Schistes Cartons Fm. Black Shale B; Table 1). In the PB, the Pont de Suert section was studied and a total
S15 Schistes Cartons Fm. Black Shale of 14 samples were collected and analyzed: one from the Barre a Pecten
S12 Marnes de Villeneuve Fm. Marl Fm., five from the Calcaires argileux à Spirifèrines Mb. of the Padrinas
S11 Marnes de Villeneuve Fm. Marl
Fm., three from the Calcaires argileux et marnes à Soaresirhynchia Mb.
S10 Marnes de Villeneuve Fm. Marl
Quercy Basin of the Padrinas Fm. and five from the Calcaires argileux à Telothyris Mb.
Cay 28 Marnes et calcaires à Hildoceras Mb. Marl of the Padrinas Fm. (Fig. 2, C; Table 1).
Cay 26 Schistes Cartons Mb. Marl
Cay 23 Schistes Cartons Mb. Marl 3.2. Kerogen isolation
Cay 20 Schistes Cartons Mb. Marl
Cay 18 Schistes Cartons Mb. Marl
Cay 13 Schistes Cartons Mb. Marl Kerogen isolation from the rock matrix was performed using stan-
Cay 10 Schistes Cartons Mb. Marl dard non-oxidative procedures according to Mendonça Filho et al.
Cay 7 Barre à Pecten Fm. Limestone (2014a, 2012) and Tyson (1995). Each rock sample was fragmented to
Cay 6 Barre à Pecten Fm. Limestone
approximately 2 mm size and subjected to acid treatment to remove
Cay 3 Barre à Pecten Fm. Limestone
Cay 1 Barre à Pecten Fm. Limestone
carbonates (HCl 37% for 18 h), silicates (HF 40% for 24 h), and neo-
Pyrenean Basin formed fluorides (HCl 37% for 3 h). Between each step the pH of the
265PS Calcaires argileux à Telothyris Mb. Calcareous marl material was neutralized with distilled water. The organic and non-
255PS Calcaires argileux à Telothyris Mb. Marl organic materials were separated by flotation using ZnCl2 (den-
470PS Calcaires argileux à Telothyris Mb. Marl
sity = 1.9–2 g/cm3). The organic fraction was recovered and the heavy
420PS Calcaires argileux à Telothyris Mb. Marly limestone
380PS Calcaires argileux à Telothyris Mb. Marl liquid was eliminated using drops of HCl (10%) followed by a wash
355PS Calcaires argileux et marnes à Marly limestone with distilled water. After this procedure, kerogen concentrate mounts
Soaresirhynchia Mb. were made with the organic residue. The isolated kerogen was also
330PS Calcaires argileux et marnes à Marl
sieved at 10 μm and strew slides were prepared from this material.
Soaresirhynchia Mb.
300PS Calcaires argileux et marnes à Calcareous marl
Soaresirhynchia Mb. 3.3. Geochemical analysis
115PS Calcaires argileux à Spiriférines Mb. Marly limestone
100PS Calcaires argileux à Spiriférines Mb. Marl Total organic carbon (TOC), total sulfur (TS) contents and insoluble
75PS Calcaires argileux à Spiriférines Mb. Limestone
residue were determined, after acidification for removal of carbonates,
65-7PS Calcaires argileux à Spiriférines Mb. Marl
45PS Calcaires argileux à Spiriférines Mb. Marl using a LECO SC 144 analyzer, following the ASTM Standard D4239-08
20PS Barre a Pecten Fm. Limestone (2008) and NCEA-C-1282 (United States Environmental Protection
Agency, U.S.EPA, 2002) methods. Total carbonate content was ob-
tained by the difference between the original sample weight and the
the Marnes de Villeneuve Fm., the finely laminated organic-rich shales insoluble residue weight.
of the Schistes Carton Fm., and by the monotonous grey marls of the
Marnes de Fontaneilles Fm. (Harazim et al., 2013; Trümpy, 1983). 3.4. Palynofacies analysis
The study interval in the Caylus section (Fig. 2, B) corresponds to a
set of grey or red massive decimetric layers of limestone of the Barre à Isolated kerogen examination was performed by microscopic ana-
Pecten Fm., the detrital marls and shales of the Schistes Cartons lysis of the strew slides, under transmitted white light (TWL) and in-
Member (Mb.) of the Penne Fm., and the marly dominated succession cident blue light (fluorescence mode – FM). The palynofacies analyses
with alternation between decimetric layers of limestone and marls of involved the qualitative (organic particle component identification)
the Marnes et calcaires à Hildoceras Mb. of the Penne Fm. (Cubaynes and quantitative (counting from 300 to 500 particles) examinations of
et al., 1989; Qajoun, 1994). the kerogen. The counting was conducted following the OM groups and
The Pont de Suert section (Fig. 2, C) is characterized, from the late subgroups classification proposed by Mendonça Filho and Gonçalves
Pliensbachian-early Toarcian, by the limestone dominated Barre a (2017), Mendonça Filho et al. (2016, 2014b, 2012) and Tyson (1995).
Pecten Fm., and the carbonate and/or argillaceous-carbonate alterna-
tion of three members of the Padrinas Fm. (alternations of marl and 3.5. Organic petrology
argillaceous limestone of the Calcaires argileux à Spirifèrines Mb., the
argillaceous limestones and marls of the Calcaires argileux et marnes à Optical petrography was performed on whole rock polished blocks
Soaresirhynchia Mb., and the marl and argillaceous limestone domi- prepared according to standard procedures (ISO 7404-2, 2009) and
nated Calcaires argileux à Telothyris Mb.) (Fauré, 2002). kerogen concentrate mounts and strew slides prepared according to
sample preparation protocol described in section 2.2.

