Gabin Colombini
email: gabin.colombini@univ-lorraine.fr

Apolline Auclerc
email: apolline.auclerc@univ-lorraine.fr

Françoise Watteau
email: francoise.watteau@univ-lorraine.fr

Techno-moder: a proposal for a new morphofunctional humus form developing on Technosols revealed

Keywords: Microstratification, Litter transformation, Faunal activity, Humipedon aggregation, Anthropized soil, Coal

Human impact on soil systems is now widely acknowledged. "Technosols" appeared in soil classification only a decade ago and the notion of "techno humus system" has emerged even more recently. Yet the variety of humus forms that could develop on Technosol remains largely unknown.

To contribute to filling this knowledge gap, we studied the humus form developing on two Technosols resulting from the activity of a former coking plant and compared it with one developed on a Cambisol as a reference for the area. We used field description and micromorphology on thin sections coupled with a point-and-count method to precisely describe the surface of the humipedons of the area studied.

A total of 13,841 counts and identifications were performed on 11 thin sections and spread into 17 fabric units. Micromorphology on thin soil sections revealed that epi-saprophagous organisms

Introduction

Human activity is profoundly modifying soil systems worldwide. Industry and urbanization lead to a degradation of soil, with either physical, chemical or biological damage [START_REF] Cundy | Brownfields to green fields: Realising wider benefits from practical contaminant phytomanagement strategies[END_REF][START_REF] Mudrák | Understory vegetation in reclaimed and unreclaimed postmining forest stands[END_REF][START_REF] Sheoran | Soil Reclamation of Abandoned Mine Land by Revegetation: A Review[END_REF]Šourková et al., 2005a;[START_REF] Wong | The Restoration and Management of Derelict Land, The Restoration and Management of Derelict Land[END_REF]. Disruption of the soil structure, organic and metallic pollution and a reduction of faunal and microbial biodiversity have been widely reported on post-industrial sites [START_REF] Frouz | Soil biota and ecosystem development in post mining sites[END_REF][START_REF] Ghosal | Particle size-density relation and cenosphere content of coal fly ash[END_REF]. In a time where pressures on soils are rapidly increasing, the rehabilitation of post-industrial sites has become a major concern. In fact, soils are important carriers of ecological functions and ecosystem services, such as carbon storage, water retention and filtration, organic matter recycling and support biodiversity [START_REF] Adhikari | Linking soils to ecosystem services -A global review[END_REF]Millennium Ecosystem Assessment, 2005) and therefore contribute to human well-being, even in anthropized soil systems [START_REF] Morel | Ecosystem services provided by soils of urban, industrial, traffic, mining and military areas (SUITMAs)[END_REF]. Technosols are a new group of soil that was added to the classification by the WRB in 2006. They result from human activities and are defined by incorporating at least 20% technogenic elements or being sealed within the first 100 centimeters of a soil [START_REF] Rossiter | Proposal for a new reference group for the World Reference Base for Soil Resources ( WRB ) 2006 : the Technosols 2 nd revised draft[END_REF]. Technosols are known to present both a wide vertical and horizontal heterogeneity. They might exert extreme physico-chemical properties resulting from their composition such as having high pH, low nutrient content, high carbon content, or high coarse element proportions [START_REF] Joimel | Physico-chemical characteristics of topsoil for contrasted forest , agricultural , urban and industrial land uses in France[END_REF][START_REF] Morel | Soil management and conservation: Urban soils[END_REF]. Technosols undergo pedogenesis processes, that might be faster than one of natural soils such as a formation of macro-and mesoaggregates, an evolution of water retention or decalcification reactions [START_REF] Séré | Early pedogenic evolution of constructed Technosols[END_REF]. Technosols are often found in post-industrial areas and might be left as derelict brownfield or on sites to be reclaimed (Frouz et al., 2006a;[START_REF] Vincent | Assessment of derelict soil quality: Abiotic, biotic and functional approaches[END_REF].

Revegetation of soil is widely used to reclaim post-industrial areas. Besides helping in soil stabilization, it allows the incorporation of neo-formed organic matter, resulting from roots, barks, twigs or senescent leaves of the plants, which is involved in soil fertility and support faunal and microbial diversity [START_REF] Bradshaw | Restoration of mined lands-using natural processes[END_REF][START_REF] Tiessen | The role of soil organic matter in sustaining soil fertility[END_REF]. In some cases, authors have suggested the natural succession of spontaneous vegetation to be an equally efficient way to reclaim ecological functioning of degraded soil (Frouz et al., 2006b). Whatever the strategy used, it is important to assess the recovery of pedological processes such as the dynamics of organic matter or the formation of soil structure on degraded areas. One way to assess this recovery is to study the evolution of the neoformed organic matter and its interactions with the initial soil components (Gillet and Ponge, 2002;[START_REF] Rabot | Soil structure as an indicator of soil functions: A review[END_REF].

