Nicolas Ducoulombier

Camille Chateau

Michel Bornert

Jean-François Caron

Patrick Aimedieu

Jonathan Perrin

Mario Scheel

X-RAY TOMOGRAPHIC OBSERVATIONS OF MICROCRACKING PATTERNS IN FIBRE-REINFORCED MORTAR DURING TENSION STIFFENING TESTS

Keywords: Fibre-Reinforced Concrete, Interfacial Damage, Micromechanical Testing, X-ray Tomography

For the last decades, new reparation or fabrication processes have been studied to replace traditional rebar by roving of different mineral or organic fibres to avoid corrosion issues. Such materials refer to the family of cementitious composite. Their tensile strength would directly depend on the proportion of reinforcement but also strongly on the interfacial mechanical properties between fibres and cementitious matrix. From now, evaluation of interfacial properties was mostly limited to the use of force-displacement curves obtained from mechanical experiments. This work presents a new methodology using micromechanical tension stiffening tests combined with X-ray computed tomography (XRCT) observations, performed at the Anatomix beamline at Synchrotron Soleil, and specific image processing procedures. Multi XRCT acquisitions with suitable scanning strategy are used to image the whole fibre-matrix interface along centimetric samples at four to five different levels of loading magnitude. Intensive image processing is then performed on tomographic images including digital volume correlation (DVC), image subtraction and Hessian-based filtering. This experiment allows to study damage mechanisms at small scale. The proposed methodology shows great potential to provide both qualitative and quantitative elements on interfacial mechanical behaviour such as crack growth and crack orientation. The interface between mortar and sufficiently small multi-fibre yarn used in this paper is shown to behave in certain condition as traditional rebar interface producing conical cracks in the surrounding matrix rather than debonding in mode 2, permitting a much higher energy dissipation during debonding. According to this study, conical cracks repartition and geometry are mostly influenced by the cementitious matrix. The spacing between cracks goes from 50 to 100 μm and the angle between crack normal vector and yarn orientation goes from 35 to 50 degrees.

INTRODUCTION

Reforming concrete reinforcement strategies is a difficult task. Indeed, traditional reinforced shuttered concrete industry is well-organised, ultra-regulated and its mechanical efficiency has been well-proven since a century. Nevertheless, reinforced concrete structures may show poor durability due to corrosion of steel rebar, which can yield to dramatic collapse. Indeed, a large part of existing infrastructures worldwide becomes quite old and would need to be either reinforced or demolished and reconstructed to avoid other accidents. This aspect linked to reparation cost and resource shortage is a driving force pushing construction actors to develop new ways of reinforcing concrete either for construction or reparation purposes. Mineral and organic fibres are good candidates to replace steel rebar. The straightforward strategy is to manufacture rebar using those materials, for instance, composite rods from mineral fibres that can be used instead of steel [1] [2] . However, these rods are generally less stiff than steel rebar (if we omit those made of very expensive high modulus carbon fibres) and the obtained reinforced concretes are often less ductile than traditional steel reinforced ones. Another method would be to use short mineral fibre-reinforced concrete. Alkali-Resistant glass fibres (AR-GF) have been used for a long time to improve concrete properties, such as ductility [3] [4] . But their mostly isotropic orientation distribution in the mix, and the strong limitation on fibre amount (lower than 3%) due to the needed workability of the fresh mix, prevent it from using them to play the role of steel rebars [5] . A more recent methodology consists in using continuous fibres or filaments, which are tied together into yarns or rovings. Their very large slenderness makes their final orientation dependent on the concrete flow, which is not appropriate for traditional construction process. However, this property could become a benefit for new fabrication processes for which such reinforcements could be oriented in the desired direction. Textile reinforced concrete or mortar (TRC or TRM) are typical examples obtained using such roving in grid form for reinforcement of cementitious matrix. They have been developed to both build efficient lightweight structures [6] - [7] and to reinforce old buildings and infrastructures [8] - [9] . In addition, automation in construction is a formidable means of developing new efficient construction processes that make a full use of alternative reinforcement for concrete. In particular, this work is part of a larger project that aims to reinforce 3D printed concrete by integrating mineral fibre rovings during concrete extrusion to obtain unidirectional cementitious composites. It is worth noting that as diameter of the reinforcement is getting lower, the number of reinforcement elements per unit cross section, which is inversely proportional to the square of diameters, increases. Thus, using small mineral fibres remains an interesting issue, as the material can be seen as a composite material with a modification of bulk mechanical properties. At the same time, using more reinforcement elements in the same section decreases reinforcement spacing, what imposes to use finer cementitious matrix, i.e. finer aggregates.

Using roving of mineral or organic fibres as reinforcement of concrete is then promising, but an important amount of research is still needed to better understand both short and long-term mechanical behaviour of the different proposed processes resulting in a particular cementitious composite. Regarding brittle matrix composites, their mechanical properties would be governed by the relative amount of reinforcement with a given matrix, but they would also strongly depend on interfacial properties between matrix and roving. An additional difficulty comes from the fact that roving is an assembly of many micrometric filaments or fibres [10] . Indeed, in that case, damage behaviour at interface and stress redistribution in the roving are much more difficult to characterize. Numerous studies have already been conducted on interface in cementitious composites. Nevertheless, the great variability and inhomogeneity in the cementitious matrix itself and the possible influence of the yarn on its compactness and composition strongly increase the variability of results. A standard method is based on comparisons between pull-out experimental force-relative displacement curves and simulations using a given model [11] [12] [13] [14] [15] [16] [17] . This methodology allows for the determination of respective interfacial parameters, usually fitting maximal pull-out force and residual frictional force, whenever non null. A recent review of pull-out tests is provided by Teklal et al. [18] . With multi-fibre yarns, impregnation by the cementitious matrix has been evidenced, from scanning electron microscopy (SEM) observations and mechanical tests, to constitute a key parameter [START_REF] Aljewifi | International Conference on Composite Materials & Renewable Energy Applications (ICCMREA)[END_REF] [START_REF] Aljewifi | Etude du comportement mécanique à l'arrachement de fils multifilamentaires enrobés dans une matrice cimentaire et influence de l'imprégnation[END_REF] influencing pull-out properties. Nevertheless, concerning direct observations, apart from specific considerations based on SEM analyses on the deterioration due to cement alkalinity of multi-fibre yarns [START_REF] Enfedaque | [END_REF] [22] , no direct observation has been made on progressive damage that develops at the interface between yarn and cementitious matrix, up to the authors' knowledge. In the present study, an alternative micromechanical test, called "tension stiffening", is proposed to study interaction between cementitious matrix and yarn (see Ducoulombier et al. [START_REF] Ducoulombier | 10th International Conference on Fracture Mechanics of Concrete and Concrete Structures (FraMCoS-X)[END_REF] for details). It consists in pulling on a single yarn locally embedded in the matrix on a ten to twenty mm-long area. It was inspired by the traditional macroscale "tension stiffening" test used for the determination of rebar/concrete interfacial properties [START_REF] Goto | [END_REF] . It has been preferred over other existing micromechanical tests because of the simplicity of the loading conditions, its ability to provide in a single experiment two pull-out tests (one at both ends of the sample) and its additional ability to give access to residual frictional stress. This work will precisely address that question of direct damage observation by a specific experimental tension stiffening set-up designed to be run within a high resolution X-ray computed tomography (XRCT) setup, namely that of the new Anatomix beamline of Synchrotron Soleil (Saint Aubin, France). This non-destructive imaging technique allows in situ experiments to be performed [25] . In addition, when associated with appropriate digital volume correlation (DVC) [26] , image subtraction techniques [27] and hessian-based segmentation technique [28] , it was shown to be efficient to detect tiny cracks in a lightweight cementitious material. In this paper, the same image processing is used for the analysis of several in situ tension stiffening tests. The methodology is shown to be powerful not only to give qualitative information on interfacial damage modes, but also to provide quantitative elements such as crack growth or crack orientation. Such elements can be of great interest to formulate or enhance assumptions underlying micromechanical modelling of the damage phenomena. Furthermore, when associated with the measurement of mesoscale forcedisplacement curves, they provide complementary information to quantitatively identify interfacial constitutive parameters.

After the first section, which deals with specimen specifications, experimental set-up and protocol, the second part of this paper describes the image processing and the resulting measurements, the accuracy of which is discussed. Then, specific observations of typical matrix/yarn couples are separately detailed. Finally, global geometrical information are obtained using hessian eigenvector analysis for each sample and are discussed.

EXPERIMENTAL SET-UP

In the present section, after a quick presentation of the specimen geometry, the mechanical properties of its components and the fabrication process, the specific set-up developed for in situ testing is carefully described together with the testing protocol. Then, a brief description of both material and controlling software of the XRCT setup of the Anatomix beamline is provided before detailing imaging settings that were used for the experiment.

-Specimen Specification and Fabrication

A specimen is made of a given yarn embedded on its central parts in a prismatic cementitious matrix. Two printable ordinary Portland cement (OPC) mortars were used for the experiment. The first one, denominated NAV has been formulated at Laboratoire Navier and the second one is a commercial printable mortar of Lafarge called NAG3. NAV was intentionally formulated to present a lower yield stress than NAG3 when casting in the specimen mould in order to provide a better impregnation. These mortars were associated with two mineral multi-fibre yarns. One is a basalt fibre yarn (BF) from Isomatex S.A. and the other is an S-Glass fibre yarn (S-GF) from AGY (S type is a high performance alkali resistant glass fibre). As a reference, both mortars were also associated with a stainless steel single-fibre yarn (SSF) from Sadevinox. "Yarn" here can then refer either to single-fibre or multi-fibre yarns. Geometrical and mechanical parameters are gathered in Table 1. Five specimens of each type were elaborated by casting concrete using a syringe in a 3D printed mould with one yarn passing through each specimen as shown in Figure 1. The plastic filament used to 3D print the mould is a BVOH filament, which dissolves in water. Then, one day after casting the concrete, the filled mould was immersed in a basin of water where it would be dissolved and specimens would cure at the same time. After 7 days, specimens with a single yarn at the centre of the mortar section were obtained. Note also that after fabrication, non-embedded parts of multi-fibre yarns were impregnated with epoxy resin with a brush. This aimed at preventing their premature rupture, ensuring homogeneous loading state at the tip of embedded yarns. But, in the case of a poor impregnation of the yarn by the cementitious matrix, as observed in the S-GF+NAG3 specimen, the resin could have partially penetrated in the embedded part of the yarn, artificially increasing the impregnation level of the embedded fibre. In that case, a potential positive influence of epoxy penetration on the interfacial properties is suspected and will be discussed in the dedicated section 4.2.

Tension Stiffening Test

Macroscopic Results

As mentioned before, interaction between yarn and matrix are here studied through a so-called "tension stiffening" test. As illustrated in Figure 2, it consists in pulling on a single yarn locally embedded in the matrix on a ten to twenty mm-long area. The non-embedded parts of the yarn are called the "free areas".