3.5.1. Spore Coloration Index

SCI was determined using the standard slides of LAFO-UFRJ with a
scale of 1–10 with intervals of 0.5. This analysis was performed when

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Table 2
Geochemical and palynofacies data. Grands Causses and Quercy basins data according to Fonseca et al. (2017).

Formation/Member Sample ID Geochemical data Palynofacies data

TOCa TCCa PHYa AMOa PALa ZOOa

Grands Causses Basin

Marnes de Fontaneilles Fm. S69 2.60 36 0.97 51.94 6.77 40.32
S64 1.28 50 6.33 44.62 21.20 27.85
S61 4.31 44 0.00 79.33 0.67 20.00
Schistes Cartons Fm. S55 3.12 41 0.00 67.44 1.00 31.56
S52 4.56 44 1.33 97.67 0.66 0.33
S50 5.97 50 0.33 99.34 0.33 0.00
S22 6.53 51 0.65 98.39 0.32 0.65
S19 4.40 58 1.31 96.72 0.66 1.31
S17 6.13 38 1.30 95.44 0.65 2.61
S15 6.79 16 0.31 97.17 0.63 1.89
Marnes de Villeneuve Fm. S12 0.91 29 10.19 35.99 19.43 34.39
S11 0.70 37 19.87 14.57 31.13 34.44
S10 0.50 36 23.92 17.28 25.91 32.89
Quercy Basin
Marnes et calcaires à Hildoceras Mb. Cay 28 0.32 41 0.95 84.18 3.48 11.39
Schistes Cartons Mb. Cay 26 8.80 29 0.00 0.00 99.35 0.65
Cay 23 7.94 22 0.00 0.00 100.00 0.00
Cay 20 3.35 18 0.00 0.00 100.00 0.00
Cay 18 3.24 18 0.00 0.00 99.37 0.63
Cay 13 1.71 34 0.00 0.00 98.43 1.57
Cay 10 0.38 46 6.31 0.00 81.40 12.29
Barre à Pecten Fm. Cay 7 0.12 83 0.65 0.00 88.27 11.07
Cay 6 0.12 85 Low Recovery
Cay 3 0.16 82
Cay 1 0.18 85 2.78 0.00 87.65 9.57
Pyrenean Basin
Calcaires argileux à Telothyris Mb. 265PS 0.25 60 0.65 0.00 2.28 97.07
255PS 0.33 33 2.31 0.00 4.32 93.37
470PS 0.25 49 1.27 0.00 52.87 45.86
420PS 0.14 79 0.00 0.00 89.35 10.65
380PS 0.30 40 1.29 0.00 28.06 70.65
Calcaires argileux et marnes à Soaresirhynchia Mb. 355PS 0.16 73 0.00 0.00 32.69 67.31
330PS 0.31 42 1.62 0.00 34.42 63.96
300PS 0.25 61 2.31 0.00 54.46 43.23
Calcaires argileux à Spiriférines Mb. 115PS 0.35 49 0.00 0.00 79.03 20.97
100PS 0.31 47 0.96 0.00 59.87 39.17
75PS 0.21 76 0.99 0.00 18.21 80.79
65-7PS 0.40 42 2.56 0.00 15.75 81.68
45PS 0.40 39 3.65 0.00 10.30 86.05
Barre a Pecten Fm. 20PS 0.24 87 3.64 0.00 26.16 70.20

