Applied Clay Science 132–133 (2016) 508–517

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Applied Clay Science

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

Research paper

Development of an industrial mineralogical framework to evaluate

mixtures from reservoir sediments for recovery by the heavy clay
industry: Application of the Durance system (France)
Frédéric Haurine a,b,⁎, Isabelle Cojan b, Marie-Anne Bruneaux a
a
CTMNC, – 17, rue Letellier, – 75786 Paris Cedex 15, France
b
MINES-ParisTech-PSL Research University, Geosciences, 35 rue Saint Honoré, - 77305 Fontainebleau Cedex, France

a r t i c l e i n f o a b s t r a c t

Article history: The use of dam reservoir sediments would contribute to preserving non-renewable resources, offer alternative
Received 17 November 2015 raw materials for the heavy clay industry, and reduce the silting of dams and the environmental impact of its dis-
Received in revised form 8 July 2016 persal following dredging.
Accepted 23 July 2016
The aim of this work is to present the structure and application of a mineralogical industrial framework (MIF) in
Available online 10 August 2016
the evaluation of reservoir sediments as a replacement for natural raw materials in the heavy clay industry. The
Keywords:
MIF is composed of two ternary plots based on the dominant minerals (quartz, clay minerals (imparting plasticity
Mineralogy for shaping and cohesion after drying and firing), feldspars, chlorite and muscovite, and carbonates) and clay
Industrial framework mineral assemblages (illite, kaolinite and swelling clay minerals) from 36 industrial mixes.
Heavy clay The application of the MIF to reservoir sediments of the Durance system indicates that they fall outside of the
Brick and tile industrial domain due to high contents of illite and silicate minerals (upstream Durance) or carbonates (middle
Reservoir sediment Durance and Verdon stream). This conclusion is supported by the technical impossibility of extruding the
Durance upstream sediments and the occurrence of cracks on the specimen bars from the carbonate-rich sediments.
Finally, we demonstrate that the Durance sediments can be recovered by incorporating some opening agent
(quartz sand or calcined clay wastes) and mixing sediments from different sites (upstream and middle course)
to adjust the grain-size distribution and lower the carbonate content. The ceramic properties of the mixtures
(drying and firing linear shrinkage, water absorption and tensile rupture) match the usual values of the heavy
clay industry.
© 2016 Elsevier B.V. All rights reserved.

1. Introduction Within the context of promoting the valorization of waste, nu-

Heavy clay bricks and tiles are produced from industrial mixtures
that are obtained from natural clay-rich materials with, if necessary,
the incorporation of additives (quartz sand, crushed calcined-clay
wastes, etc.) to obtain the desired quality for the industrial process
(limited drying and firing shrinkage, no cracks, etc.) and the product
(mechanical strength, thermal behaviour, colour and surface aspect,
etc.). In France, tile and brick production is ensured by factories that
are distributed all over the country as a result of a regional tradition dat-
ing back to the Roman period. Fifty industrial sites account for nearly
95% of French production, and the remainder is fabricated by artisanal
operators. The French heavy clay annual production amounts to 5 Mt,
which necessitates approximately 6 Mt of raw materials, obtained
from quarries mined close to the factories (FFTB, 2015).
⁎ Corresponding author at: CTMNC, – 17, rue Letellier, – 75786 Paris Cedex 15, France.
E-mail address: frederic.haurine@mines-paristech.fr (F. Haurine).
merous studies have evaluated the types of wastes or residues that
could be incorporated in raw materials, resulting in substitutions
from 2 to 50%, allowing for the reduction of natural clay resource
consumption and the attainment of specific product performances
(Alonso-Santurde et al., 2011; Bories et al., 2014; Monteiro and
Vieira, 2014; Zhang, 2013). The envisaged materials range from
rock wastes (granite sludge (Menezes et al., 2005), marble
(Montero et al., 2009), limestone (Turgut and Algin, 2007) or slate
(Campos et al., 2004)) to elaborate industrial wastes, such as paper
making pulp (Asquini et al., 2008; Furlani et al., 2011; Maschio et al.,
2009); spent foundry sands (Alonso-Santurde et al., 2012; Furlani et
al., 2012); tannery sludge dumps (Basegio et al., 2002) and organic
wastes (tea leaves or coffee grounds (Demir, 2006; Eliche-Quesada et
al., 2011)); sawdust (Turgut and Algin, 2007); and water treatment
sludge (Jordan et al., 2005; Merino et al., 2007; Zhou et al., 2013).
Fewer studies have been conducted on the incorporation of dredged
sediments from canals or harbours (Baruzzo et al., 2006; Chiang et al.,
2008; El Fgaier et al., 2013; Frar et al., 2014; Hamer and Karius, 2002;