Similarly to pull-out tests, each experiment provides a particular force-deformation curve. Figure 2 presents typical tension stiffening force-deformation curves of single-fibre yarn specimens on the left and multi-fibre yarn specimens on the right. Here, the deformation of the composite 𝜀 𝑐 is calculated from the displacement 𝑢 of extreme points A and B located on nonembedded parts of the yarn very close to the matrix as illustrated in Figure 2, i.e. 𝜀 𝑐 = (𝑢 𝐴 -𝑢 𝐵 )/‖𝐴𝐵‖ 0 . The displacements were measured using digital image correlation as described in Ducoulombier et al. [START_REF] Ducoulombier | 10th International Conference on Fracture Mechanics of Concrete and Concrete Structures (FraMCoS-X)[END_REF] In Figure 2, the obtained tension stiffening curves 𝐹(𝜀 𝑐 ) are associated with the force-deformation curves of free yarns 𝐹(𝜀 𝑓 ) for comparison, where 𝜀 𝑓 is estimated from the displacement of points 𝐵 and 𝐶 similarly to 𝜀 𝑐 . The various loading levels at which tomography investigations would be performed (see next section) are plotted on the same graph using punctual markers. Although these curves cannot provide direct identification of interfacial properties, they allow for comparisons between different types of yarns and matrix. Moreover, the macroscopic curves of the embedded yarns exhibit changes in the tangent stiffness, which suggests that damage events occur at microscopic scale. These events may result from three phenomena. The first damage mode is a progressive interfacial debonding between yarn and matrix, without external matrix cracking, which was expected and is suggested by the progressive slope change of the curves in Figure 2b. The second one is the yarn damage. It was however never observed on free yarns, which rather brutally break. The third one is the multi-cracking of the matrix, which was visually observed on the external surface of the specimen BF+NAG3 and S-GF+NAV3 and suggested by the jagged shapes of the last part of the curves in Figure 2c. However, during the experiment at Anatomix, all multifibre specimens' yarn breaks always occurred before significant multi-cracking of the matrix, at a rather low overall elongation. This observation might suggest that possible damage or deterioration of the yarns occurred due to X-rays radiation. But, during the experiment, no significant influence of X-rays radiation on the force or displacement data was observed. They remained stable all along the image acquisition. Besides, it is worth noting that the multicracking stage was observed on tests performed 3 months after the experiment at Anatomix with specimens of the same set. Consequently, these modifications seem to be rather linked with longer hydration period.

In this paper, only three different specimen would be deeply studied as an example to validate the interest of the proposed methodology. Further investigations would be the purpose of a future work.

In situ setup

In order to perform in situ tension stiffening tests, a specific mechanical frame was designed to fit on the XRCT setup of the Anatomix beamline. The latter essentially consists in a hollow airbearing rotation stage (LAB Motion Systems, Heverlee, Belgium) with an internal diameter of 250 mm, associated with appropriate centring translation tables, and an indirect high-resolution image detector based on a single-crystal scintillator, visible-light microscope optics and a scientific-grade CMOS camera (details in following section). For an absorption-contrast experiment such as this one, the detector should ideally be placed close to the sample. As the overall force was quite low, we decided to take advantage of low-cost Fused Deposition Modelling (FDM) 3D printing technology to prototype the experimental frame. The scheme and a picture of the final design are shown in Figure 3. It integrates a LVDT displacement sensor (AMETEK OP1.5), which records the motion of a rigid loading beam, and a 30 N load sensor, which directly measures the load applied on the yarns. A specific acquisition device was programmed (LabView, National Instruments) to continuously record the actual loading, displacement and load/displacement curve. Furthermore, the yarn was only anchored by mechanical clamping using bolting. A constant-thickness load-bearing PMMA tube, almost transparent to X-rays, was used at specimen height to ensure no change in X-ray absorption during frame rotation and thus avoid image artefacts. The setup fits on a plate directly bolted onto the XY centring stage on top of the rotation stage of the tomography setup. The loading is manually applied by a micrometric screw that causes a displacement of the lower yarn anchorage by rotation of the loading beam as illustrated in Figure 3.

However, the load sensor capacity turned out to be too small for the multi-fibre yarn specimens. Therefore, when loading needed to be higher than the sensor capacity, the loading force was further evaluated by the measurement by DIC of the axial strain of the free area of the yarn whose stiffness was known precisely. To do so, an additional optical camera (AVT Pike 521) equipped with a Schneider Kreuznach 120mm-lens and appropriate extension tubes, fixed on an independent tripod, was used. The free yarn was marked with black and white paint. The modified set-up is illustrated in pictures of Figure 3. This allowed increasing the loading up to 40 N for multi-fibre yarn specimens. Although that measurement was less accurate (in particular because of the unavoidable rotation of the yarn about its axis), it permits to estimate with an acceptable accuracy the relative increase of load between two successive tomography scans.

Mortar component

NAV

NA G3 For each specimen, the experiment protocol sequence was defined as follows:

1) Specimen is mounted in the frame 2) The yarn is tightened using micrometric screw (and reference image for DIC are recorded whenever necessary) 3) Reference tomography scan is performed 4) Loading is increased until the first level of force is reached (with regular recording of images for DIC and associated evaluation of strain) 5) Wait for 15 min for the relaxation deformations to stabilise 6) New tomography scan is recorded 7) Repeat 4), 5) and 6) until yarn break

2.3-XRCT Imaging in Anatomix

Experiments were run on the recently established Anatomix ("Advanced Nanotomography and Imaging with coherent X rays") beamline of Soleil synchrotron facility [29] located in Gif-sur-Yvette, France, in the context of beamtime proposal no. 20181572. Anatomix is a 200-m-long beamline based on a cryogenic in-vacuum undulator (U18) and offers various tomographic setups for 3D imaging over a wide range of length scales, for various types of materials and using various contrasts. In the present study, a rather classical parallel-beam absorption tomography setup was used. The undulator was set with a gap of 5.5 mm and the beam was filtered by both an Au filter and Cu filter with appropriate thicknesses, resulting in a large-band pink beam centered at a photon energy around 38 keV. The X-ray radiographs were obtained with LuAG scintillator with adapted thickness mounted in front of a right-angle mirror, which redirects images to the CMOS sensor of an ORCA Flash 4.0 v2 camera from Hamamatsu, through either a 10x objective lens (numerical aperture NA = 0.28, working distance WD = 33.5 mm) or a 20x one (NA = 0.28, WD = 30.5 mm) from Mitutoyo and an adequate tube lens. The pixel size of the camera being 6.5 µm, this results in a voxel size of the reconstructed volumes of, respectively, 0.65 µm or 0.325 µm.

Typical acquisition includes the recording of a flat-field image for normalization before and after the scan, obtained by averaging 50 radiographs without sample, and a 180° scan of the sample containing 2000 projections (i.e., angle between projections was 0.09°). The scan duration was about 5 minutes for a pixel size of 0.65 μm and 10 minutes for pixel size of 0.325 μm. The acquisitions were made in continuous rotation mode using the FlyScan acquisition system [START_REF] Leclercq | Proceedings of the 15th Int. Conf. on Accelerator and Large Experimental Physics Control Systems 2015[END_REF] developed by SOLEIL. Every fifty scans or so, a background dark field without beam (to subtract the zero-intensity offset) was also recorded. All scanning information is summed up in table 2. As illustrated in Figure 4, various numbers of overlapping scans were necessary to cover the whole embedded yarn, depending on the specimen length and the magnification. Total duration to record the complete volume for each level of loading linearly depends on the number of scans. For small value of force, damage was supposed to be located near the embedded yarn ends and only partial acquisitions were made (see Figure 4). Note that in all cases, tomographic imaging was local, as the cross sections of the samples were larger than the detector field of view and the diameter of the reconstructed volume. Moreover, due to the long duration of a single acquisition, only one specimen of each type was tested in situ.

Radiographs were normalized using the corresponding dark and flat field images, and 3D images have been reconstructed from previously filtered projections using both ring filters and Paganin filters [START_REF] Paganin | [END_REF] by means of the academic software PyHST2 [32] . Using these options with manually optimized parameters was efficient to significantly reduce ring and phase contrast artefacts.

Acquisition was controlled using the Spyc language, the SOLEIL Python command line interface, through a specific Python object developed by King et al [33] . It allows users to control in a unified interface both stage motions and image acquisition parameters, and thus to program procedures for the scanning sequence. In the present study, this feature was of great technical interest. The multiple acquisition procedure with 50 μm image overlaps required to record the whole interfacial area could be run in one single command using a specifically written Python script based on Spyc commands. For instance, the yarn centring, which can be quite time consuming, was made at both specimen ends only before launching the acquisition and was deduced by linear interpolation for all intermediate acquisitions.

3.2-DVC

Digital Volume Correlation (DVC) analyses were performed on pairs of images, using the academic software CMV_3D developed at Laboratoire Navier [27], [START_REF] Bornert | Instrumentation, Mesure[END_REF] . It consists in finding homologous positions of a set of material points in two images, considering the grey-level distribution in a small subvolume around each point [26] . As DVC principles can be found in existing literature [START_REF] Schreier | Image Correlation for Shape, Motion and Deformation Measurements[END_REF] , [START_REF] Buffiere | Imagerie 3D En Mécanique Des Matériaux[END_REF] as well as CMV_3D implementation details, only main features and used parameters are recalled here. The repartition of the correlation points is regular and forms a parallelepipedic grid. Spacing between points was chosen equal to the size of the correlation windows. The latter was determined from reference volume to include enough contrast in the cement paste, even in the larger OPC grains, what resulted in 30 3 voxels for 0.65µm voxel size and 50 3 pixels for 0.325µm voxel size. Each correlation point is located at the centre of its respective correlation window. Despite very small strain in concrete, a non-negligible rotation and translation of the specimen can occur during the test when load is applied. Therefore, the approximation 𝜙 0 of the local mechanical transformation at the position 𝑿, located in the neighbourhood of the position 𝑿 𝟎 of one correlation point in the reference image, has to take into account a rotation and a homogeneous deformation in addition to a simple rigid translation. Thus, it is defined as:

𝜙 0 (𝑿) = 𝑿 0 + 𝑻(𝑿 0 ) + 𝑭 ⋅ (𝑿 -𝑿 0 ), for all 𝑿 in 𝐷 (1)
where 𝑻 is a pure translation, with 3 components to be evaluated, and 𝑭 is the transformation gradient associated to an affine transformation. Here, the nine components of 𝑭 are fixed and supposed to be equal to the overall deformation gradient (i.e. defined for the whole sample). It essentially captures the rigid motion between reference and loaded states. It needs to be estimated before the DVC algorithm is run and can be updated for a subsequent DVC calculation. In practice, the first estimation of 𝑭 is made by matching by hand at least four noncoplanar points and using a standard least square fit. Thus, the correlation refers here to the minimisation of the so-called zero centred normalized cross-correlation coefficient (ZNCC), which leads to the determination of the three optimal components of the local translation T for all correlation points in the regular grid. This technique permits to decrease the complexity of the minimization, dividing by 4 the number of local transformation components (3 instead of 12) with no loss of accuracy with respect to the order of the assumed transformation, as the actual transformation is nearly a rigid motion (except for cracked areas). We refer to Bornert and al. [START_REF] Bornert | [END_REF] for a discussion on the links between order of the DIC shape function and measurement accuracy.