a
TOC: Total organic carbon (wt.%); TCC: Total carbonate content (wt.%); PHY: Phytoclast (%); AMO: Amorphous (%); PAL: Palynomorph (%); ZOO: Zooclast (%).

slides showed the presence of sporomorphs. It was carried out on a Carl 50× magnification in immersion oil (ηe = 1.518–23 °C), according to
Zeiss Axio Imager A1 microscope with 20× magnification through the ASTM Standard D7708 (2014). The microscope was calibrated with
optical comparison of sporomorphs coloration in transmitted white Spinel (0.425% Rr) or YAG (0.893% Rr) standards.
light. Equivalent vitrinite reflectance (VReq) values were determined The OM reflectance was measured in hydroid fragments and the
according to the SCI, temperature, and age correlation chart proposed reflectance values were converted to equivalent vitrinite reflectance
by Fisher et al. (1980). using equation (1) as proposed by Bertrand and Malo (2012) and
Hartkopf-Fröder et al. (2015):
3.5.2. Spectral fluorescence analysis VReq = 0.6493*HRr + 0.2126 (1)
Spectral fluorescence analysis is based on the measure of spectral
intensity at 400–700 nm (Ottenjann, 1980, 1975; Ottenjann et al., where VReq is the equivalent vitrinite reflectance and HRr is the mea-
1981, 1974). Spectral fluorescence measurements were executed with a sured hydroid random fragment reflectance.
Zeiss Axioskop 2-plus microscope, with 50× magnification in immer-
sion oil (ηe = 1.518–23 °C), and (Zeiss) ultraviolet G 365, FT 395 and
4. Results
LP 420 filters. The correction factor was obtained based on the cali-
bration of a lamp (Baranger et al., 1991). Spectral fluorescence analysis
4.1. Organic geochemistry and palynofacies data
was performed on selected macerals from the liptinite group (Pickel
et al., 2017) (Tasmanites - Prasinophyte algae), using calibration pro-
For the Suèges section (GCB) TOC values range between 0.50 wt%
cedures described by Araujo et al. (2002, 2003).
and 6.79 wt%, with the highest values being associated with the black
shales of the Schistes Cartons Fm. (average of 5.36 wt%). Total carbo-
3.5.3. Organic matter reflectance nate content values range from 16 wt% to 58 wt%, with the highest
Reflectance measurements were performed on plugs of concentrated carbonate content being registered in both the Schistes Cartons and
kerogen and whole rock polished blocks with a Zeiss Axioskop 2-plus Marnes de Villeneuve formations (Table 2).
microscope, equipped with spectrophotometer J&M (MSP 200), with In the Caylus section (QB) TOC values vary from 0.12 wt% to

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Fig. 3. Photomicrographs highlighting the optical characteristics of hydroids. A: Fragment of polyp showing lateral budding (S10); B: Portion of polyp showing lateral budding (20PS); C:
Feature of tentacle form of Hydrozoan polyp showing cells of cnidocytes (S11); D: Fragment of hydroid colonial stalk showing the cnidocyte cells preserved (20PS); E: Hydroid particle
displaying a rugose texture in the polished surface (S10); F: Hydroid displaying the typical sympodial pattern of growth (45PS); G: Hydroid displaying tube-like structures (65-7PS); H–I:
Hydroid exhibiting a rugose texture and a sympodial pattern of growth (470PS, 380PS). Transmitted white light: A, B, C, D; Reflected white light: E, F, G, H, I.