http://dx.doi.org/10.1016/j.clay.2016.07.022
0169-1317/© 2016 Elsevier B.V. All rights reserved.
 F. Haurine et al. / Applied Clay Science 132–133 (2016) 508–517
Lafhaj et al., 2008; Mezencevova et al., 2012; Romero et al., 2008, 2009;
Samara et al., 2009; Xu et al., 2014). Some of the dredge material can be
used as raw materials (Huang et al., 2001; Remini, 2006; Yusuf et al.,
2012), while others need some processing to reduce the toxicity
(Lafhaj et al., 2008; Romero et al., 2008; Roziere et al., 2015).
In this paper, we address the question of the evaluation of an alter-
native material, i.e., dam sediments, in the brick and tile industry. A
mineralogical industrial framework (MIF) is proposed based on the
bulk mineralogy and clay mineral assemblages. The MIF is applied to
reservoir sediments from the Durance watershed. Following the initial
evaluation, several substitutions are tested to enhance the natural sedi-
ment properties by mixing with calcined-clay wastes, quartz sand or in-
between reservoir sediments.
2. The Durance drainage basin
The Durance river is the second largest tributary of the Rhône river
and the major stream of Southeastern France (Fig. 1A). The Durance
river rises in the Western Alps near Montgenèvre, passes through the
Prealps and flows into the Rhône near Avignon. Its main tributaries
are the Buech and the Verdon rivers on the right and left banks, respec-
tively (Fig. 1B). The Durance is 390 km long, and its drainage basin
covers 14,200 km2.
In its upper course, the bed load and suspended sediments originate
from the crystalline basement that constitutes the high reliefs of the
internal Alps (the Ecrins Massif). Downstream of the high reliefs, the
sediment load originates from sedimentary successions that are domi-
nantly composed of marls and limestones (Mesozoic successions) or
clay, silt and sandstone (Cenozoic deposits).
The Durance river management started in the mid-fifties and lasted
until the early eighties with the building of several dams in response to
the increased demand for water (irrigation, drinking water, and
Fig. 1. The Durance watershed. (A - The Durance river, a tributary of the Rhône river; B - Simplified geologic map of the Durance watershed).
509
industries), hydropower (electricity) and, more lately, recreational pur-
poses. More than 14 dams are still in operation.
However, the Durance drainage basin is characterized by one of the
highest erosion rates in France with an average chemical erosion rate of
121 t/km2/yr and a mechanical rate of 364 t/km2/yr (Alary, 1998). Most
of the eroded material is attributed to the Marnes noires badlands of Ju-
rassic age despite their limited outcropping surface (7% of the Durance
drainage basin) (Alary, 1998; Descroix and Olivry, 2002).
The dams along the Durance drainage network break the hydraulic
continuity of the stream by altering the flow regime and sediment
load. As a consequence of the Durance management, the sediments
that are exported downstream, at the location of the Cadarache dam,
are reduced from 500 to 44 kt/yr (SOGREAH, 2004). Sediments carried
by the flow are deposited in the still water of the dam reservoirs during
floods, impairing their storage capacity, a process known as “trap effi-
ciency”. Reservoir sedimentation occurs worldwide at a mean rate of
approximately 0.8% per year (Palmieri et al., 2003); however, the values
of the Durance system are far larger, up to a few percent.
3. Material and methods
3.1. Material
Two sets of samples were considered. The first sample corresponds
to 36 industrial mixtures; the second sample corresponds to samples
collected along the Durance drainage network (60 samples).
The industrial samples were provided by CTMNC (Centre Technique
de Matériaux Naturels de Construction) and brick and tile industrial
companies. For confidentiality reasons, the origins of the samples are
not mentioned. These samples, each weighing b100 g, originated from
industrial mixtures that are suitable for the production of either bricks
(13 samples) or tiles (23 samples).
510 F. Haurine et al. / Applied Clay Science 132–133 (2016) 508–517
Sampling along the Durance river was performed upstream and
downstream of each confluence as well as in the tributary merging at
the confluence, resulting in 20 samples from the tributaries. Several
samples were gathered along the Verdon river (3 samples), i.e., the
main Durance tributary. Attention has been paid to collect fine-grained
materials deposited during the spring floods prior to the sampling
campaign.
Sediments from several dam reservoirs were collected. Twenty kilo-
grams of sediments were extracted from each site to perform all of the
experiments using the same sample. Along the Durance, three samples
came from the upstream part of the Serre-Ponçon reservoir (upstream
of Savine-le-Lac), and one sample came from the centre of the
Cadarache settling pond (a sample that was provided by Electricité de