These interactions between biotic and abiotic components occur in a part of the soil system named the humipedon, corresponding to the OL, OF, OH and A horizons (Zanella et al., 2017a). This compartment houses complex interactions between microorganisms, soil fauna, roots, decaying organic matter or mineral constituents. Depending on the biotic and abiotic components of the humipedon, different layers or horizons will develop over time and space, depending on the varying nutrient and energy cycling dynamics [START_REF] Ponge | Plant-soil feedbacks mediated by humus forms: A review[END_REF]. The ability of soil fauna, such as earthworms to colonize or thrive in a given environment has been reported as one of the main drivers in the morphological organization of the humipedon, in slightly [START_REF] Bernier | Humus form dynamics during the sylvogenetic cycle in a mountain spruce forest[END_REF] to highlyanthropized soils [START_REF] Ghosal | Particle size-density relation and cenosphere content of coal fly ash[END_REF]. Plant litter may accumulate on the soil surface, be consumed and transformed into feces by soil saprophagous organisms, or mixed with mineral material when consumed by anecic earthworms. This morphological organization of the humipedon thus depends on the chemistry of the organic matter, the climate, the bedrock properties and the community of soil fauna and microorganisms [START_REF] Barratt | A revised classification and nomenclature of microscopic soil materials with particular reference to organic components[END_REF]. Such interactions drive physical parameters such as organo-mineral aggregation, the size and shape of the porosity, as well as participating in the functions provided by the soil profile. Thus, the spatial organization and morphology of the constituents in the humipedon can provide useful information on the functioning of the ecosystem [START_REF] Ponge | Plant-soil feedbacks mediated by humus forms: A review[END_REF]. This morpho-functional organization is called "humus form" and is defined as a "reference for a group of humus profiles displaying the same series of diagnostic horizons", according to Zanella et al. (2017b).

It has been described in little anthropized ecosystems for decades [START_REF] Barratt | A revised classification and nomenclature of microscopic soil materials with particular reference to organic components[END_REF] and its classification is still evolving. Forms such as "Para" and "Anthropogenic" have recently been added (Zanella et al., 2017c). Para-humus systems are driven by specific ecological determinants such as bryophytes, roots or even biological crusts (Zanella et al., 2018a), while Anthropogenic, or "techno" humus system result from human activities (Zanella et al., 2018b).

One way to characterize the humus form developing on the soil surface is the use of thin-section micromorphology. This is based on a morphological classification of the organic material and minerals developing in a natural ecosystem that forms humus layers [START_REF] Bal | Micromorphological analysis of soils. Lower levels in the organization of organic soil materials[END_REF][START_REF] Bal | Morphological investigation in two moder-humus profiles and the role of the soil fauna in their genesis[END_REF] and fits the identification of humus form resulting from natural pedogenetic processes, as shown by [START_REF] Zaiets | Use of micromorphology for humus characterization and classification in some mediterranean calcareous soils[END_REF] on Mediterranean soils. Furthermore, it allows a discrimination between neo-formed and anthropogenic soil components [START_REF] Stoops | Guidelines for Analysis and Description of Soil and Regolith Thin Sections[END_REF] and this method is well-adapted to Technosols, even when the heterogeneity and diversity of components can render the task arduous [START_REF] Stoops | Interpretation of micromorphological features of soils and regoliths[END_REF]. In fact, micromorphology has already been used to identify Technosol constituents [START_REF] Monserie | Technosol genesis: Identification of organo-mineral associations in a young technosol derived from coking plant waste materials[END_REF] and to study pedogenetic processes, such as organic matter dynamics, soil porosity evolution, the impact of faunal activity or physical properties, such as hydric conditions [START_REF] Watteau | Micropedology to reveal pedogenetic processes in Technosols[END_REF][START_REF] Watteau | A micromorphological analysis for quantifying structure descriptors in a young constructed Technosol[END_REF].

So far, Technosol studies using humus form identification are scarce, probably because Technosols resulting from industrial activities are a young entity of study, while humus form investigation requires a time scale sufficient for neo-formed organic matter to evolve (Zanella et al., 2017b).

Because of their high carbon content, some studies have already focused their interest on the morphological assessment of soil organic matter on anthropized soils (Abakumov et al., 2014;[START_REF] Frouz | Soil biota and upper soil layer development in two contrasting post-mining chronosequences[END_REF][START_REF] Frouz | Development of soil microbial properties in topsoil layer during spontaneous succession in heaps after brown coal mining in relation to humus microstructure development[END_REF][START_REF] Huot | Diversity and activity of soil fauna in an industrial settling pond managed by natural attenuation[END_REF]. However, only two studies have proposed the notion of « techno humus », although with two different definitions [START_REF] Markiewicz | Characteristics of soil organic matter of edifisols -An example of techno humus system[END_REF]Zanella et al., 2018b). While these two papers have open a door for an integrated view of both Technosols and humus systems, the relationships between technogenic elements and humus form development on Technosols still require much more attention.

In this vein, the aim of this paper is to identify and classify the humus form developing on Technosols of a former coking plant area, using micromorphology to assess the recovery of pedogenetic processes on the site. We hypothesized that (i) the succession of diagnostic horizons of Technosol humipedons would not follow the one described in the already existing humus form classification and (ii) that soil fauna footprints would be limited or absent since technogenic elements constitute most of the soil matrix and would not suit their requirements. By coupling a Technosol profile study and micromorphological analysis of thin sections, the vertical organization and interaction of anthropogenic and neo-formed organic constituents of the humipedon will be described. The identification and classification of humus form developing on Technosols as a promising way to assess thel recovery of soil processes such as organic matter decomposition and soil aggregation after rehabilitation on post-industrial areas is discussed.