8.80 wt%. The highest values were recorded for the marls of the Suert section samples are dominated by either the Palynomorph group
Schistes Cartons Mb. of the Penne Fm. (average 4.24 wt%). Total car- (up to 87.74% of amorphous zoomorphs - hydrozoans) or the Zooclast
bonate content values vary between 16 wt% and 85 wt%. The Barre à group (up to 97.07% of hydrozoan polypoid forms fragments) (Table 2).
Pecten Fm. presents the highest carbonate content of the section
(average 83.75 wt%) (Table 2).
4.2. Optical characteristics of the hydroids
The Pont de Suert section (PB) displays TOC values ranging between
0.14 wt% and 0.40 wt%. The highest values recorded correspond to the
In transmitted white light (TWL), hydroids are dark brown to black
Calcaires argileux à Spiriférines Mb. of the Padrinas Fm. (average
in color and usually show no fluorescence. However, in some cases they
0.34 wt%). Highest total carbonate content is displayed by the Barre a
can display a fluorescence coloration ranging from dark orange to dark
Pecten Fm. (87 wt%) (Table 2).
brown. In some particles were identified tube-like structures, a sym-
The summarized palynofacies data for the three studied sections are
podial pattern of growth, and the presence of cnidocytes cells, typical
listed in Table 2. These data from the Suéges and Caylus sections are
characteristics that allow the classification of hydroids (Fig. 3, A-D).
presented as published by Fonseca et al. (2017). The three sections
In reflected white light (RWL), hydroids are grey and isotropic,
revealed the presence of hydrozoans as a major component of the OM
presenting a rugose texture in the polished surface. Petrographic ob-
assemblages. Since the reflectance assessment study was based on re-
servations revealed various degrees of amorphization and oxidation of
flectance of animal particles, and a palynofacies analysis is not the
the particles. Some hydroid particles display the typical sympodial
objective of this work, only the animal or animal-derived organic
pattern of growth; the identification of tube-like structures is also
fraction is discussed in this section.
possible (Fig. 3, E-I).
The Suèges section is dominated by the Amorphous group (up to
99.34% of hydrozoan-derived Amorphous Organic Matter – AOM), with
the exception of samples S10 and S11, where the Zooclast group pre- 4.3. Organic petrology
dominates (average 33.67% of hydrozoan polypoid forms fragments)
(Fonseca et al., 2017). The OM assemblage of Caylus section samples 4.3.1. Grands Causses basin
present very high values of the Palynomorph group (up to 98.75% of For samples from Suèges section, SCI presents a value of 3.5–4.0
amorphous zoomorphs - hydrozoans), with representative proportions which corresponds to an equivalent vitrinite reflectance (Req) of 0.45%
of the Zooclast group in samples Cay7, Cay10 and Cay28 (up to 12.29% according to Fisher et al. (1980) (Fig. 4, A-B; Table 3).
of hydrozoan polypoid forms fragments) (Fonseca et al., 2017). Pont de Spectral fluorescence analysis was performed on Tasmanites in
eleven samples from this section. The lambda maximum (λmax) is

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Fig. 4. Photomicrographs of OM from the Suèges section samples. A–B: Example of spore used to determine SCI (S69); C–E: Example of liptinite maceral (telalginite – Tasmanites) used for
spectral fluorescence measurements (S61); F–L: Example of reflectance measured hydroid particles. Transmitted white light: A; FM: B, D, E; Reflected white light: C, F, G, H, I, J, K, L.