In practice, the optimisation of the local translation components is performed in two steps to increase the computational efficiency and robustness of the DVC routines. First, sets of discrete translations (i.e., with components equal to integer numbers of voxels) are systematically explored for the best correlation coefficient. Then, a new estimation of the global transformation gradient is calculated before subvoxel accuracy is searched by using an appropriate iterative continuous optimisation algorithm associated with an interpolation of the grey levels in the deformed image. DVC is computed only on correlation points that show enough local contrast and brightness, to insure that correlation provides physically meaningful position. In addition, optimisation is only performed for points at which the correlation coefficient obtained after the first step is below a user-selected threshold, fixed to 0.15 in the present study. It is recalled that ZNCC varies between 0 for perfect matching and 2 for perfect "opposite" contrast (never observed), with 1 corresponding to the absence of matching. This procedure might be iterated to check convergence but turns out to be very stable. Pairs of 3D 2048 3 voxels volumes, with about 300 000 correlation points, can be almost automatically processed this way, after a short manual pre-processing, in a couple of hours of computation on a standard workstation.

3.3-Image Subtraction

For brittle material with a rich microstructure such as concrete, image subtraction has been shown to be very efficient to detect tiny cracks [27] . Indeed, local modification of contrast due to cracks initiation and growth are difficult to discern from microstructure in XRCT image as illustrated in Figure 5. Perfect subtraction between cracked and reference images should permit to remove all the microstructure information that does not change after loading and then only highlight changes between both images, such as crack growth. Nevertheless, image noise and imaging artefacts would affect the quality of the subtraction result by creating artificial change between reference and cracked image. Specific artefacts that had occurred during XRCT imaging and their influence on image subtraction will be discussed below. The principle of image subtraction technique used in this article is explained in detail in a previous article [27] . It extends the concept of DVC residuals, which was already used in another context to quantify cracks in heterogeneous materials [38] , to local DVC and to images exhibiting domains with almost uniform grey levels. Only a quick overview, highlights on slight modifications and used parameters are mentioned here.

The subtracted image is defined in the reference configuration as:

𝑟(𝑿) = 𝑔(𝜙 1 (𝑿)) -𝑓(𝑿) + 𝑘 (2)
where 𝑓, 𝑔 and 𝑟 stand for the grey levels in reference, deformed and subtracted images, respectively, and 𝑿 is the location of a voxel in reference image. The voxel-wise transformation 𝜙 0 , determined by DVC in all correlation windows in which DVC was successful, is extended to every voxel by interpolating the transformation of nearby correlation points. The obtained local transformation 𝜙 1 allows transforming the deformed image back to the frame of the reference image, which results in the so-called transformed image, by using a tricubic interpolation to compute the grey level 𝑔(𝜙 1 (𝑿)). Finally, the subtracted image is computed in 8-bit grey-scale using the offset value 𝑘 set to 128 to ensure positive grey levels. Note that, because the imaging conditions remained stable, it was not necessary to account for global evolution of contrast and brightness between reference and deformed images. A distance criterion 𝑑 is used to select the neighbour correlation points involved in the estimation of the local transformation 𝜙 1 . In the present paper, this parameter has been chosen equal to twice the spacing of the correlation grid. As mentioned in [27] , the search of neighbour correlation points in a very large set can be really time consuming. Here, it was drastically reduced by taking advantage of the regularity of correlation points' grid: the search volume was reduced to a cube centred on the considered voxel with a side length of 2𝑑.

3.4-Discussion on crack detection performance

The methodology used to evaluate the performance of crack detection methodology is first introduced and illustrated in Figure 5 and Figure 6 on the BF+NAG3 specimen images (voxel size of 0.65μm). It is then applied on S-GF+NAG3 images, with a smaller voxel size (0.325 μm), leading to a discussion on the best choice for the voxel size.

As discussed by Chateau et al. [27] , the image subtraction methodology is able to detect cracks with subvoxel opening and its performance is essentially controlled by the ratio of image noise level to the contrast between grey levels in solid phase and pores. It is thus of primary importance to evaluate these quantities.

A simple quantification of the image noise level in the reference image can be performed by considering grey level fluctuations in the sole sand particles, which can be supposed to be areas of almost uniform grey-level in an ideal noiseless image. As the grey levels in a noiseless subtracted image is expected to be fully uniform, apart from cracks, the fluctuation of any subdomain of the subtracted image can be considered. For the BF+NAG3 specimen, the image noise 𝜎 𝑓 in the reference image is estimated using the single slice shown in Figure 6-a. It is defined as the standard deviation of the grey level values located in the areas circled in yellow, containing about 300 000 voxels, leading to 𝜎 𝑓 ≤ 1,74, where the inequality results from the possible physical variability of the sand particles X-Rays linear attenuation coefficient. The image noise 𝜎 𝑠 in the subtracted image is estimated using the 3D cylindrical area delimited by the yellow circle in Figure 6-b and extending over a height of 200 slices, containing about 300 million voxels. It is equal to 𝜎 𝑠 = 2,49. Note that noise in subtracted images can also be calculated when considering the subtraction of the overlapping area of two neighbour 3D images of the reference stage (illustrated in Figure 4). It is thus estimated to 2.51, which shows that the loading of the sample does not influence the subtraction efficiency and that the possible presence of cracks does not significantly affect the grey level statistics. In addition to random noise, real XRCT images used in the present study show various artefacts, illustrated in Figure 6:

-The edge artefacts, i.e. wrong attenuation indications of X-rays near particle edges due to X-rays refraction, or so-called phase contrast, are observed even though the Paganin filter has been used to limit this effect. -The ring patterns do not coincide in reference and loaded images and are thus still present in the subtracted images, in particular when they are close to phase opposition. They are clearly visible in the subtracted image in Figure 6-b. Some larger rings can also appear when some additional large dust particle pollutes the scintillator during the experiment. In this case, microstructure information of the corresponding toroidal area is lost. -Subtracted images also show parallel lines patterns in one or more directions that spread over the whole sample, as highlighted in Figure 6-b by the set of white lines. In author's minds, these artefacts might be due to approximations induced by local tomography performed on cubic specimen, i.e. with non-axisymmetric statistical repartition of density and X-rays absorption in the non-reconstructed part of the sample.

All these image artefacts and noises, which are barely visible in the images but are definitively present, are strongly emphasised by image subtraction and will limit the method's ability to detect crack occurrence and growth. In order to illustrate this fact, three corresponding transversal slices of the BF+NAG3 specimen in reference, transformed at last loading stage and subtracted images are shown in Figure 5. First, qualitative observations confirm the ability of the technique to remove all microstructural features on the subtracted image, including preexisting cracks, and to enhance new cracks. Looking at the transformed image only, it would have been difficult, if not impossible, to notice the new crack and differentiate it from preexisting ones. Once highlighted by the subtracted image, it is much simpler to detect and eventually segment the crack. In this particular case, the main new crack induces a local grey level variation much stronger than image artefacts (rings, lines and edges), which are also visible. Smaller crack like features are hard to separate from artefacts and noise.

Next, particular grey level profiles along lines located on these images are plotted in Figure 5.

They illustrate in a quantitative way that the microstructure of mortar makes the crack detection a difficult problem. The subtracted profile shows that microstructure and pre-existing cracks are removed, while new cracks are highlighted.

Finally, following previous work [27] , crack detection accuracy can be assessed by a quantification of the minimal crack opening 𝑒 𝑚𝑖𝑛 needed for detection, considering that the crack cannot be distinguished in the subtracted image if the induced grey-level drop δ is smaller than the standard deviation 𝜎 𝑠 of the noise in the undamaged phase in the subtracted image:

𝜎 𝑠 Δ 𝑚𝑎𝑥 ≤ 𝑒 𝑚𝑖𝑛 ≤ 2 𝜎 𝑠 Δ 𝑚𝑎𝑥 , (3)
where 𝑒 𝑚𝑖𝑛 is the minimal opening expressed in voxels and Δ 𝑚𝑎𝑥 is the maximal grey level drop, which is calculated as the difference between the mean grey level in dense solid phase 𝑔̅ 𝑠𝑜𝑙 and the grey level in a porosity 𝑔 𝑝𝑜𝑟 . It is worth noting that in the worst case, grey level drop can be distributed over two neighbour voxels what explains the coefficient 2 in the upper bound of the above inequality. However, this simple accuracy assessment holds only for ideal imaging conditions such that actual spatial resolution of images coincides with the voxel size.

In practice, the physical limitations of the imaging system or the subsequent image processing routines may induce a blur such that image spatial resolution might be significantly coarser than voxel size. Such a blur is characterised by its kernel or point spread function 𝐾(𝑦), which extends over a support larger than one voxel. The grey level drop induced by a crack would then not be localized on one or two pixels, but rather distributed over a window of pixels according to 𝐾(𝑦). A curious reader can refer to [39] for more specific information.

On the first hand, for the BF+NAG3 specimen (Figure 5, voxel size of 0.65μm), mean grey level in cement paste is equal to 𝑔̅ 𝑠𝑜𝑙 = 70, and grey level in porosity is equal to 𝑔̅ 𝑝𝑜𝑟 = 40.

Using equation (3) and the above evaluated standard deviation of grey level in the subtracted image, the minimal crack opening that would be detected in ideal conditions is then estimated as 0.08 ≤ 𝑒 𝑚𝑖𝑛 ≤ 0.16 voxels, which corresponds to 0.05 µ𝑚 ≤ 𝑒 𝑚𝑖𝑛 ≤ 0.11 µm (voxel size of 0.65 µm). However, due to the spatial resolution limitation induced by imaging conditions (sample to scintillator distance, scintillator thickness, numerical aperture of lens) and reconstruction algorithm (in particular ring artefact correction and Paganin filter), equation (3) needs to be corrected for estimating of the crack thickness using the procedure described in [39] , based on the integration of the grey levels in the subtracted image along a path normal to the crack surface. Looking at the graph in Figure 8, the maximal grey level drop in the above example is found to be close to 15 (to be compared to 𝑔̅ 𝑠𝑜𝑙 -𝑔̅ 𝑝𝑜𝑟 = 30), but spreads over several voxels, which suggests a crack opening of the order of one voxel.

On the other hand, images with the smallest voxel size 0.325 μm (S-GF+NAG3 specimen) offer twice the magnification (though not twice the spatial resolution) at the cost of a field of view half the size, with a total size of 0.66mm as illustrated in the schematic view in Figure 4. The subtracted image between reference and last loading stage obtained with this higher magnification shows a lower signal to noise ratio, with a standard deviation of noise between 7 to 10 and a maximal grey-level drop induced by cracks in deformed images equal to ∆ 𝒎𝒂𝒙 = 𝟖𝟎. In such conditions, the use of equation ( 3) indicates that the smallest detectable crack aperture 𝐞 𝒎𝒊𝒏 is between 7/80 = 0.09 voxel and 10*2/80 = 0.25 voxel in the worst-case scenario, i.e. 𝟎. 𝟎𝟑 < 𝐞 𝒎𝒊𝒏 < 𝟎. 𝟎𝟖 µ𝐦, assuming an ideal imaging setup.