France - EDF). Along the Verdon, five samples were obtained, three
from the Castillon reservoir and one from each of the Chaudanne and
Ste-Croix reservoirs.
3.2. Methods
The mineralogical and geochemical studies were conducted on a
grain-size fraction b 40 μm for the river sediment and bulk industrial
mixes and reservoir sediments.
The mineralogical analyses were carried out via X-ray diffraction
(XRD) using PANalytical's X-ray diffractometers (Philips), CuKα radia-
tion, a wavelength of 1.5418, no monochromator, a soller slit of
0.04 rad, step scan size of 0.0167462° from 2 to 60° 2θ for the bulk sed-
iment and 0.0083731° from 2 to 29° 2θ for the clay minerals, and a
counting time of 39 min 34 s for the bulk sediment and 19 min 21 s
for the clay minerals. The quantitative mineral analysis of the bulk sam-
ple was conducted using random powder mounts. EVA software
(Bruker DIFFRACPlus 2007) was used for identification and quantitative
phase analysis. Quantification involved using the normalized intensity
ratio (RIR) method (Chung, 1974).
Following the removal of carbonate by weak acid, particles smaller
than 2 μm were separated via sedimentation by sampling the upper
2 cm of the clay suspension after 100 min. Three XRD runs were per-
formed on the oriented mounts of the clay-size particles following air-
drying, ethylene-glycol salvation and heating at 490 °C for 2 h (Moore
and Reynolds, 1997). Identification of the clay minerals was performed
according to the position of the (00l) series of basal reflections on the
three XRD diagrams. The characteristic peaks of the mixed-layer clays
(mainly random illite-smectite and chlorite-smectite) were displaced
according to the preparation, reflecting the random interstratifications
of smectite with illite or chlorite. Their relative proportion was derived
from an appropriate combination of the XRD diagrams, using the miner-
al intensity factors based on the integrated peak intensities to eliminate
the effects of crystallite variability, together with the 100% approach
(review in Kahle et al., 2002). The error estimate was ±5%.
The grain-size distribution was measured by applying the sieving
method to the bulk sediment to record the distribution of sediment
coarser than 40 μm. The retaining fraction (b 40 μm) was analysed
using the sedimentation technique (SediGraph 5100 Particle Size
Analyser - Micromeritics) with the addition of a dispersing agent
(sodium hexametaphosphate) to the aqueous suspension (error
was ±10%).
The elemental analysis was conducted using ICP-OES (Varian Vista
MPX Inductively Coupled Plasma (ICP) Spectrophotometer), following
the digestion of the sample in an acidic solution; the analytical error
was b 1%.
The physical properties of the dam reservoir samples were charac-
terized. The sediments were pre-dried at low temperature (105 °C) in
an oven. For a given weight of sediment, the amount of water necessary
to obtain a moist clay paste that shows a good plasticity was recorded.
The moist material was then extruded to obtain specimen bars on
which physical tests could be conducted as follows: shaping water con-
tent, plasticity (penetrometer), drying behaviour (Bigot's curve), linear
shrinkage, water absorption and aspect changes (colour, texture, etc.)
during firing (for temperatures ranging from 850 to 1100 °C), and flex-
ural strength before (on dried specimens) and after firing at 950 °C and
1100 °C (3-point flexural bending test, press LFPlus - Lloyd Instruments
LTD).
4. Results
4.1. The industrial raw materials
4.1.1. The mineralogical industrial framework (MIF)
The mineralogical composition of the raw industrial materials is
presented for the two main types of fired-clay products, bricks and tiles.
The mineralogy of 36 industrial mixtures indicates that six minerals
are present in more than two-thirds of the samples and constitute on
average 94% of the mineral assemblage. Among these, clay minerals
(40%) and quartz (34%) are dominant. The other four minerals (musco-
vite, microcline, albite and calcite) are present in minor proportions, on
average b7%. Some other minerals (chlorite, orthose, goethite, hematite
and dolomite) have been identified in less than one-third of the samples
as traces (b 2%).
A principal component analysis (PCA) was applied to the bulk sedi-
ment minerals, considering the following 10 minerals (i.e., variables):
clay minerals (phyllosilicates that contribute to plasticity and harden
during drying and firing, Guggenheim et al., 2006), muscovite, chlorite,
quartz, feldspars (albite, microcline and orthose), carbonates (calcite
and dolomite) and goethite. It should be noted that the number of sam-
ples (36) is slightly smaller than desirable for conducting a principal
component analysis (PCA) (min 50). The first four principal compo-
nents are retained for interpretation; when combined, they account
for nearly 70% of the total variance.