560 nm for the majority of samples with the exception of sample S12 0.60 (Cay26) (Fig. 5, C; Table 4).
that presented λmax of 510 nm. Red/green quotient (Q) values ranged Hydroid random reflectance ranges from 0.32% (Cay 18) to 0.50%
between 0.53 (S12) and 0.77 (S17) (Fig. 4, C-E; Table 3). HRr (Cay 6), corresponding to 0.42%–0.54% VReq (Fig. 5, D-I; Table 4).
The hydroid random reflectance varies from 0.36% (S61) and 0.47% Barre à Pecten Fm. and Marnes et calcaires à Hildoceras Mb. display
HRr (S50, S64, S69), which corresponds to 0.45% and 0.52% VReq. higher average values, 0.43% HRr (0.49% VReq) and 0.41% HRr (0.48%
Marnes de Villeneuve Fm. and Schistes Cartons Fm. samples show the VReq) respectively, when compared with the Schistes Cartons Mb. that
same average value of 0.42% HRr (0.48% VReq), with Marnes de presents an average of 0.37% HRr (0.45% VReq).
Villeneuve Fm. samples exhibiting a slightly higher average of 0.43 %
HRr (0.49% VReq) (Fig. 4, F-N; Table 3).
4.3.3. Pyrenean Basin
For samples from Pont de Suert section the SCI presented values
4.3.2. Quercy Basin ranging between 8.0-8.5 and 8.5–9.0 which corresponds to a Req value
The Caylus section samples exhibit SCI values of 3.5–4.0 which of 0.90%–1.20% (Fisher et al., 1980) (Fig. 6, A-B; Table 5).
corresponds to a Req value of 0.45% according to the %Rr, SCI, tem- The hydroid reflectance varies between 0.85% (470PS) and 1.18%
perature, and age correlation chart proposed by Fisher et al. (1980) HRr (65–7 PS), equivalent to a vitrinite reflectance of 0.76% (470PS) to
(Fig. 5, A-B; Table 4). 0.98% VReq (65-7PS) (Fig. 6, C-I; Table 5). Barre a Pecten Fm. exhibits
Spectral fluorescence analysis was performed on two samples from the highest average of the section with 1.16% HRr (0.97% VReq).
the section with the liptinite (telalginite - Tasmanites) exhibiting λmax of Calcaries argileux à Spiriférines Mb. and Calcaires argileux et marnes à
560 nm for both samples and Q ratio ranging between 0.59 (Cay28) and Soaresirhynchia Mb. present similar average values of 1.08% HRr

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Table 3
Thermal maturity data from the Suèges section samples.

Sample ID SCIa %Reqa Organic matter reflectance Spectral fluorescence

Fisher et al. (1980)
%HRra Stdeva na %VReqa λmaxa Qa na

Marnes de Fontaneilles Fm.

S69 (kc) 3.5–4.0 0.45 0.47 0.04 6 0.52 560 0.67 10
S64 (kc) 3.5–4.0 0.45 0.47 0.06 13 0.52 560 0.71 2
S61 (kc) 3.5–4.0 0.45 0.36 0.06 3 0.45 560 0.64 4
Schistes Cartons Fm.
S55 (kc) 3.5–4.0 0.45 0.39 0.08 7 0.46 560 0.68 1
S52 (kc) 3.5–4.0 0.45 0.43 0.04 7 0.49 560 0.74 14
S50 (kc) 3.5–4.0 0.45 0.47 0.06 8 0.52 560 0.63 3
S22 (kc) 3.5–4.0 0.45 0.42 0.11 2 0.48 560 0.60 12
S19 (kc) 3.5–4.0 0.45 0.43 0.07 13 0.49 560 0.64 2
S17 (kc) 3.5–4.0 0.45 0.43 0.05 19 0.49 560 0.77 1
S15 (kc) 3.5–4.0 0.45 0.39 0.07 18 0.46 – – –
Marnes de Villeneuve Fm.
S12 (kc) 3.5–4.0 0.45 0.43 0.06 12 0.49 510 0.53 3
S11 (kc) 3.5–4.0 0.45 0.41 0.04 13 0.48 560 0.78 8
S10 (kc) 3.5–4.0 0.45 0.43 0.06 39 0.49 – – –

a
SCI: Spore Coloration Index; %Req: equivalent vitrinite reflectance (Fisher et al., 1980); %HRr: mean hydroid random reflectance (%); %VReq: equivalent vitrinite reflectance (%)
based on equation (1) by Bertrand and Malo (2012); Stdev: standard deviation (%); n: number of particles measured; λmax: lambda maximum; Q: red/green quotient (Q650/500); kc:
kerogen concentrate.