Materials and methods

Localization and properties of the study sites

The study area is located on the former coking plant of Homécourt, in north-eastern France, on the group of scientific interest for soil study (GISFI) experimental station at Homécourt (www.gisfi.univlorraine.fr). The ceasing of the plant's activity in 1985 was followed by an embankment of a 3 ha site, composed of a mix of coking plant by-products, building residues, and industrial ground and left derelict since, resulting in derelict spolic Technosols. This area is mainly covered by Populus tremula (L.), Robinia pseudoacacia (L.) and Betula pendula (L.) that developed spontaneously. Two forest stations (20 m x 20 m) were selected for morphological study of the humipedon at the surface of the Technosols (stations T1 and T2, Fig. 1). In order to compare the surface of the humipedon of the Technosols with a reference, we added a woodland station located near the former coking plant (Station A, Fig. 1). This station is dominated by Acer campestre (L.) and Fraxinus excelsior (L.) and is developing on a Cambisol. This station was chosen as the local reference of humus form developing in the area because it resulted from (i) the action of the soil fauna community (ii) in a soil resulting from pedogenetic processes occurring on the natural bedrock and (iii) under a spontaneously developed vegetation. Thus this forest station might represent a potential sink for soil fauna colonization toward the Technosols. The samples for chemical analyses across all stations were collected between the 25 th and the 30 th of April, 2018. For each station, five soil samples were taken to a depth of 20 cm for abiotic characterization corresponding to soil chemical and physical analyses. At each sampling point, four 500 g soil samples, taken from the first 0-20 cm soil layer, were pooled into one composite sample. Prior to analyses, soils were air-dried for 72 h then sieved at 2 mm. The size of each sample were reduce homogeneously to 500 g using an open-bin riffle splitter [START_REF] Schumacher | Comparison of Three Methods for Soil Homogenization[END_REF], then divided into two homogenous samples using a rotary splitter coupled with a vibratory feeder with a Vshaped channel (Laborette 24, Fritsch). One sample was kept in the laboratory for chemical analyses and the other was sent for particle size distribution. Table 1 shows the physico-chemical properties of the soils from each studied stations.

Description of the humipedons

In September 2018, one soil pit was opened to a depth of 1 m wherever possible on each station and a description (i.e. depth of each horizon, nature and origin of the organic and mineral constituents) of each humipedons' horizons was made.

In order to describe the humus form developing on the humipedon of each station of the former coking plant area, eleven undisturbed soil samples were taken vertically using Kubiena boxes (9 × 6 cm) at the soil surface and distributed as follow: 4 boxes on Station A (Aa, Ab, Ac, Ad), 3 on Station T1 (T1a, T1b, T1c) and 4 on Station T2 (T2a, T2b, T2c, T2d). From each Kubiena box, one thin soil section (20 µm thick) was prepared according to the protocol developed by [START_REF] Guilloré | Méthode de fabrication mécanique et en série des lames minces[END_REF] and [START_REF] Murphy | Thin section preparation of soils and sediments[END_REF].

Two types of analyses were carried out on these thin sections: (i) a general description of the micromorphological features such as microstructures, voids, organic materials and minerals, or technogenic elements for at least one thin soil section of each station, following Stoops, (2003) to reveal 4 contrasting situations (1 from Station A, 1 from Station T1 and 2 from Station T2); (ii) pointcounting observations to quantify the proportion of the micromorphological features, conducted on the 11 thin sections. In total, 17 fabric units, as explained below, were used to describe the 11 thin sections.

Based on the works of [START_REF] Babel | Micromorphology of Soil Organic Matter[END_REF], [START_REF] Stoops | Guidelines for Analysis and Description of Soil and Regolith Thin Sections[END_REF] and [START_REF] Zaiets | Micromorphology of organic matter and humus in Mediterranean mountain soils[END_REF], 9 fabric units were used: pore, leaf fragment, other plant tissue, root, fungi, macro-arthropod dropping (> 200 µm), mesofaunal dropping (< 200 µm), earthworm cast and fine organic material (FOM). We followed the definition of "organic fine material" given by [START_REF] Zaiets | Micromorphology of organic matter and humus in Mediterranean mountain soils[END_REF] adapted from [START_REF] Stoops | Guidelines for Analysis and Description of Soil and Regolith Thin Sections[END_REF] which is in short: "organic material with no recognizable origin, including groups of five or less interconnected cells, amorphous organic fine material, punctuations and organic pigment in the inorganic micromass." We also added a "particulate organic matter" (POM) fabric for groups of 5 or more interconnected cells, without organic o-plasma sensu [START_REF] Bal | Micromorphological analysis of soils. Lower levels in the organization of organic soil materials[END_REF] and with no recognizable origin. We added a "animal tissue" fabric for the few animal parts that can be encountered on thin section, such as external skeletons [START_REF] Stoops | Guidelines for Analysis and Description of Soil and Regolith Thin Sections[END_REF].

As additional fabric units, we distinguished fine minerals (< 2 mm) from coarse minerals (> 2 mm) and we added 4 fabric units in order to highlight Technosol specificities. The two first were organic, namely fine (< 2 mm) and coarse (> 2mm) coal fabric units that referred to coal, charcoal by-products and coal fly ashes, likely to be found in the humipedon of a former coking plant area. Examples of these micromorphological features can be found in [START_REF] Stoops | Interpretation of micromorphological features of soils and regoliths[END_REF]. The 2 remaining fabric units that we added to our study were fine (< 2 mm) and coarse (> 2mm) mostly mineral, technogenic artefacts and refer to all other features resulting from or added by human activity such as brick or glass fragments, cement blocks or individualized cement constituents.

The point and count method is usually carried out for each horizon in natural soils [START_REF] Zaiets | Micromorphology of organic matter and humus in Mediterranean mountain soils[END_REF] or each centimeter in anthropized soils [START_REF] Frouz | The effect of earthworms and other saprophagous macrofauna on soil microstructure in reclaimed and un-reclaimed post-mining sites in Central Europe[END_REF] where pedogenetic processes may not have yet separated proper horizons. As we studied Technosols, the second method was chosen.