Moreover, at that magnification, we observe the presence of a new kind of artefact that distorts the particles shape in the XRCT images. This is highlighted at the top of Figure 11 (zoom in the transversal cut of the transformed image at the last loading stage) where the GF filaments cross-sections do not look round. This distortion is supposed to be due to deformation associated with relaxation. Indeed, to obtain the same signal to noise ratio in the 3D images, a longer acquisition time is needed, so that delayed deformation has more time to develop during the scans. Moreover, the same displacement amount appears larger in images at higher magnification. In order to be less sensitive to the local distortion induced by relaxation and to embed enough contrast, the size of correlation window has been increased to 50 voxels. Taking into account the actual conditions inducing a spatial resolution coarser than the voxel size, the actual detection would be less accurate, but in any case somewhat more efficient than with the optical conditions used for the lower magnification. The use of a smaller pixel size might thus permit to enhance the crack detection, though not by the same factor than voxel size decrease, but a particular care needs to be taken with respect to relaxation for in situ experiments. When relaxation displacement is important, a lower magnification could be the better choice, providing an optimal trade-off between crack detection and size of field of view.

3.5-Hessian based segmentation and measurement of cracks orientation.

At this point, the method permits to detect cracks and to qualitatively discuss general damage patterns and their evolutions with loading. It should however be noticed that using the obtained subtracted image for the purpose of cracks segmentation would be rather difficult. Indeed, the particular case presented in Figure 5 shows that the segmentation using a simple thresholding method would probably yield to either loss of tiny cracks or include many voxels that do not belong to a crack. A more sophisticated solution to differentiate cracks from noise and acquisition artefacts such as rings, also proposed in [27] , is the use of geometric information of the local grey-level drop provided by the comparison of eigenvalues 𝜆 3 ≥ 𝜆 2 ≥ 𝜆 1 of the local hessian matrix, i.e. the second derivative of the grey-level in the subtracted image. Indeed, a crack is essentially a dark planar geometry, characterised by a local grey level drop following a particular direction, which is indicated by a large absolute difference between the higher eigenvalue and the two others. Therefore, the quantity 𝐴(𝑿), called "crackness" image, proposed in [28] and defined by equation ( 4), is a suitable quantity to evaluate the presence of a crack at a given position X.

𝐴(𝑿) = 𝜆 3 (𝑿) -|𝜆 2 (𝑿)| -|𝜆 1 (𝑿)| (4)
The crackness has then been used to compute the binary image of detected cracks by a thresholding followed by the removal of smaller particles. The grey level threshold value was determined by hand and only particles larger than 300 voxels were retained. On various figures of next section, respective binary image of cracks is superimposed in yellow on the transformed images. Obtained images would be called "crack+transformed images". If this method showed a real practical interest, it should be however noticed that so far no quantitative element is given on the potential improvement of crack detection.

Finally, a broader use of the image hessian matrix is proposed in the present paper to analyse the mean crack orientation with respect to the yarn central axis. Indeed, the eigenvector 𝒗 𝟑 (𝑿) associated with the larger eigenvalue 𝜆 3 (𝑿) is an estimate of the normal vector of the crack local orientation 𝒏(𝑿) [28] . Then, the crack orientation map coded as a 16-bit RGB colour image is defined as follow:

∀𝑿, { 𝒏(𝑿) = 𝒗 𝟑 (𝑿) , 𝐴(𝑿) ≥ 𝐴 𝑚𝑖𝑛 𝒏(𝑿) = [0,0,0] , 𝐴(𝑿) < 𝐴 𝑚𝑖𝑛 (5)
Eventually, the orientation map is smoothed, by convolution with a uniform kernel, and renormalized to remove irrelevant local fluctuations. This map provides rich quantitative information. In the present study, for each studied case, the crack orientation will be characterised by the statistical distribution of inclinations of cracks' normal vector with respect to the fibre direction (which in practice is along the z direction), noted 𝜑 = arccos (𝒏 . 𝒆 𝒛 ); and the deviation angle of its transversal component 𝒏 𝒕 with respect to 𝒆 𝒓 , noted 𝜃 𝑑 = arcsin ( 𝒏 𝒕 ‖𝒏 𝒕 ‖ . 𝒆 𝜽 ). {𝒆 𝒓 , 𝒆 𝜽 , 𝒆 𝒛 } are the unit vectors of the cylindrical coordinate system centred in the yarn central axis. Geometrical illustration of those specific angles is provided in Figure 7. From these distributions, many geometrical information can be computed. For instance, we propose in section 4.5 to estimate the representative crack geometry, based on an assumption about its geometry made from the observation.

Interfacial damage of various single yarns embedded in mortar systems

This section describes the main observations of interfacial behaviour for various yarn/mortar couples. The combination of XRCT imaging of loaded specimens with the image subtraction technique allows for determining damage patterns and cracks' geometry as well as their evolution with increasing load. All general results on damage mode, geometry and failure load for each specimen are gathered in Table 3. It indicates that the yarn type and the shape of its cross section primarily influence the interfacial bond, which is associated with a particular type of damage. In this part, the discussion is focused on the most interesting examples and the influence of these parameters on interfacial behaviour and damage pattern is carefully highlighted.

4.1 Basalt multi-fibre yarn (BF) embedded in NAG3 matrix 4.1.1 Geometry of interfacial debonding along the yarn In this system, interfacial damage is characterised by the presence of pseudo periodic series of conical cracks in the surrounding matrix around the yarn. As illustrated in Figure 8, they are emitted from the yarn interface and they develop in the surrounding matrix towards the tip of the matrix cylinder. The detailed shape of those conical cracks is also affected by the matrix microstructure. Indeed, particles of sand tend to deviate the crack propagation. In addition, the crack transversal cross-section is similar in shape to the yarn cross-section. This damage pattern, with a network of cracks in the matrix rather than a single one along the yarn/matrix interface, testifies a strong bond between the yarn and matrix. It is also very similar to internal cracking pattern that develops at concrete-rebar interface near rebar ribs [START_REF] Goto | [END_REF] . Another interesting feature the dense transversal multi-cracking that develops between main part of the multifibre basalt yarn and a smaller portion of fibre separated from the main yarn in subdomain sd2 at the top of Figure 8. In that case, the damage pattern is similar to that of brittle matrix unidirectional composite, which is another proof of the good interfacial bond between multifibre yarn and matrix. Nevertheless, in the same sample, one may also find some local splitting debonding between yarn and matrix, which reflects a weaker bond between yarn and matrix. In particular, the bottom of Figure 8 illustrates a situation with a mixed damage mode, with one side of the interface splitting and the other emitting cracks in the surrounding matrix. For both conical and transversal cracks, the spacing is about 100μm. 3: Collection of experimental results: impregnation is sorted from "-", the lowest rate where most filaments are left un-impregnated to "++" for which most filament are impregnated by mortar. The "*" is added to mention that epoxy resin penetrates in the un-impregnated filament.

Figure 8: Geometry of debonding in the BF+NAG3 sample at the last loading stage. For both subdomains sd2 and sd9 (defined in Figure 4), a longitudinal slice, represented in both crack+transformed and crackness images on the left, is associated with two transversal slices of the crack+transformed image on the right. A 3D rendering, highlighting the conical shape of the cracks, is also provided for subdomain sd9. These slices are defined on the schematic 3D view by yellow and blue planes respectively. The green cylinder represents the field of view of the local tomography. Voxel size is 0,65µm.

Debonding versus increasing loading

Figure 9 shows interfacial cracks evolution on transformed images of subdomains sd9 (defined in Figure 4) at several stages of increasing loads. For each loading stage, the position of the last crack emitted from the yarn can be identified. Defining the "debonded length" as the position along the yarn of the last emitted crack with respect to the mortar tip, one can follow its evolution with increasing load, as emphasised with red lines in Figure 9. From this identification, the force-debonded length curves for both ends of the sample are plotted in Figure 10. Both curves appear to be very similar, which shows that the symmetry of the mechanical problem is preserved during the whole experiment. The evolution of the debonded length with increasing load is found to be affine. Figure 10: Evolution of debonded length versus applied force in BF+NAG3 at both ends of the specimen (subdomain sd2 and sd9 are defined in Figure 4).

Glass (S-GF) yarn embedded in NAG3 matrix

Geometry of interfacial debonding along the yarn

Two different damage patterns appeared at both sides of the specimen. They are illustrated in Figure 11. The first one, visible at the upper end (sd2) shows conical cracks emitted from the yarn that grow in the surrounding matrix, similar to those observed in the BF+NAG3 specimen. However, despite the deviation of some cracks by sand grains, cracks form more regular cones with rather circular transversal cross-sections, and almost no splitting is observed, as illustrated at the top of Figure 11. It is worth noting that at that tip, it seems that a substantial amount of epoxy resin penetrated through the non-impregnated yarn.

The opposite end of the specimen (sd16), illustrated at the bottom of Figure 11, shows a very different damage mode. Although a few small conical cracks are observed, yarn debonding occurs mostly by splitting between yarn and matrix. One can also observe some epoxy resin that penetrated through the non-impregnated filaments. More precisely, the splitting occurs between non-impregnated GF filaments and filaments impregnated in mortar, as shown in the zoom in transversal slice of the transformed image at the bottom of Figure 11.

To sum up, both ends of the specimen exhibit a significantly different behaviour, with a relatively low bond between yarn and matrix at the bottom (sd16-15-14-13), which induced splitting, and a better bond at the top (sd2) which induced a regular network of matrix cracks. At this point, the reasons for these opposite behaviours are still difficult to clarify, but the authors suspect that artificial improvement of impregnation is induced by the penetration of epoxy resin. The unequal repartition between both subdomains may explain the difference between respective damage patterns.

Evolution with increasing loading

Similarly to the BF+NAG3 specimen (section 4.1.2), the debonded length is estimated at both ends of the specimen for each applied load. Obtained debonded lengths are then plotted as a function of load in Figure 12. These curves show that at the end where debonding mostly happens by splitting, the debonded length for a same applied force is approximately twice the length of the other side where matrix cracking occurs. As expected, splitting occurs at a lower level of shear stress than matrix cracking. The symmetry of the mechanical problem is therefore lost during increasing loading.

Basalt (BF) yarn embedded in NAV matrix

In existing literature [START_REF] Aljewifi | Etude du comportement mécanique à l'arrachement de fils multifilamentaires enrobés dans une matrice cimentaire et influence de l'imprégnation[END_REF] , impregnation is identified to have a great impact on interface bond. To study this effect more in detail, the two mortars used in this study presented different rheological behaviour at early age. As stated in section 2.1, NAV was formulated with a smaller yield stress than NAG3 to improve impregnation. As expected and illustrated by the comparison between the BF+NAV transversal slice on the left of Figure 13 and the transversal slice of S-GF+NAG3 on the right bottom corner of Figure 11, the impregnation of BF+NAV is qualitatively better. In fact, the NAG3 mortar flew only through a small peripheral skin of the S-GF yarn, with a thickness of a few tens of micrometres, while the NAV mortar was able to penetrate deeply in the BF yarn over hundreds of micrometres. However, the NAV mortar that actually flew through the BF yarn shows more porosity than in the bulk and is only composed of the finer elements of the paste. Besides, both NAV and NAG3 mortars produced ettringite needles in the yarns porosity.