Fig. 5. Photomicrographs of OM from the Caylus section samples. A–B: Example of spore used to determine SCI (Cay6); C: Example of liptinite maceral (telalginite – Tasmanites) used for
spectral fluorescence measurements (Cay28); D–I: Example of reflectance measured hydroid particles. Transmitted white light: A; FM: B, C; Reflected white light: D, E, F, G, H, I.

(0.91% VReq) and 1.06% HRr (0.90% VReq), respectively. Calcaires particles were found possible to make quality readings in the plugs of
argileux à Telothyris Mb. displays the lowest reflectance average value kerogen concentrate.
of the section with 0.96% HRr (0.84% VReq).
Spectral fluorescence analysis was not performed for the Pont de 5. Discussion
Suert section samples. Although few Tasmanites particles with very
weak fluorescence were identified in the palynofacies slides, no Thermal maturity of the dispersed OM in sediments of these three

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Table 4
Thermal maturity data from the Caylus section samples.

Sample ID SCIa %Reqa Organic matter reflectance Spectral fluorescence

Fisher et al. (1980)
%HRra Stdeva na %VReqa λmaxa Qa na

Penne Fm.
Marnes et calcaires à Hildoceras Mb.
Cay 28 (kc) 3.5–4.0 0.45 0.41 0.05 7 0.48 560 0.59 3
Schistes Cartons Mb.
Cay 26 (kc) 3.5–4.0 0.45 0.34 0.05 3 0.43 560 0.60 4
Cay 23 (kc) 3.5–4.0 0.45 0.35 0.03 3 0.44 – – –
Cay 20 (kc) 3.5–4.0 0.45 0.34 0.04 11 0.44 – – –
Cay 18 (kc) 3.5–4.0 0.45 0.32 0.01 6 0.42 – – –
Cay 13 (kc) 3.5–4.0 0.45 0.39 0.03 19 0.47 – – –
Cay 10 (wr) 3.5–4.0 0.45 0.48 0.04 6 0.53 – – –
Barre à Pecten Fm.
Cay 7 (wr) 3.5–4.0 0.45 0.40 – 1 0.47 – – –
Cay 6 (wr) 3.5–4.0 0.45 0.50 0.04 2 0.54 – – –
Cay 3 (wr) 3.5–4.0 0.45 0.38 0.04 9 0.46 – – –
Cay 1 (wr) 3.5–4.0 0.45 0.44 – 1 0.50 – – –

a
SCI: Spore coloration index; %Req: equivalent vitrinite reflectance (Fisher et al., 1980); %HRr: mean hydroid random reflectance (%); %VReq: equivalent vitrinite reflectance (%)
based on equation (1) by Bertrand and Malo (2012); Stdev: standard deviation (%); n: number of particles measured; λmax: lambda maximum; Q: red/green quotient (Q650/500); kc:
kerogen concentrate; wr: whole rock.

Fig. 6. Photomicrographs of OM from the Pont de Suert section samples. Photomicrographs of OM from the Caylus section samples. A–B: Example of spores used to determine SCI (100PS,
355PS); C–I: Example of reflectance measured hydroid particles. Transmitted white light: A, B; Reflected white light: C, D, E, F, G, H, I.

basins, as obtained through OM reflectance, λmax and SCI, are similar located near the collision front of the Pyrenees mountain, records a
for the Suèges and Caylus sections but entirely different for the Pont de more complex sedimentary and tectonic history.
Suert section. This confirms different thermal maturity evolutions For the Suèges section (GCB), and according to Fisher et al. (1980)
among these basins. The tectonic and sedimentary context of the and Mukhopadhyay (1994), HRr and VReq show a good correlation with
Quercy (Caylus section) and Grands Causses (Suèges section) basins is SCI values for all samples (Fig. 7, A; Table 3). Spectral fluorescence data
relatively close. These two basins are relatively far from the Pyrenean for the majority of the samples shows a λmax value of 560 nm, de-
and the Alpine orogens. The Pont de Suert section (Pyrenean Basin), monstrating a good correlation with SCI according to Mukhopadhyay

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Table 5
Thermal maturity data from the Pont de Suert section samples.