Because the number of counts per thin section varied in the literature and at least 300 were performed [START_REF] Zaiets | Micromorphology of organic matter and humus in Mediterranean mountain soils[END_REF], we counted 1200 points for each thin section, divided into about 200 points (mean = 210, SD = 13, n = 66) for each of the 6 cm of the 11 thin sections.

The point and count method was conducted under a stereomicroscope (MZ FLIII, Leica), using a x16 to x200 magnification. A transparent plastic sheet pierced with 1200 holes along the parallel lines of the thin sections was placed on top of the thin sections. We used an eyepiece reticle to classify the component under the crosshairs inside one of the 17 fabric units described above. In order to avoid a misinterpretation of a feature on the sides of the thin sections, where the thickness of the sample could slightly decrease (edge effect), we moved the grid and counted again until the adequate number of observations was reached.

For a given thin section, the result was expressed as a proportion of each fabric unit within each centimeter, using the following formula:

Proportion X= 𝐶𝑜𝑢𝑛𝑡 𝑋 𝑐𝑎𝑡𝑒𝑔𝑜𝑟𝑦 𝑇𝑜𝑡𝑎𝑙 𝑐𝑜𝑢𝑛𝑡 x 100
With « count X category» being the number of counts of the category X within a given depth of a given thin section and « total count » the total number of points counted within the same depth of the thin section.

Multivariate and statistical analyses

To compare the morphological composition of the 11 studied humipedons, a principal component analysis (PCA) was performed using the dudi.pca function of the ade4 package in R software (version 1.1.383, 2017). This was performed using the proportion of each fabric within each centimeter of the thin sections. Correlations between variables and dimensions of the PCA were obtained using the dimdesc() function of the FactoMineR package using one way analysis of variance (ANOVA) to test for statistically significant correlations (p-value ≤ 0.05).

Results

Humipedon description on the macroscale

The three soil profiles are shown in Fig. 1. The vertical organization of the stations were highly heterogeneous.

At the Station A, the OLn layer was composed of Acer campestre and Fraxinus excelsior leaves and represented less than 1 cm. The soil profile was composed of a 20 cm thick A organo-mineral horizon on top of a 10 cm B horizon, laying on a calcareous bedrock.

At the T1 station, the profile was composed of 0.5 cm thick OLn and OLv layers, mostly of Robinia pseudoacacia and Salix caprea, a 2 to 5 cm thick OF layer including fragmented leaves of R. pseudoacacia, herbaceous leaf sheaths and a few wood fragments. The 2 cm thick OH layer was composed of a mix of fecal pellets and fine black coal particles. Underneath these organic layers laid a 50 cm thick technic (carbonic) soil material, composed of fine and blocky coal elements.

At the T2 station, the profile was composed of a 1 cm thick OLn and OLv layer, with Populus tremula leaves and a few Betula pendula and Salix caprea leaves. The 1 cm thick OF layer was composed of leaves of the previously-cited tree species, as well as wood and bark fragments. The 3 to 5 cm thick OH layer was mainly composed of dark colored fecal materials. The underlying horizon was heterogeneous at the profile scale (Fig. 1). A 20 cm thick AB organo-mineral brown horizon (Munsell code 7.5YR 4/4) varied laterally toward a black technogenic horizon (Munsel code 10YR 2/1) and with 50 to 70% blocky elements. This horizon laid upon a 10 cm thick concrete slab underneath which was found 1 m of technogenic embankments, composed of coal by-products, gravels and bricks.

Humipedons' description at the microscale

The general description of the microstructures of 4 thin sections (1 from Station A, 1 from Station T1 and 2 from Station T2) are shown in Table 2. The depth, continuity and boundary of the layers were measured and described according to the evolution of the main morphological features: microstructure and porosity, organic components, soil fauna excrements, mineral material and technogenic material.

Scans of soil thin sections of the three stations and examples of morphological features such as macro and mesofaunal droppings, roots, fine and coarse coal particles or fine and coarse technogenic artefacts are shown in Figures 2 to 4.

Following the point and count method, a total of 13.841 identifications were made on the 11 thin sections according to the 17 chosen fabric units. Barplots were drawn following the proportion of each unit (Fig. 5, S1 and S2). Figure 5 showed the proportion of each of the 17 fabric units within the 11 thin sections. For the second barplot (Fig. S1), we pooled the fabric units into one of the following four categories: organic component, mineral component, Fine Organic Matter (FOM) and anthropogenic component. We separated FOM from organic components, because FOM usually describes organic material aggregated with the inorganic micromass. At the magnification of the study, minerals < 20 µm are hardly recognizable, so pooling FOM and organic component would have led to an imbalance between organic and mineral components. Anthropogenic components might be either organic (coal and coal by-products) or mineral (building block residues, cements), but the addition of this category might be useful in order to highlight the relationships between anthropogenic components and neo-formed organic material. The four categories combined together represent 100% of the solid volume of a given thin section. The third barplot (Fig. S2) represents the proportion of each fabric of neo-formed organic matter as a proportion of the total organic component as described above.

Description of humipedon of each station

Humipedon of the Cambisol on Station A

The 4 thin sections of Station A were composed of a total of 24 layers of 1 cm (Fig. 5). The main constituents of the solid fraction of Station A were FOM, fine mineral, fine coal, and earthworm casts.

They constitute 50 to 75% of the overall volume. These constituents were aggregated and formed a crumb microstructure (Table 2).