As for the other multifilament samples, the interfacial damage pattern in the BF+NAV sample (Figure 13) is composed of conical cracks emitted by the matrix which develop in the surrounding matrix. Their transversal cut seems again similar to the yarn cross-section. It is also worth emphasizing the dense transverse multi-cracking that occurs in the matrix that penetrated into the yarn, illustrated by the zoom made in the transversal slice on Figure 13-b. This damage pattern is also similar to those observed in other brittle matrix composite [4][40] and is the sign of a great interfacial bond and a good penetration of the matrix inside the yarn. The spacing is here smaller than the one observed in BF+NAG3 sample and equals to about 50μm.

Other composite systems with single-fibre yarn

This subsection discusses the use of the proposed methodology when a smooth single-fibre steel yarn is used as reinforcement for mortar. The study of such simpler case would be of great interest to better understand interface behaviour as this specific situation involves a simplified geometry, which would allow one to use simpler models. Unfortunately, observations of tests on SSF based specimens were not conclusive because of numerous practical difficulties. Qualitative observations do not reveal any crack emitted in the matrix or any other proof showing that interfacial damage occurs. Nevertheless, the force-elongation tension stiffening curve plotted on left graph in Figure 2 shows, for both SSF specimens, a strong decrease in the stiffness of the overall system with the increasing of the loading. When put together, these observations suggest that decohesion between yarn and matrix is likely to take place in the vicinity of the yarn. Unfortunately, this location is also subject to a strong edge artefact due to the large X-ray absorption contrast between steel and mortar. This artefact is revealed by subtracting the overlap areas of two successive images in the reference state, i.e. with an intact interface. The image subtractions of different loading states, i.e. with presumed debonded interface, show similar features and therefore do not allow detecting other features than this artefact. Moreover, as the single-fibre yarn is smooth and does not show enough internal greylevel contrast, no measurement of local displacement discontinuity between yarn and mortar was possible using DVC. The use of another material for the single-fibre yarn, which would show enough internal contrast and a lower difference of absorption with the mortar, would ensure the image processing to be run much more efficiently. This is left for further investigations.

Analysis of crack orientations in different specimens.

Previous observations show that cracks orientation is very sensitive to microstructure heterogeneity. Consequently, the observation of one single crack does not permit to characterise the representative geometry of all interfacial cracks. Therefore, a statistical analysis of crack orientation is provided in Figure 14, which shows the statistical distributions of the two angles presented in section 3.5 (Figure 7) for the three studied specimens. The angle 𝜃 𝑑 (Figure 14 top left) is the angle between the crack normal transversal component and radial direction 𝒆 𝒓 , while the angle 𝜑 (Figure 14 top right) is the one between crack normal and yarn direction.

Considering that cracks are mostly conical, 𝜃 𝑑 distribution then represents the roundness of the crack cone (a Dirac distribution located at zero would then be the distribution for a circular transversal profile) and 𝜑 distribution represents the slope of the crack plane with the transversal plane.

Based on the assumption of conical cracks, it is possible to quantify in average the geometrical characteristics of the cracks from their orientation map 𝒏(𝑿). Such analysis results in a more visual representation of the crack geometry than the orientation histograms and can provide overall typical patterns related to interfacial properties. To that end, we propose two simplified descriptions of crack geometries by considering separately the mean transversal section of cracks 𝑟(𝜃), obtained by averaging over all distances to the yarn, and the mean axisymmetric profile 𝑧(𝑟), obtained by averaging over all polar angles (Figure 14 bottom). The details of the calculation are available in the appendix.

Regarding the roundness of the crack cones, the SGF+NAG3 specimen exhibits the most round one among all mean transversal cross-sections 𝑟(𝜃), i.e. corresponds to the slightly narrowest distribution of 𝜃 𝑑 . Complementarily, comparing mean transversal profiles with shape and orientation of yarn cross-section confirms the influence of the yarn cross-section shape and orientation on the crack transversal profiles. This effect was previously observed qualitatively on some transversal tomography slices. Regarding the inclination of the crack cones, the distribution on the angle 𝜑 and the axisymmetric profile 𝑧(𝑟) both suggest it is mostly controlled by the matrix properties. This simplified geometrical modelling is useful to obtain first quantitative information on the crack shape to compare globally the damage features of the various systems. It would be imprecise when the crack transverse cross section are not sufficiently round or when they evolve with the distance to the yarn. A more accurate averaged geometrical description of the evolution of crack normal vector orientation as a coupled problem 𝒏(𝑟, 𝜃, 𝑧), albeit more complex, would be an interesting perspective of the present analysis.

CONCLUSIONS / PERSPECTIVES

A specific in situ tension stiffening test was conducted at the Anatomix beamline of Synchrotron Soleil. It allows, with non-destructive observation of the damage typology, for studying its link with the materials microstructure, and its evolution with increasing loading. The testing frame was designed using fast prototyping techniques to adapt it to the microtomography setup of Anatomix. Several increasing monitored levels of force were applied to six different specimens, and local X-ray computed tomography imaging was performed at each level, covering efficiently the whole interfacial area, with submicrometric voxel size. From these raw 3D images, despite possible tracking of the larger cracks, detection of tiny cracks is very difficult due to the strongly heterogeneous microstructure of the mortar. To enhance cracking detection, a specific method based on DVC, image subtraction technique and hessianbased segmentation was used. This technique permits to enhance the identification of tiny cracks with a subvoxel aperture around 0.1μm, by removing similar information between reference and loaded images. It keeps only changes between both states such as tiny cracks. To further distinguish cracks from imaging artefacts, the crackness image is computed from the hessian of grey level of subtracted images. Moreover, the crack orientation map is also calculated for voxels belonging to a crack. This methodology is shown to be an efficient tool to characterise interfacial debonding damage typology and geometry for multi-fibre yarn in a cementitious matrix. Different damage typologies have been identified depending on the type of composite system. They are gathered in Table 3 and their mean geometries have been described quantitatively from the local orientation of cracks.

In most multi-fibre yarn systems, the cracks are shaped as cones emitted from the fibre and developing in the matrix towards the sample tip. The transverse shape of the cones is very similar to the transverse shape of the yarn. The angle of the cones is observed to depend on the type of mortar. This type of damage, similar to cracking patterns that appear at rebar ribs in reinforced concrete demonstrates the great interfacial strength between yarn and matrix. This great interfacial strength is also highlighted by the dense transversal multi-cracking that occurs in matrix located between separate groups of fibres. The second type of interface damage is a local splitting between yarn and matrix that indicates a smaller local interfacial bond. Mixed situations have also been identified. The present study highlights the influence of the yarn crosssection shape on the interfacial bond between multi-fibre yarn and cementitious matrix, characterised by the damage mode type.

A straightforward perspective would be to use the presented methodology to study other multifibres structure, such as multi ends roving and different impregnation systems [START_REF] Aljewifi | Etude du comportement mécanique à l'arrachement de fils multifilamentaires enrobés dans une matrice cimentaire et influence de l'imprégnation[END_REF] . The methodology would also provide interesting quantitative data for calibrating micromechanical models and thus permit to optimise the yarn choice depending on a particular matrix in a particular process. Finally, the experimental methodology could be performed on specimens with several parallel yarns close to each other to specifically study transversal multi-cracking damage patterns and the reciprocal influence between yarns.

Figure 1 :

 1 Figure 1: 3D printed mold with yarns before casting the printable mortar

Figure 2 :

 2 Figure 2: (a) Schematic loading conditions and (b, c) mesoscopic tension stiffening force-elongation curves with punctual markers indicating the levels of loading for tomographic investigations

  Fibre traction Strength are the value obtained with specimen without mortar prism.

Figure 3 :

 3 Figure 3: Scheme and pictures of the final design of the in situ tension stiffening frame

Figure 4 :

 4 Figure 4: Schematic view of the XRCT acquisition procedure for a 10mm-long specimen with a voxel size equal to 0.65μm (BF+NAG3 and BF+NAV) on the left and 0.325 µm (S-GF+NAG3) on the right

Figure 5 :

 5 Figure 5: Typical 8-bit grey level XRCT image transversal slice of BF+NAG3 images and corresponding grey level profiles in different material phases: 𝑓(𝑋): Reference Image, 𝑔(𝜙 1 (𝑋)): transformed image using best local transformation and 𝑟(𝑋): defined by equation (2) with k=128 (Contrast and brightness are adjusted to enhance visual aspect); yellow arrows indicate location of the respective grey-level profiles.

Figure 6 :

 6 Figure 6: Examples of XRCT image transverse slices a) Reference image b) Subtracted image of the BF+NAG3 specimen; yellow lines delimit areas on which image noise is quantified; white lines emphasise local tomography artefacts

Figure 7 :

 7 Figure 7: Definition of characteristic local angles of a crack in the cylindrical coordinate system

Figure 9 :

 9 Figure 9: XRCT longitudinal slice of BF+NAG3 system showing evolution of debonded length (red line) and crack growth from crack+transformed images images of subdomain sd9 at various loading stage.

Figure 11 :

 11 Figure 11: Geometry of debonding in the S-GF+NAG3 sample at the last loading stage, in the sd2 (top) and sd16 (bottom) sub-domains. The same longitudinal slice represented in crack+transformed and crackness image (left) is associated with two transversal slices of the crack+transformed image (right) that are defined in the central schematic 3D view by blue and yellow planes respectively. The green cylinder represents the field of view of the local tomography (voxel size is 0.325µm)

Figure 12 :

 12 Figure 12: Yarn debonded length versus applied force at both ends of the S-GF+NAG3 sample, showing splitting in subdomains sd13-14-15-16-17 and matrix cracking in subdomains sd1-2-3. Subdomains are defined in Figure 4.

Figure 13 :

 13 Figure 13: Transversal and longitudinal slices of crack+transformed image at the upper end of BF+NAV (sd1) specimen at a force level of 34 N (dashed lines on both slices indicate the section plane used to draw the other slice).

Figure 14 :

 14 Figure 14: Top: Angular distribution of normal vector of crack plane with respect to yarn direction: angle 𝜃 𝑑 at the left and angle 𝜑 at the right (see fig.7); Bottom left: mean transversal cross-section of cracks 𝑟(𝜃) normalized to an arbitrary size; Bottom right: mean longitudinal crack profile 𝑧(𝑟) at the right-bottom corner. In these plots, position and cross-section of yarns are recalled in dotted lines.