Sample ID SCIa %Reqa Organic matter reflectance

Fisher et al. (1980)
%HRra Stdeva na %VReqa

Padrinas Fm.
Calcaires argileux à Telothyris Mb.
265PS (wr) 8.0–8.5/8.5–9.0 0.90–1.20 1.01 0.10 19 0.87
255PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 0.86 0.07 11 0.77
470PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 0.85 0.09 5 0.76
420PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 1.16 0.10 4 0.96
380PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 0.93 0.08 5 0.81
Calcaires argileux et marnes à Soaresirhynchia Mb.
355PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 1.08 0.04 2 0.91
330PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 1.00 0.06 6 0.87
300PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 1.11 0.07 31 0.93
Calcaires argileux à Spiriférines Mb.
115PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 1.13 0.04 6 0.95
100PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 1.04 0.10 11 0.89
75PS (wr) 8.0–8.5/8.5–9.0 0.90–1.20 1.01 0.09 16 0.87
65-7PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 1.18 0.07 7 0.98
45PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 1.02 0.08 7 0.88
Barre a Pecten Fm.
20PS (kc) 8.0–8.5/8.5–9.0 0.90–1.20 1.16 0.10 11 0.97

a
SCI: Spore coloration index; %Req: equivalent vitrinite reflectance (Fisher et al., 1980); %HRr: mean hydroid random reflectance (%); %VReq: equivalent vitrinite reflectance (%)
based on equation (1) by Bertrand and Malo (2012); Stdev: standard deviation (%); n: number of particles measured; kc: kerogen concentrate; wr: whole rock.

Fig. 7. Relationship between the measured hydroid random reflectance (%HRr), the equivalent vitrinite reflectance (%VReq) determined through the equation as proposed by Bertrand
and Malo (2012) and Hartkopf-Fröder et al. (2015), and equivalent vitrinite reflectance (%Req) according to the %Rr, SCI, temperature and age correlation chart proposed by Fisher et al.
(1980). (A) for the Suèges section samples; (B) for the Caylus section samples; (C) for the Pont de Suert section samples.

(1994) (Table 3). When Req values determined through SCI (Fisher value of Fisher et al. (1980). These data indicate that the majority of the
et al., 1980) are compared with equivalent vitrinite reflectance values samples from the Suèges section are in the immature to early mature
determined through λmax (Mukhopadhyay, 1994), a redshift of the evolution stages (Tissot and Welte, 1984; Hartkopf-Fröder et al., 2015).
fluorescence spectrum data is observed. In most samples the Q ratio These results are in agreement with Rock-Eval pyrolysis published data
ranges between 0.60 and 0.78 which, according to Taylor et al. (1998), for samples from the Marnes de Villeneuve and Schistes Cartons for-
is in agreement with the Req value of Fisher et al. (1980) (Table 3). mations in the Saint-Paul-des-Fonts and Tournadous sections with
Sample S12 is characterized by a lower λmax value (510nm) which does average Tmax values of 425 °C and 426 °C, respectively (Mailliot et al.,
not match with SCI data (Mukhopadhyay, 1994). The Q ratio for this 2009).
sample is 0.53, corresponding to a vitrinite reflectance (Rr) value of For the Caylus section (QB) spectral fluorescence data was acquired
about 0.45% (Taylor et al., 1998), which is consistent with the Req only for samples Cay 26 and Cay 28, which show similar values for both