The most abundant morphological feature in this station was FOM. This represented more than 30% of the solid volume in 21 out of the 24 layers and more than 55% of the organic matter in 19 out of 24 layers of the 4 thin sections and reached 83% in Ac thin section. Earthworm casts varied from 0 to 11.8% of the overall volume of the surface of the humipedon and welding of ageing earthworms' casts was visible. Casts were mostly composed of FOM and fine minerals, as well as fine coal fragments embedded in the inorganic micromass. Coarse minerals never exceeded 0.9% of the overall volume, while fine minerals could reach 16.7%. Roots were present in each layer of the 4 thin sections studied and their morphology attest that they were living. Mesofaunal features such as biogenic aggregates were visible, as indicated by the presence of mesofaunal droppings smaller than 200 µm within macroaggregates, leading to small dropping infillings. Only a few animal parts were found on the thin sections, and reached a maximum of 1.0% of the overall volume of the 2-3 cm layer of the Ab thin section with the presence of snail exoskeletons. Visible fine minerals were mostly composed of fine quartz grain. No coarse coal was found in any layer of the 4 thin sections of this station. Yet, the fine coal microfeatures were present in every one of the 24 layers. Their proportion reached 22.8% of 5-6 cm layer of the Aa thin section and was greater than 10.0% in 19 out of the 24 layers.

Humipedon of the Technosols on stations T1 and T2

Fragments of leaves represented 14.1 to 21.1% of the overall volume of the first layer of the humipedon sampled in station T1 and 10.3 to 16.3% for the one of the T2 stations. On neither of the stations did the leaf fragments show much decomposition and presented a laminated microstructure (Fig. 3-b and4c-d). Other plant tissues were mostly woody, such as barks and twigs and represented 12.2 to 18.9% of the overall volume of the first layer of the humipedon from the station T1 and 7.5 to 14.9% for the one of the T2 stations. Such observations confirmed the diagnosis of the OLn and OLv layers.

Below this first layer, a crumb microstructure was observed with compound packing voids between mesofaunal feces and fine coal particles. Mesofaunal feces could represent up to 17% and 24% of the volume of the humipedon at depths between 1 cm and 3 cm while, at the same depth, the macrofaunal feces could represent 24% and 8% of the overall volume of stations T1 and T2, respectively. The fine coal particles represented up to 42% of the overall volume of the fractions on both stations. Multiple morphological features of organic matter occurred within the same layer in Technosol humipedons including neo-formed organic matter such as macro-and mesofaunal feces and fragmented shoot materials or technogenic organic matter such as coal particles. Yet little to no aggregation was found between the two categories of components (Fig. 3c, 4e-f). The only aggregation of these two component categories occurred in feces of invertebrate macroarthropods such as diplopods, in which neo-formed OM and coal particles were packed.

A morphological feature that differed between the two stations was the mycelium. The presence of mycelium was observed in 24 out of 24 layers of the T2 station, while only occurring in 5 out of 24 layers in station T1. Quantitatively, mycelium represented up to 8.1% of the overall volume in the 2-3 cm layer of the T2b thin section, while never exceeding 1.5% of the humipedon at the T1 station, all thin sections considered. The high proportion of meso-and macrofaunal feces on top of the humipedon, together with fungi mycelium and a rapid decrease in the proportion of leaf fragments were all morphological criteria of a OF and a zOH layers. The evidence of the zoological nature and genesis of the OH horizon, namely the epi-saprophagous feces, allowed it to be specified as a "zOH".

The porosity tended to decrease with depth in the thin sections, falling by 2.7 fold on average between the first and the deepest layers of the T1 station and by 1.7 fold on average on the T2 station (Fig. 5).

The proportion of technogenic elements showed an inverted trend to that of porosity and reached 75% of the solid volume at a depth of 6 cm (Fig. S1). Most of the technogenic elements were either fine or coarse coal fragments. A peculiar situation was found in the T2b thin section, in which the only technogenic elements were coarse and centimetric embankments, probably residuals of building blocks, while no coal particles were visible. T2b thin sections exhibited the thickest layers of neoformed organic-matter, most of which was composed by both macro-and mesofaunal feces. In fact, within the 4 first cm of this soil thin section, 28 to 35% of the overall volume consisted of faunal excrement, representing more than 50% of neo-formed organic matter (Fig. 5 andS2). The proportion of minerals in the solid volume of Technosol humipedons were below 10% in 38 out of the 42 layers studied for both stations T1 and T2, (Fig. 5), without considering the minerals linked to organic matter in the FOM fabric unit. According the presence of roots in the deeper layers of the thin sections composed mostly of anthropic material (Fig. 3e-f), roots seemed to be able to grow within this technogenic horizon and might be decomposed by soil fauna as revealed by the accumulation of excrement within some decaying roots (Fig. 4f).

Multivariate analysis

The PCA performed with the proportion of every fabric unit in the 66 layers is shown on Figure 6. The first 2 axes of the PCA explained 47.1% of the total inertia. The statistically significant correlations between each variable and the first two dimensions of the PCA are shown in Table S1.

On the right of the first axis, variables such as percentage of particulate organic matter, meso-and macrofaunal feces, leaves and plant tissues, as well as mycelium percentage in a given humipedon, covaried and were negatively correlated to the percentage of earthworm casts, fine organic matter and fine minerals in the humipedon. Soil surface components such as earthworm casts, leaves and plant tissues and the high porosity percentage in a given humipedon were positively correlated with the second dimension of the PCA. The variables that were negatively correlated to this second dimension are the 4 technogenic components found in the humipedon of the coking plant area, such as coal and technogenic artefacts.