Table 1 :

 1 Mortars and yarns composition, geometrical and mechanical properties.

	Yarn properties	S-GF BF	SSF

Table 2 :

 2 General information on XRCT acquisition

			NAG3	NAG3+	NAG3+	NAV+	NAV+	NAV+
			+ BF	S-GF	SSF	BF	S-GF	SSF
	Side length	~2.5	~2.5	~2.5	~2.5	~2.5	~2.5
	(mm)
	Length (mm) 10	10	20	10	10	20
	Voxel	size	0.65	0.325	0.65	0.65	0.65	0.65
	(µm)
	Number of	10	17	17	8	9	17
	acquisitions
	Time	per	~5	~10	~5	~5	~5	~5
	acquisition
	(min)
	Total time for	50	170	80	40	45	40
	one loading
	(min)
	Number of	6	4	5	4	6	5
	loading levels
	Total beam	300	680	400	160	270	200
	time (min)

Table

	Specimen	Impre-gnation	Yarn cross-section shape	Damage mode	Cracks shape in matrix	𝑭 𝒎𝒂𝒙 (N)
	BF+NAG 3	top bottom	+ +	Flattened	Matrix cracking Mixed mode	Flattened Conical Flattened Conical	40
	S-	top	-*		Matrix cracking	Conical
	GF+NAG			Round			32
	3	bottom	-*		Splitting	/
	BF+NAV	top bottom	++ ++	Rather round	Matrix cracking Matrix cracking	Conical Conical	35
	S-GF+NAV	top bottom	++ ++	Round	Matrix cracking Matrix cracking	Conical Conical	36
	SSF+NA G3	top bottom	/ /	Round	Splitting Splitting	/ /	19
	SSF+NA V	top bottom	/ /	Round	Splitting Splitting	/ /	19

ACKNOWLEDGEMENT

The work presented in this article is part of a PhD project supported by Labex MMCD (MultiScale Modelling and Experimentation of Materials for Sustainable Construction), which benefits from French government grants managed by the French National Research Agency ANR within the frame of the national program Investments for the Future (grant no. ANR-11-LABX-022-01). ANATOMIX is an Equipment of Excellence (EQUIPEX) also funded by the Investments for the Future program, project NanoimagesX, grant no. ANR-11-EQPX-0031. The authors want to express their gratitude to Marine Lemaire for the design of the acquisition electronics and the programming of the dedicated LabView application, and to Dr Sébastien Brisard for his helpful presence during image acquisition at Synchrotron Soleil.

APPENDIX

This appendix details the determination of the simplified representative geometry of the cracks. According to section 4.5, we suppose that the cracks mostly conical and that their representative geometries can be defined by two uncoupled descriptions: the transversal crosssection of cracks 𝑟(𝜃) and the mean axisymmetric profile 𝑧(𝑟). On one hand, the transversal section of cracks 𝑟(𝜃) is supposed to be independent of 𝑟 and 𝑧 apart from a homothety. Then, it can be obtained from the evolution of 𝜃 𝑑 with respect to 𝜃, given by the orientation map, by integration of 𝑑𝑟 𝑟 𝑑𝜃 = tan (𝜃 𝑑 (𝜃)). The function 𝜃 𝑑 (𝜃) is obtained by averaging the data of the orientation maps over all detected cracks.

On the other hand, the axisymmetric profile 𝑧(𝑟) is the same for all cracks apart from a translation, and does not depend on 𝜃. We also consider that 𝒏 belongs to {𝒆 𝒓 , 𝒛 }.

Consequently, it yields

𝑑𝑧 𝑑𝑟 = tan (𝜑(𝑟)). It can then be computed from the evolution of 𝜑 with respect to 𝑟, given by the orientation map. The function 𝜑(𝑟) is again obtained by averaging the data of the orientation maps over all detected cracks. Distances smaller than 𝑟 < 200 voxels are here rejected because they may correspond to locations in the fibre.

Despite the important fluctuations in the orientation map, the great amount of data permits to perform a moving average. A sampling procedure provides a 0.5 voxel discretization for both 𝜃 𝑑 (𝜃) and 𝜑(𝑟). These sampled evolutions are both plotted in Figure 15. Numerical integrations are then performed to obtain the respective transversal and axisymmetric profiles, plotted at the bottom of Figure 14.


Masatake Kobayashi

Olivier Huttin

Erwan Donal

Kevin Duarte

Arnaud Hubert

Hervé Le Breton

Elena Galli

Maxime Fournet

Philippe Mabo

Frederic Schnell

Christophe Leclercq

Patrick Rossignol

Nicolas Girerd
email: n.girerd@chru-nancy.fr

Pr Nicolas Girerd

Association of Estimated Plasma Volume Status with Hemodynamic and Echocardiographic Parameters

Keywords: Plasma volume, congestion, left ventricular filling pressure, sex difference

Background: Estimated plasma volume status (ePVS) has diagnostic and prognostic value in patients with heart failure (HF). However, it remains unclear which congestion markers (i.e., biological, imaging and hemodynamic markers) are preferentially associated with ePVS. In addition, there is evidence of sex differences in both the hematopoietic process and myocardial structure/function.

Method and results:

Patients with significant dyspnea (NYHA≥2) underwent echocardiography and lung ultrasound within four hours prior to cardiac catheterization. Patients were divided according to tertiles based on sex-specific ePVS thresholds calculated from hemoglobin and hematocrit measurements using Duarte's formula.

Among the 78 included patients (median age 74.5 years; males 69.2%; HF 48.7%), median ePVS was 4.1 (percentile 25-75 =3.7-4.9) ml/g in males (N=54) and 4.8 (4.4-5.3) ml/g in females (N=24). Patients with the highest ePVS had more frequently HF, higher NT-proBNP, larger left atrial volume and higher E/e' (all p-values<0.05), but no difference in inferior vena cava diameter or pulmonary congestion assessed by lung ultrasound (all p-values>0.10).

In multivariable analysis, higher E/e' and lower diastolic blood pressure were significantly associated with increased ePVS. The association between ePVS and congestion variables was not sex-dependent except for left ventricular enddiastolic pressure, which was only correlated with ePVS in females (Spearman Rho=0.53, p<0.01 in females and Spearman Rho=-0.04, p=0.76 in males; p interaction =0.08).

Conclusion:

ePVS is associated with E/e' regardless of sex, while only associated with invasively measured left ventricular end-diastolic pressure in females. These results suggest that ePVS is preferably associated with left-sided hemodynamic markers of congestion.

Introduction

Plasma volume is a marker of volume overload and is linked to the regulation between interstitial and intravascular spaces [START_REF] Miller | Fluid Volume Overload and Congestion in Heart Failure: Time to Reconsider Pathophysiology and How Volume Is Assessed[END_REF][START_REF] Francis | Comparison of neuroendocrine activation in patients with left ventricular dysfunction with and without congestive heart failure. A substudy of the Studies of Left Ventricular Dysfunction (SOLVD)[END_REF] . Estimated plasma volume status (ePVS) derived from hemoglobin and hematocrit has been repeatedly reported to be associated with clinical outcomes in patients with acute or chronic heart failure (HF) [START_REF] Duarte | Prognostic Value of Estimated Plasma Volume in Heart Failure[END_REF][START_REF] Ling | Calculated plasma volume status and prognosis in chronic heart failure[END_REF][START_REF] Kobayashi | Prognostic value of estimated plasma volume in acute heart failure in three cohort studies[END_REF][START_REF] Chouihed | Diagnostic and prognostic value of plasma volume status at emergency department admission in dyspneic patients: results from the PARADISE cohort[END_REF] . Previous reports showed only a moderate association between ePVS using various equations and radiotracer-based quantitative plasma volume measurements [START_REF] Ling | Calculated plasma volume status and prognosis in chronic heart failure[END_REF][START_REF] Fudim | Calculated Estimates of Plasma Volume in Patients With Chronic Heart Failure-Comparison With Measured Volumes[END_REF][START_REF] Martens | The optimal plasma volume status in heart failure in relation to clinical outcome[END_REF] . However, the correlation between PV estimated from hemoglobin/hematocrit and measured PV by 125I-human serum albumin in diabetic patients was recently showed to be acceptable (concordance index 0.6, P<0.01) [START_REF] Dekkers | Effects of the sodium-glucose cotransporter-2 inhibitor dapagliflozin on estimated plasma volume in patients with type 2 diabetes. Diabetes, obesity & metabolism[END_REF] . There are only sparse data however regarding the association of ePVS with clinical, biological and echocardiographic congestion as well as with invasive hemodynamic parameters [START_REF] Kobayashi | Prognostic value of estimated plasma volume in acute heart failure in three cohort studies[END_REF][START_REF] Chouihed | Diagnostic and prognostic value of plasma volume status at emergency department admission in dyspneic patients: results from the PARADISE cohort[END_REF][START_REF] Greene | Haemoconcentration, renal function, and post-discharge outcomes among patients hospitalized for heart failure with reduced ejection fraction: insights from the EVEREST trial[END_REF][START_REF] Testani | Potential effects of aggressive decongestion during the treatment of decompensated heart failure on renal function and survival[END_REF][START_REF] Van Der Meer | The predictive value of short-term changes in hemoglobin concentration in patients presenting with acute decompensated heart failure[END_REF] . Whether ePVS is more closely associated with pulmonary or systemic congestion markers has yet to be ascertained.

In addition, current evidence suggests that there are underlying sex differences in hematopoiesis [START_REF] Murphy | The sex difference in haemoglobin levels in adults -mechanisms, causes, and consequences[END_REF] , myocardial structure and function [START_REF] Beale | Sex Differences in Heart Failure With Preserved Ejection Fraction Pathophysiology: A Detailed Invasive Hemodynamic and Echocardiographic Analysis[END_REF][START_REF] Beale | Sex Differences in Cardiovascular Pathophysiology: Why Women Are Overrepresented in Heart Failure With Preserved Ejection Fraction[END_REF] . These sex differences may have a substantial impact on the appropriate ePVS thresholds.

However, whether the association between congestion markers and ePVS is sex-dependent remains to be established.

The present study aimed to investigate 1) the association of ePVS with clinical, biological, echocardiographic as well as invasive hemodynamic congestion variables and 2) whether these associations are sex-dependent.

Methods

Patient Population

This study prospectively included 81 patients with significant dyspnea (NYHA≥II) who underwent a coronary angiography with left heart catheterization (LHC) between May 2016 and July 2017 [START_REF] Hubert | Diagnostic accuracy of lung ultrasound for identification of elevated left ventricular filling pressure[END_REF] . Seventy-eight patients who had available hemoglobin/hematocrit data were included in this subsequent analysis. Exclusion criteria were: mitral stenosis, known pulmonary fibrosis, pneumonia, active lung cancer and history of recent chest trauma. Demographic characteristics, comorbidities and biological profiles were obtained from review of medical records. HF was diagnosed according to the ESC guidelines [START_REF] Ponikowski | ESC Guidelines for the diagnosis and treatment of acute and chronic heart failure: The Task Force for the diagnosis and treatment of acute and chronic heart failure of the European Society of Cardiology (ESC). Developed with the special contribution of the Heart Failure Association (HFA) of the ESC[END_REF] . Estimated glomerular filtration rate (eGFR) was calculated by the Chronic Kidney Disease Epidemiology Collaboration formula [START_REF] Levey | A new equation to estimate glomerular filtration rate[END_REF] . The study protocol was approved by the local ethics committee (authorization number: 2014-A01331-456).