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parameters - a λmax value of 560nm and Q ratio ranging between 0.59 its identification, with authors having to rely on the texture of the
and 0.60 (Table 4). These values show a good correlation of λmax with particles and the presence of a typical sympodial pattern of growth to
SCI according to Mukhopadhyay (1994). When Req values determined differentiate hydroids from vitrinite. Moreover, hydroid reflectance is
through SCI (Fisher et al., 1980) are compared with vitrinite reflectance still a poorly studied thermal maturity parameter and it is clear there is
values determined through λmax (Mukhopadhyay, 1994), a redshift of the need for further studies for calibration with different rank para-
the fluorescence spectrum is detected, as observed in samples from the meters, in different maturity ranges.
Suèges sections (Table 4). HRr and VReq show a correspondence with
SCI values for most samples, according to Fisher et al. (1980) and 6. Conclusions
Mukhopadhyay (1994) (Fig. 7, B). Samples from the Schistes Cartons
Mb., particularly samples Cay 13 to Cay 26 display lower reflectance This study shows the potential of the use of hydroid reflectance as a
values, with HRr values showing a discrepancy with SCI values. These key thermal maturity parameter in marine sediments, in light of the
inconsistencies could be attributed to sample preparation methods as, new classification system of dispersed organic matter that allows a
in this section, OM reflectance was measured in both whole rock more precise identification of these particles. Furthermore, this paper
(samples Cay1 to Cay10) and kerogen concentrate (Cay 13 to Cay 28). presents the first OM reflectance measurements performed on Jurassic
However, further examination shows that these small variations in HRr hydroids, showing a good correlation with other rank parameters, as
values cannot be assigned to the acid treatment involved in kerogen well as VReq values determined through the equation for conversion of
concentrate isolation because, according to Mendonça Filho et al. hydroid reflectance into equivalent vitrinite reflectance proposed by
(2010), vitrinite reflectance measured in whole rock tends to be lower Bertrand and Malo (2012). Nevertheless, further studies are needed to
than in kerogen concentrate, particularly in low maturity marine se- calibrate the equation for conversion of hydroid reflectance into
diments, and this is contrary from what is observed in samples Cay13 to equivalent vitrinite reflectance for different maturity (and age) ranges
Cay26. Therefore, it is suggested that the lower HRr values are possibly as well as to improve the identification of these particles using organic
related to the higher degree of amorphization that hydroid particles petrographic techniques, particularly in whole rock and kerogen con-
from these samples displayed (Fig. 5, G; Table 4). This same effect of centrate mounts.
degradation in hydroid particles in vitrinite reflectance values was This thermal maturity assessment study shows that the majority of
briefly described by Mendonça Filho et al. (2017) in samples from the the samples from the Suèges (GCB) and Caylus (QB) sections are in the
Cretaceous of Brazil (Parnaiba Basin) and from the Permian of south- immature to early mature evolution stages and that all samples from
west Germany (Saar-Nahe Basin). SCI, fluorescence spectrum and re- Pont de Suert section (PB) are in late mature to early overmature
flectance data indicate that the majority of the samples from the Caylus evolution stages for liquid hydrocarbon generation. Therefore, this
section are in the immature to early mature evolution stages (Tissot and study supports a very similar thermal evolution for the Grands Causses
Welte, 1984; Hartkopf-Fröder et al., 2015). These results correlate well and Quercy basins and an entirely different thermal history for the
with Rock-Eval pyrolysis data of Qajoun (1994) which show a Tmax Pyrenean basin.
value of 420 °-429 °C for samples from the Schistes Cartons Mb. of the
Penne Fm. in the Barrie section. Acknowledgements
The discrepancies between λmax and SCI and Req values for λmax of
560nm observed in both sections may be related to a shift to red wa- This study had the support of the Fundação para a Ciência e
velengths described by Stasiuk (1994) and Araujo et al. (2014) at Tecnologia (FCT), through the strategic project UID/MAR/04292/2013
higher thermal maturities. In the former, the author suggested that the granted to MARE. The authors recognize the team from the Laboratory
proposed correlation between vitrinite reflectance and λmax of of Palynofacies and Organic Facies of the Federal University of Rio de
Mukhopadhyay (1994) is flawed at higher thermal maturities for Pra- Janeiro (LAFO-UFRJ) for their technical support in sample preparation
sinophyte algae, possibly due to differences in fluorescence changes and all geochemical analyses. The authors also acknowledge the valu-
with increasing maturation for the specific type of algae that con- able contributions and suggestions of associate editor Hui Tian and
tributes to alginite. The results of this study seem to point out this reviewers Paul C. Hackley and Thomas Gentzis.
redshift at a more low maturity range (0.42%–0.54% VReq). It should be
taken into account that SCI is a very subjective technique and that OM References
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