The humipedon of Station A showed little evolution in the morphology of its components with depth, except a decrease in the porosity and earthworm cast quantity. In contrast, the T1 and T2 stations shared a similar trend in the evolution of the morphological features and were characterized by specific sets of variables at each depth (Fig. 6b). The first centimeters were characterized by porous layers, mostly composed of organic matter originating from the shoot part of the vegetation developing on the Technosol, such as leaf fragments or plant tissue. Then, from 1 to 4 cm, a layer was composed of neo-formed organic matter, transformed by soil fauna as indicated by the positive correlation of meso-and macrofaunal feces, together with fungi mycelium and particulate organic matter. The deepest layers were mostly composed of technogenic elements such as artefacts, fine and coarse coal.

Discussion

Classification of the humipedon humus forms on the former coking plant

At the time of the study, the morphological organization of the organic matter of the humipedons clearly indicated two different humus forms between the forest stations developed on the two Technosols studied in comparison with that on Cambisol. Indeed, the first dimension of the PCA allowed discrimination between the morphology and the size of the neo-formed organic matter that composed the humipedon of Station A and from that of the two Technosol stations (T1 and T2) of the coking plant area.

Humus form of the Cambisol from station A

The morphological features of the humipedon developed on Station A, observed in the 4 thin sections are typical of an eumull according to the classification of [START_REF] Zanella | A European morpho-functional classification of humus forms[END_REF]. The macroaggregates composed of a mix of fine organic matter and fine minerals is a key feature of the mull and can be diagnostic as a macroA horizon, formed by macroaggregates greater than 4 mm (Zanella et al., 2017d). The soil pH above the threshold of 5 confirm the diagnostic horizon proposed by Zanella et al. (2017d). The slight changes in the morphological features type with increasing depth, revealed by the second axis of the PCA, may result from the mixing activity of burrowing earthworms in this forest [START_REF] Lavelle | Soil function in a changing world: The role of invertebrate ecosystem engineers[END_REF]. The welding of casts with ageing has been described by [START_REF] Bal | Morphological investigation in two moder-humus profiles and the role of the soil fauna in their genesis[END_REF] and is coherent with the observation of welded structures on the thin sections studied. Furthermore, the observation of numerous mesofauna excrement in the casts have also been reported in the mull humus form in natural forests, as earthworm casts and macroaggregates are sources of carbon and nutrients for enchytraeids or collembola [START_REF] Bal | Morphological investigation in two moder-humus profiles and the role of the soil fauna in their genesis[END_REF][START_REF] Salmon | The impact of earthworms on the abundance of Collembola: improvement of food resources or of habitat?[END_REF].

Thanks to the precision of micromorphology, our results showed that fine coal particles are present in anecic earthworms casts from Station A, while they were not visible to the naked eye during field description. Thus, according to the classification proposed by [START_REF] Jabiol | A proposal for including humus forms in the World Reference Base for Soil Resources (WRB-FAO)[END_REF], this humus form is an Haplic eumull (technic) on Cambisol. The prefix "Haplic" indicates that no other prefix proposed in the classification fits the humus form, while the suffix "technic" indicates that the diagnostic horizon A contained at least 10% of anthropic artefacts. Even though the microprofiles of Station A seemed homogeneous, micromorphological analysis of humipedon thin sections allowed precise classification and anthropization traces to be revealed. The consumption of fine coal particles by earthworms have been described in other ecosystems, notably in cultivated land in Amazonian rain forest, where Pontoscolex corethrurus mixed separated charcoal with organo-mineral aggregates [START_REF] Ponge | Ingestion of charcoal by the Amazonian earthworm Pontoscolex corethrurus : a potential for tropical soil fertility[END_REF]Topoliantz andPonge, 2003, 2005). In our sites, these particles are probably coal fly ashes, known to be generated by coking plants [START_REF] González | Fly ashes from coal and petroleum coke combustion: Current and innovative potential applications[END_REF]. Deposits of fly coal ashes would be carried by the dominant west-wind of the region, while Station A is located east of the former coking plant (Fig. 1). The coal particles observed in the thin sections were smaller than 200 µm (Figs. 2 and5) which correspond to the range of sizes described by [START_REF] Ghosal | Particle size-density relation and cenosphere content of coal fly ash[END_REF] for ashes resulting from the burning of different coals. The mull humus form and the soil fauna footprints in the Cambisol developed on Station A, indicate that the coking plant activity has not impacted nearby ecosystems sufficiently to prevent an earthworm community from developing.