Transthoracic Echocardiography

A c c e p t e d M a n u s c r i p t

All patients underwent a standard echocardiography using a Vivid S6, E7 or E9 ultrasound system (General Electric Healthcare, Horten, Norway). Images were recorded on a remote station for off-line analysis using a dedicated software (EchoPAC PC, version BT 13, General Electric Healthcare, Horten, Norway). Interpretation was blinded for clinical and hemodynamic data. Left ventricular ejection fraction (LVEF) was measured using the biplane Simpson's method [START_REF] Nagueh | Recommendations for the Evaluation of Left Ventricular Diastolic Function by Echocardiography: An Update from the American Society of Echocardiography and the European Association of Cardiovascular Imaging[END_REF] . Diastolic function was assessed from the pattern of mitral inflow by pulsed-wave Doppler. Mitral annular early diastolic velocity (e') was assessed at the septal and lateral sites of the mitral annulus using tissue Doppler imaging. E/A ratio, e' mean and E/e' mean ratio were calculated. Inferior vena cava (IVC), tricuspid annulus plane systolic excursion and left atrial volume (LAV) were obtained as recommended [START_REF] Nagueh | Recommendations for the Evaluation of Left Ventricular Diastolic Function by Echocardiography: An Update from the American Society of Echocardiography and the European Association of Cardiovascular Imaging[END_REF] . Pulmonary arterial systolic pressure was estimated using tricuspid velocity and inferior vena cava compliance and diameter [START_REF] Nagueh | Recommendations for the Evaluation of Left Ventricular Diastolic Function by Echocardiography: An Update from the American Society of Echocardiography and the European Association of Cardiovascular Imaging[END_REF] . Right ventricular (RV) function was assessed according to recent guidelines [START_REF] Nagueh | Recommendations for the Evaluation of Left Ventricular Diastolic Function by Echocardiography: An Update from the American Society of Echocardiography and the European Association of Cardiovascular Imaging[END_REF] .

Hemodynamic Data and Lung Ultrasonography

LHC was performed within four hours following echocardiography. Prior to coronary angiography, transducers were calibrated, with a 0-level set at the mid-axillary line. The left ventricular end-diastolic pressure (LVEDP) was continuously recorded (25 mm/s) with a 5 French Judkin R4 catheter (ICU Medical, San Clemente, CA, USA) placed at the mid-LV cavity. Waveform analysis was blinded from clinical and echocardiographic data. LVEDP was calculated as the mean value of 4 consecutive heart cycles.

Lung ultrasound was performed immediately before echocardiography with patients in supine or near-tosupine position, as previously described [START_REF] Picano | Ultrasound lung comets: a clinically useful sign of extravascular lung water[END_REF] . Loops were stored on a remote station for off-line analysis using the same tools as those used for echocardiography. For each lung ultrasound zone, the number of B-lines was quantified from 0 to 10, with resulting LUS scoring ranging from 0 to 80 (8-zone method). An excellent reproducibility of measurements, performed by experienced cardiologists, has previously been reported in this population [START_REF] Hubert | Diagnostic accuracy of lung ultrasound for identification of elevated left ventricular filling pressure[END_REF] .

Estimated Plasma Volume Status

ePVS was calculated from the Strauss-derived Duarte formula using hematocrit and hemoglobin values 3 as follows: ePVS (mL/g)=100 × (1-hematocrit) ⁄ hemoglobin in g/dL

The Hakim formula was also used for calculating plasma volume estimation derived from hematocrit and dry body weight using the following equations [START_REF] Plasmapheresis | Handbook of dialysis[END_REF] Ideal plasma volume=c × body weight in kg (males: a=1530, b=41.0, c=39; females; a=864, b=47.9, c=40), ePVS=[(actual plasma volume -ideal plasma volume)/ideal plasma volume]×100.

Statistical Analysis

Continuous data are expressed as median (25 and 75 percentile) and categorical data as numbers (%). Patients were divided into three groups according to sex-specific ePVS tertiles [median (IQR) = 4.07 (3.73-4.93) ml/g in males and 4.76 (4.37-5.27) ml/g in females]. Group differences were assessed using Kruskal-Wallis tests for continuous variables and χ² tests or Fisher's exact test for categorical variables. Unadjusted correlations were expressed using Spearman's correlation coefficients.

Linear regression analyses were performed to evaluate the association of ePVS with clinical, biological, echocardiographic and invasive hemodynamic variables. All variables with a P<0.10 in univariable analysis were used as candidate variables in the multivariable model prior to backward selection procedures. An interaction test was performed to determine whether the associations between ePVS and congestion markers are sex-dependent.

Statistical analyses were performed using R version 3.4.0 (R Development Core Team, Vienna, Austria). A two-sided p-value <0.05 for associations and p < 0.10 for interactions were considered statistically significant.

Results

Baseline Characteristics according to Renin and Aldosterone Levels

Among the 78 patients included in this study, 54% were male, median age was 74.5 (67.0-80.0) years, one-fifth (21.8 %) of the population had a BMI ≥30kg/m² and a half (48.7%) had HF and coronary artery (Table 1).

Patients in the highest ePVS tertiles had more frequently HF, higher N-terminal pro-B-type natriuretic peptide (NT-proBNP), LAV index, E/e' and lower RV isovolumic acceleration compared to patients in the lowest ePVS tertiles (all p<0.05) (Table 1). In contrast, there was no significant difference in IVC, LVEDP and B-line counts across ePVS tertiles.

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Clinical Determinants of Estimated Plasma Volume Status

Univariable linear regression analysis showed that elderly age, female sex, lower BMI, diastolic BP, higher NT-proBNP, larger LAV index and higher E/e' were significantly associated with higher ePVS (Table 2). In multivariable linear regression models, only female sex, higher E/e' and lower diastolic BP were significantly associated with higher ePVS (Table 2).

Correlation between ePVS and congestion markers across heart rhythm and LVEF strata is shown in Supplementary table 1. ePVS significantly correlated with E/e' only in patients with sinus rhythm, whereas similar correlations between ePVS and congestion marker were found across LVEF strata.

Interplay between Sex, Estimated Plasma Volume Status and other Congestion Markers

ePVS was found to be significantly correlated with NT-proBNP (rho=0.36, p=0.01), E/e'(rho=0.33, p<0.01) and LAV index (rho=0.31, p<0.01). Among congestion markers, only LVEDP was observed to have a sex-specific association with ePVS solely in females (rho=0.53, p<0.01 in females and rho=-0.04, p=0.76 in males; p interaction =0.08) (Figure 1).

Of note, LVEDP was not associated with higher ePVS in either univariable or multivariable analysis (Table 2).

Estimated Plasma Volume Status Calculated by the Hakim formula

Sex-specific ePVS tertiles derived from the Hakim formula were also applied in the present population [median (IQR)= -9.45 (-15.61 -1.06) % in males and -7.29 (-10.01 -4.02) % in females] (Supplementary table 2). Patients with the highest ePVS tertiles were older, had lower BMI and were less likely to have atrial fibrillation (all p-value<0.05). However, there were no significant differences in biological, echocardiographic and invasive hemodynamic congestion markers across ePVS tertiles.

Multivariable linear regression models showed that ePVS was only associated with BMI and diastolic BP (Supplementary table 3).

Discussion

The current study is the first to assess the association of ePVS with clinical, biological, echocardiographic and invasive hemodynamic congestion markers. Our main findings are that: 1) higher ePVS derived from the Duarte formula was significantly associated with higher E/e' in multivariable analysis; 2) LVEDP was correlated with ePVS using the Duarte formula in females, while not associated with ePVS in the overall population; 3) ePVS derived from the Hakim formula was not associated with usual congestion markers. The above results suggest that ePVS derived

Estimated Plasma Volume Status -a left-sided congestion variable

Our findings outline certain underlying features of plasma volume that have not been previously addressed. Among all patients included in our study, results showed that higher E/e' was associated with a higher ePVS level, but not with B-lines or LVEDP. There is growing evidence linking pulmonary interstitial edema quantified by lung ultrasound and elevated invasive measurements of LV filling pressures [START_REF] Hubert | Diagnostic accuracy of lung ultrasound for identification of elevated left ventricular filling pressure[END_REF][START_REF] Platz | Utility of lung ultrasound in predicting pulmonary and cardiac pressures[END_REF] . In contrast, a recent meta-analysis emphasized the lack of diagnostic value of E/e' ratio in predicting LV filling pressure [START_REF] Sharifov | Diagnostic Accuracy of Tissue Doppler Index E/e' for Evaluating Left Ventricular Filling Pressure and Diastolic Dysfunction/Heart Failure With Preserved Ejection Fraction: A Systematic Review and Meta-Analysis[END_REF] . This being said, E/e' is nevertheless a recognized congestion marker shown to be associated with clinical outcome in population-based or HF cohorts [START_REF] Nagueh | Left Ventricular Diastolic Function: Understanding Pathophysiology, Diagnosis, and Prognosis With Echocardiography[END_REF][START_REF] Shah | Contemporary Assessment of Left Ventricular Diastolic Function in Older Adults: The Atherosclerosis Risk in Communities Study[END_REF][START_REF] Dokainish | Incremental predictive power of B-type natriuretic peptide and tissue Doppler echocardiography in the prognosis of patients with congestive heart failure[END_REF] . Given that we did not identify a significant association between ePVS and IVC, our findings further suggest that ePVS is more likely a left-sided congestion marker. This premise is also supported by the biological findings presented herein: patients within the highest ePVS tertiles had higher NT-proBNP, which is also typically considered as a left-sided congestion marker [START_REF] Neeland | Biomarkers of chronic cardiac injury and hemodynamic stress identify a malignant phenotype of left ventricular hypertrophy in the general population[END_REF][START_REF] Girerd | Integrative Assessment of Congestion in Heart Failure Throughout the Patient Journey[END_REF] . This result is also in keeping with previous reports in patients with HF and reduced or preserved LVEF [START_REF] Duarte | Prognostic Value of Estimated Plasma Volume in Heart Failure[END_REF][START_REF] Ling | Calculated plasma volume status and prognosis in chronic heart failure[END_REF][START_REF] Rossignol | Eplerenone survival benefits in heart failure patients post-myocardial infarction are independent from its diuretic and potassium-sparing effects. Insights from an EPHESUS (Eplerenone Post-Acute Myocardial Infarction Heart Failure Efficacy and Survival Study) substudy[END_REF][START_REF] Grodin | Prognostic implications of plasma volume status estimates in heart failure with preserved ejection fraction: insights from TOPCAT[END_REF] . In addition, we observed a better correlation between ePVS and E/e' in patients with sinus rhythm. It may be partly explained by the lack of predictive performance of Doppler echocardiography for LV pressures in patients with atrial fibrillation [START_REF] Nagueh | Recommendations for the Evaluation of Left Ventricular Diastolic Function by Echocardiography: An Update from the American Society of Echocardiography and the European Association of Cardiovascular Imaging[END_REF] .