Humus form of the T1 and T2 station Technosols

Considering the humipedons of the 2 Technosols studied, the evolution of soil organic matter's morphological features with depth appears to be analogous to a moder form of humus according to the classification of [START_REF] Zanella | A European morpho-functional classification of humus forms[END_REF]. The moder humus form is composed of poorly decomposed plant material resulting from the activity of diplopods, isopods, collembola, enchytreids or oribatid mites and from the absence of anecic earthworms [START_REF] Bal | Morphological investigation in two moder-humus profiles and the role of the soil fauna in their genesis[END_REF]. In temperate regions, an absence of anecic earthworms is caused by low soil pH or sandy texture causing a poor water regime. In the case of the studied Technosols, the high sand content together with the low water holding capacity might explain the absence of earthworm's footprints. While the moder stricto sensu is composed of the same ectorganic horizons OL, OF and zOH that we found in this study, it is also characterized by its underlying horizon, which is an organo-mineral A horizon, that is generally meso-or micro-structured (Zanella et al., 2017e). Mixes of neo-formed organic matter with underlying horizons have been widely reported in moder on natural soil systems, attributing a significant role to enchytraeids [START_REF] Ponge | Humus forms in terrestrial ecosystems: A framework to biodiversity[END_REF]Zanella et al., 2017b). On the T1 and T2 stations, the underlying horizons differed from this definition, being mainly composed of fine coal embankments or coarser technogenic artefacts that represented 55 to 89% of the solid volume at a 5 to 6 cm depth. In contrast to the station A humipedon, fine coal particles had not been incorporated into organo-mineral aggregates, but constituted most of the groundmass, resulting in a technogenic horizon with a granular structure. The high TOC concentration and the high C to N ratio measured in the Technosols result directly from the nature of the substrate used as embankments. The high pH values found for the Technosol are not surprising as a slight alkalinity is often described in Technosols literature [START_REF] Joimel | Physico-chemical characteristics of topsoil for contrasted forest , agricultural , urban and industrial land uses in France[END_REF], although the development of ectorganic horizons occurs generally on acidic soils [START_REF] Andreetta | Microbial dynamics in Mediterranean Moder humus[END_REF][START_REF] Bernier | Hotspots of biodiversity in the underground: A matter of humus form?[END_REF][START_REF] Bernier | Humus form dynamics during the sylvogenetic cycle in a mountain spruce forest[END_REF][START_REF] Toutain | Activité biologique des sols, modalités et lithodépendance[END_REF]. A neutral to slightly alkaline horizon underlying an ectorganic one does not fit the actual classification, yet could occur frequently on Technosols. Finally, saprophagous activity had induced the mixing of feces and fine coal particles within the same depth, leading to a transitory boundary between neo-formed and technogenic horizons as revealed by the second axis of the PCA. The reason for the low proportion of mycelium found in the thin sections of the T2 station is still unclear, but could result from a higher grazing activity of the mesofauna, as may be inferred from the higher proportion of mesofaunal feces in the T2 station than in T1.

On the basis of the diagnostic horizons that we observed in the Technosols humipedons, we would like to propose the term "techno-moder" to characterize this new humus form within the "techno humus system" of the European morpho-functional classification proposed by Zanella et al. (2018b).

According to the above-mentioned classification, the humus form present in the thin sections of the Technosols humipedons are techno-dismoder, as zOH horizons were > 1 cm, except in T1c thin-section. We think that keeping the term "moder" is important because it comes from « vermoderung » as proposed by [START_REF] Kubiëna | Bestimmungsbuch und Systematik der Böden Europas[END_REF] to describe the consumption of plant litter by soil fauna without mixing this organic matter with minerals. This is the case for the Technosols studied here and it is highlighted by the composition of the meso-and macrofaunal feces, which are either holoorganic or are, to some extent, mixed with fine technogenic material. The prefix "techno" would be used to indicate that the evolution of neo-formed organic-matter occurred on a diagnostic technogenic layer, in the absence of an A horizon. We think that the addition of subsystems within the "techno humus system" could allow specific soil-plant-fauna interactions to be highlighted in the same manner it has been done in natural ecosystems [START_REF] Zanella | A European morpho-functional classification of humus forms[END_REF]. When looking at the classification proposed by [START_REF] Jabiol | A proposal for including humus forms in the World Reference Base for Soil Resources (WRB-FAO)[END_REF] within the World Reference Base for soil resources, the humus form described in this study would be a Hyperspolic techno-moder on Technosol for the 3 profiles from Station T1 and 3 out of 4 profiles from Station T2. The Hyperspolic prefix indicates that the diagnostic horizons, here the organic and technogenic horizons, contain at least 75% artefacts, with 35% or more of industrial waste. The only exception found on the T2b thin section would be described as a techno-moder (urbic) on Technosol. The suffix "urbic" indicates that the diagnostic horizons, contain at least 25% artefacts, with 35% of them being rubble and refuse from human settlements. The addition of "techno" to the qualifier "moder" would be necessary in this case for two reasons. Firstly, the prerequisite for the moder humus form is not met, i.e. the absence of an organo-mineral horizon underlying the ectorganic ones and the presence of a slightly alkaline technogenic horizon. Secondly, the parahumus system could fit the morphological diagnostic, but this would reduce the amount of information regarding the vertical organization of the organic matter and mask the animal activity, revealed by micromorphology.

Consideration of the humus form on Technosols as a tool to assess the recovery of ecological processes on the coking plant area

In 2002, Ponge et al. proposed the humus index as an integrated tool to assess the properties of the topsoils in a little anthropized forest ecosystem and in 2018, Korkina and Vorobeichik showed the humus index to be an effective indicator of the impact of metal pollution on topsoil fauna communities [START_REF] Korkina | Humus Index as an indicator of the topsoil response to the impacts of industrial pollution[END_REF][START_REF] Ponge | Humus index: An integrated tool for the assessment of forest floor and topsoil properties[END_REF]. In post mining sites, Šourková et al. (2005b) proposed the formation of the organic layers to be an indicator of the recovery of ecological functions.

Such previous studies have already suggested interesting responses of the humus form to human activities that can be assessed from the soil profile to the microprofile scale, using microstratification.

The PCA allowed us to discriminate the constituents of the humipedons of the Cambisol and Technosols according to the morphology of the organic matter and consequently to reveal its evolution within a given humipedon with depth. From a functional point of view, the vertical and gradual stratification of the Technosol humipedons indicates that pedogenesis is currently occurring and is driven jointly by soil animal activity, although without the participation of anecic earthworms, and also by roots and shoots that appeared to be an important source of neo-formed organic matter. The morphology of the organic matter in these Technosols suggests a limitation of the bioturbation process when compared with the Cambisol, as highlighted by the accumulation of arthropods feces on the soil surface of the techno-moder and the negative correlation of fine organic matter with arthropods feces.

While the observed humus form developed on Technosols differed micromorphologicaly from the reference used in our study, our results suggest that neo-formed organic matter allowed an epigeic soil fauna community to colonize the Technosols stations. The techno-moder form developing on Technosols could highlight an ecological strategy allowing plants, soil fauna and microorganisms to cope with extreme environments, as suggested by [START_REF] Ponge | Humus forms in terrestrial ecosystems: A framework to biodiversity[END_REF], but this hypothesis is still to be tested. Following the evolution of the humus form of the studied Technosols could represent a promising way to understand humus form resilience on highly anthropized soils.

Usefulness of micromorphology for humus form classification on Technosols

Micromorphological analysis of soil thin sections appears to be particularly well adapted to the study of the vertical organization of the Technosol humipedon constituents, following the microstratification developed by [START_REF] Ponge | Etude écologique d'un humus forestier par l'observation d'un petit volume, premiers résultats. I. La couche L1 d'un moder sous pin sylvestre[END_REF], who described a moder humus under a Pinus sylvestris forest station. The use of thin sections, coupled with a point and count method allows a semi-quantitative evaluation of the proportion of each fabric unit composing Technosol humipedons. In addition to field measurements, the two-scale approach of the humipedon allows complementary information to be gathered, which is useful for humus form classification. Precise localization and identification of soil fauna fecal material can be made using thin sections and thereby provide relevant information as to the interactions between specific taxa and their environment [START_REF] Bal | Morphological investigation in two moder-humus profiles and the role of the soil fauna in their genesis[END_REF]. The nature and origin of the morphological features can be determined precisely using the classification developed by previous authors for natural soils [START_REF] Stoops | Guidelines for Analysis and Description of Soil and Regolith Thin Sections[END_REF][START_REF] Zaiets | Use of micromorphology for humus characterization and classification in some mediterranean calcareous soils[END_REF]. However, in the case of humipedon developed on Technosol, additional fabric units are required in order to cover the whole spectrum of the constituents that can be encountered. In our case, the "fine and coarse coal" fabric unit appeared to be a required fabric unit on a former coking plant and allow discrimination between those site-specific features from other anthropogenic artefacts [START_REF] Howard | Composition, micromorphology and distribution of microartifacts in anthropogenic soils[END_REF]. In the case of Technosols high spatial heterogeneity, micromorphology on thin sections can highlight peculiar situations and specific links between neo-formed organic matter and parent technogenic material, such as the lack of aggregation between technogenic coal by-products and neo-formed organic matter.

Conclusion

Micromorphology have been shown to be a relevant tool for describing humus forms developing on Technosols. Our study has allowed the description of a new humus form that had developed on the humipedons of a former coking plant and led us to propose the name "techno-moder". Footprints of specific soil fauna taxa revealed by micromorphology, as well as the identification and composition of diagnostic horizons are key elements required for the classification of humus form and help the description of current ecological processes occurring on Technosols. We think that an addition of details to the current "techno humus system" label is the next step toward an integrative understanding of anthropic activities and soil ecological processes such as organic matter transformation and bioturbation. Moreover, in a context of increasing anthropic pressure on soil systems, the capacity to

Figure 1 :

 1 Figure 1: Aerial view of the former coking plant area of Homécourt with the localization of the 3 study

Figure 2 :

 2 Figure 2: Main microstructure and pedofeatures of the humipedon of the station A. (a) and (d)

Figure 3 :

 3 Figure 3: Main microstructure and pedofeatures of the humipedon of the station T1. (a) and (d)

Figure 4 :

 4 Figure 4: Main microstructure and pedofeatures of the humipedon of the station T2. (a) and (d)

Figure 5 :

 5 Figure 5: Percentage distribution of each morphological features within the first 6 cm of each thin

Figure 6 :

 6 Figure 6: PCA of the proportion of every fabric unit at the 6 depth of the 11 thin sections.

Figure 1 Figure

 1 Figure 1

Figure 6

 6 Figure 6

Acknowledgments

The authors would like to thank the GISFI (gisfi.univ-lorraine.fr) members, especially the technical staff, namely Adeline Combat and Yannick Cazes for the access to the study sites, as well as Jean-Claude Begin for the preparation of the soil thin sections.

Funding

This work was financially supported by the "Ministère de l'Enseignement Supérieur, de la Recherche et de l'Innovation" with a three-year doctoral scholarship.

specify the exact humus form developing on such soils, could represent a promising way to understand (i) their pedogenesis and (ii) their ability to support ecological functions and biodiversity. Bulk density (g cm -3 ) 0.97 ± 0.14 0.69 ± 0.07 0.98 ± 0.20 a Soil pH was measured according to the standard ISO 10390. Total organic carbon (TOC) and total nitrogen (N) were measured according to the standards NF ISO 10694 and NF ISO 13878 respectively. Total cation exchange capacity (CEC) were measured using the cobalthyhexamine method (NF ISO 23470).

Declarations of interest

None

Particle size distribution analysis was performed according to the standard NF X 31-107. Bulk density (Bd) was calculated according to the norm NF EN ISO 11272. Water holding capacity (WHC) was assessed according to the standard NF EN ISO 274.