The absence of a strong association between IVC and ePVS may be partly explained by the fact that over twothirds of the total blood volume resides in the venous circulation, which is relatively unaffected by changes in fluid volume given its high capacitance [START_REF] Gelman | Venous function and central venous pressure: a physiologic story[END_REF] . Another noteworthy finding of the present study is the strong association between lower diastolic BP and increased ePVS. BP is an important modulator of the complex interaction between interstitial fluid and plasma volume [START_REF] Miller | Fluid Volume Overload and Congestion in Heart Failure: Time to Reconsider Pathophysiology and How Volume Is Assessed[END_REF] . This could provide some pathophysiological basis for decreased diastolic BP favoring intravascular volume retention, which would translate into higher ePVS.

Sex Difference in the association of Estimated Plasma Volume Status with other markers of congestion

LVEDP was observed herein to be positively correlated with ePVS in females but not in males. Women have been shown to be more prone to impaired LV diastolic reserve [START_REF] Beale | Sex Differences in Heart Failure With Preserved Ejection Fraction Pathophysiology: A Detailed Invasive Hemodynamic and Echocardiographic Analysis[END_REF][START_REF] Galderisi | Echocardiographic evidence for the existence of a distinct diabetic cardiomyopathy (the Framingham Heart Study)[END_REF] . This may partly explain why a higher left volume load (as measured by ePVS) was better correlated with LVEDP since the left ventricle in women (particularly in older women) is unable to mitigate intravascular pressure. The same amount of volume could indeed translate into different pressure levels according to the intrinsic diastolic properties of the heart. Irrespectively, these findings suggest that increased ePVS may be a more relevant marker of cardiopulmonary congestion in females [START_REF] Redfield | Age-and gender-related ventricular-vascular stiffening: a community-based study[END_REF][START_REF] Najjar | Age and gender affect ventricular-vascular coupling during aerobic exercise[END_REF] . In contrast, there was A c c e p t e d M a n u s c r i p t no sex-dependent interaction of ePVS with other congestion markers such as NT-proBNP and E/e'. Both congestion markers were reported to have sex-dependency [START_REF] Daniels | Natriuretic peptides[END_REF][START_REF] Rueda-Ochoa | Risk factors for longitudinal changes in left ventricular diastolic function among women and men[END_REF][START_REF] Flint | Echocardiographic correlates of left ventricular filling pressures and acute cardio-renal syndrome in ST segment elevation myocardial infarction patients[END_REF] , which may influence this sex-dependent interaction. The pathophysiological mechanism which may explain the sex-different association of ePVS with LVEDP needs to be further evaluated in future studies. Both clinical studies and animal studies would be interesting to refine our understanding of these differences in association between congestion variables.

Clinical Perspectives

Hemodynamic congestion can precede symptoms of congestion by several days. Plasma volume, estimated from hemoglobin/hematocrit using Duarte's formula or hematocrit/body weight using the Hakim formula, could represent easy-to-use markers in routine clinical practice. In contrast, we observed no significant association between congestion markers and ePVS derived from the Hakim formula. This differential association could be related to the Hakim formula incorporating "dry" body weight. There is a complex interplay of congestion and cachexia in HF patients which may explain that PV estimated from Hakim formula becomes less effective in this clinical setting [START_REF] Ambrosy | Body Weight Change During and After Hospitalization for Acute Heart Failure: Patient Characteristics, Markers of Congestion, and Outcomes: Findings From the ASCEND-HF Trial[END_REF][START_REF] Anker | Prognostic importance of weight loss in chronic heart failure and the effect of treatment with angiotensin-converting-enzyme inhibitors: an observational study[END_REF] .

Importantly, previous reports showed moderate associations between ePVS derived from Duarte/Hakim formula and radiotracer-based quantitative plasma volume measurements which could explain variations of association between ePVS and other congestion markers. In contrast, Duarte-derived ePVS was significantly associated with E/e' (in the whole population) and LVEDP (in females) in the current study (Figure 2). ePVS using Duarte's formula may be a useful integrative marker of left-sided hemodynamic congestion. Other congestion markers such as E/e' and LVEDP often cannot be repeatedly measured especially in the context of ambulatory patients with HF [START_REF] Girerd | Integrative Assessment of Congestion in Heart Failure Throughout the Patient Journey[END_REF] . Therefore, PV estimated from Duarte formula could potentially become a useful congestion marker in the management of HF given its low cost and practicability. Large-scale multicenter studies are invariably needed to determine whether ePVS-guided treatment can improve clinical outcome in HF patients.

Limitations

First, this is a single-center cohort study; thus, there may be residual confounding and generalizability is not unequivocal. The moderate size of our cohort only yielded moderate statistical power. Second, we had no direct measurement of plasma volume by conventional radioisotope-labeled albumin or red blood cell assays, although these techniques are relatively impractical in routine clinical practice. The concordance between estimated and measured PV is still a matter of debate. Adequation for ePVS in the specific context of HF, especially in patients with large variations in body weight, should be further studied. In addition, Patients did not undergo catherization with a highfidelity micromanometer-tip catheter. Third, ambulatory patients were recruited in this study and consequently Lastly, the sex-specific association identified herein could also be a chance finding. Further investigations are needed to determine whether a reproducible sex-specific pattern is observed for the association between ePVS and other congestion markers.

Conclusion

ePVS is associated with E/e' regardless of sex difference and is associated with invasively-measured LV filling pressure only in females. These results suggest that ePVS may be a marker of left-sided hemodynamic congestion rather than pulmonary interstitial edema or systemic congestion. M, male; F, female; COPD, chronic obstructive pulmonary disease; ACEi, angiotensin converting enzyme inhibitor; ARB, angiotensin receptor blocker; MRA, mineralocorticoid receptor antagonist; NYHA, New York Heart Association; BP, blood pressure; eGFR, estimated glomerular filtration rate; NT proBNP, N-terminal prohormone brain natriuretic peptide; ePVS, estimated plasma volume status; LVSV, left ventricular systolic volume; LAV, left atrial volume; LVEF, left ventricular ejection fraction; E/A, ratio of peak early and late diastolic velocities; e', mean value of early diastolic velocity at the septal and lateral sites of the mitral annulus; E/e', ratio of early mitral inflow velocity and mitral annular early diastolic velocity; RAV, right atrial volume; TAPSE, tricuspid annular plane systolic excursion; IVA, isovolumic acceleration; IVC, inferior vena cava; PASP, pulmonary artery systolic pressure; LVEDP, left ventricular end-diastolic pressure.

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Table 2. Multivariable Model for the Association of Clinical, Biological and Hemodynamic Parameters with Estimated Plasma Volume Status

NYHA, New York Heart Association; BP, diastolic blood pressure; eGFR, estimated glomerular filtration rate; NT proBNP, Nterminal prohormone brain natriuretic peptide; LVSV, left ventricular stroke volume; LAV, left atrial volume; E/A, ratio of peak early and late diastolic velocities; E/e', ratio of early mitral inflow velocity and mitral annular early diastolic velocity; RAV, right atrial volume; TAPSE, tricuspid annular plane systolic excursion; IVA, isovolumic acceleration; IVC, inferior vena cava; PASP, pulmonary artery systolic pressure; LVEDP, left ventricular end-diastolic pressure.

  :

A c c e

  p t e d M a n u s c r i p t Actual plasma volume=(1 -hematocrit) × (a + b × body weight in kg)

  A c c e p t e d M a n u s c r i p t from the Duarte formula may be an easily-accessible surrogate of measured markers of left-sided hemodynamic congestion in routine clinical practice.

A c c e

  p t e d M a n u s c r i p t experienced less severe degrees of congestion than patients typically included in acute HF registries: Our results are thus only relevant for these lower risk patients.

A c c e p t e d M a n u s c r i p t Graphic abstract Figure 1 .Figure 1 .

 abstract11 Figure 1. Scatterplots of Congestion Markers with Estimated Plasma Volume Status according to Sex Difference

Table 1 . Patient Characteristics according to Sex-specific Tertiles of Estimated Plasma Volume Status

 1 Sex-specific tertiles indicate the tertiles derived from males and females separately.

*

Table 2 . Multivariable Model for the Association of Clinical, Biological and Hemodynamic Parameters with Estimated Plasma Volume Status

 2

		Univariable model	Multivariable model
	Variables	β (95%CI)	p-Value	β (95%CI)	p-Value
	Clinical parameters
	Age, yrs (per 5 yrs)	0.15 (0.04 -0.26)	0.01	-	-
	Male sex	-0.54 (-0.99 --0.08)	0.02	-0.67 (-1.25 -0.08)	0.03
	Body mass index, kg/m² (per 5 kg/m²)	-0.20 (-0.39 --0.01)	0.04	-	-
	Hypertension	0.16 (-0.31 -0.62)	0.50
	Diabetes mellitus	0.44 (-0.09 -0.97)	0.09	-	-
	Coronary artery disease	0.27 (-0.16 -0.70)	0.21
	Heart failure	0.52 (0.10 -0.94)	0.02	-	-
	NYHA III+IV	0.41 (-0.07 -0.89)	0.09	-	-
	Diastolic BP, mmHg (per 5 mmHg)	-0.13 (-0.21 --0.05) <0.001	-0.22 (-0.41 --0.02)	0.03
	Biological parameters
	Sodium, mmol/l (per 5 mmol/l)	-0.14 (-0.44 -0.16)	0.35
	eGFR, ml/min/1.73m² (per 5 ml/min/1.73m²) -0.03 (-0.08 -0.03)	0.34
	Log NT proBNP	0.24 (0.04 -0.43)	0.02	-	-
	Left ventricular function
	LVSV index, ml/m² (per 5 ml/m²)	0.02 (-0.02 -0.05)	0.43
	LAV index, ml/m² (per 5 ml/m²)	0.05 (0.01 -0.10)	0.03	-	-
	LV ejection fraction, % (per 5%)	-0.02 (-0.09 -0.04)	0.46
	LV ejection fraction <40%	0.42 (-0.03 -0.87)	0.07	-	-
	Global longitudinal strain, %	0.02 (-0.02 -0.06)	0.24
	E/A ratio	0.02 (-0.25 -0.28)	0.91
	E/e' mean	0.04 (0.01 -0.06)	<0.001	0.03 (0.01 -0.06)	0.03
	Right ventricular function
	TAPSE, mm	-0.02 (-0.06 -0.02)	0.27
	RV IVA, m/sec	-0.09 (-0.29 -0.12)	0.40
	IVC dimension, mm	0.01 (-0.03 -0.05)	0.51
	estimated PAPS, mmHg (per 5 mmHg)	0.06 (-0.02 -0.13)	0.15
	Other parameters
	LVEDP, mmHg	0.01 (-0.02 -0.04)	0.37
	Total B-Lines	0.02 (-0.01 -0.04)	0.18