The leading component (PC1) accounts for 22% of the total variance
and describes the different behaviours of two species of fluxes as fol-
lows: feldspars (albite and orthose), which lead to vitrification and
lower porosity, and carbonates (calcite and dolomite), which decom-
pose during firing and allow for a high level of porosity (Fig. 2A). PC2 ac-
counts for 17% of the total variance and illustrates the effect on plasticity
of clay minerals and muscovite, which increase plasticity, whereas
quartz reduces plasticity and cohesion. PC3 accounts for the same
amount of the total variance as PC2 and illustrates the high water ab-
sorption capacities associated with clay minerals versus the opening
substance effect (inert elements that do not lead to any variation in
size during drying) of quartz and microcline. PC4 accounts for 13% of
the total variance and illustrates the following effect on the cohesion
of the industrial material: chlorite and muscovite favour lamination
compared to clay minerals.
As part of this study, the following six groups of minerals are identi-
fied based on the PCA results: clay minerals, carbonate (calcite, dolo-
mite), quartz, feldspars (microcline, albite, orthose), chlorite and
muscovite. These six components can be grouped into the following
three categories: clay minerals, other silicates (including quartz chlorite,
muscovite and feldspars) and carbonate (Fig. 3). The ternary plot of
these variables shows that the mineralogical composition of the indus-
trial samples (including those from Fiori et al., 1989; González et al.,
2016) is restricted to a small domain defined by b 20% of carbonate
and clay minerals, and other silicates comprise between 40 and 60%
(Fig. 3A). The compositions of the brick and tile industrial materials
are very similar, and the brick materials show a lower content of calcite
(approximately 10%). A second ternary plot is proposed to investigate
the relative percentages of quartz and other silicates, while maintaining
the clay mineral component (Fig. 3B). Quartz and clay mineral contents
vary between 20 and 60%. Other silicate mineral (feldspar, muscovite,
chlorite) content is b30%, showing higher values and a lower dispersion
for the brick raw materials (20–30%) than for the tile ones (10–30%).
The clay fraction is dominated by the following four minerals:
kaoline, illite, smectite and mixed-layer illite-smectite. These minerals
 F. Haurine et al. / Applied Clay Science 132–133 (2016) 508–517
Fig. 2. Principal components plots of minerals of industrial mixtures (A - bulk material, B -
fraction b2 μm).
are present in more than two-thirds of the samples and constitute 88%
(mean value) of the clay minerals of the clay fraction. Interstratified
clay minerals (chlorite-smectite and kaolinite-smectite) and chlorite
have been observed in less than half of the samples and constitute up
to 12% of the clay fraction.
The PCA results show that most of the information is carried by
the first two components, which account for 67% of the total variance
(Fig. 2B). The first component (40% of the total variance) shows the
differences in fluxing behaviour with a positive correlation with illite,
illite/smectite and chlorite and a negative one with kaolinite (increases
refractoriness). The second component (27% of the total variance)
illustrates the drying shrinkage with a positive correlation with smectite
511
and chlorite and a negative one with mixed-layer illite/smectite and
kaolinite.
The clay minerals are grouped into the following three categories:
kaolinite, illite and swelling clays (smectite and mixed-layer illite-smec-
tite). The ternary plot of the values from the raw industrial materials
(Fig. 3C) shows that the brick or tile data are scattered and largely over-
lap. The swelling clay content is nearly always above 20%, while the illite
or kaolinite content can be as low as 5%. A second ternary plot enables
the introduction of the chlorite content by grouping the non-swelling
clays (kaolinite and illite) (Fig. 3D). As already indicated, chlorite is
present in less than half of the samples; its occurrence is greater in the
tile raw materials (52%) compared to the brick ones (38%). No distinc-
tive criterion for any of the other clay minerals is observed.
4.1.2. Chemical composition diagram
The elemental distribution, which determines the behaviour of an
industrial material during the firing process, is classically plotted on
an Augustinik diagram (Augustinik, 1957) or three ternary diagrams
(ref in Fiori et al., 1989). The Augustinik diagram compares an index
of the chemical alteration (“argilosity”, Al2O3/SiO2 ratio) versus the ac-
cessory element total content (alkali metal (Na2O and K2O), alkaline
earth metal (MgO and CaO) and transition metal (Fe2O3 and MnO)).
The Augustinik diagram was revised to include data from the Italian
(stoneware, Fiori et al., 1989) and Spanish (tile and bricks, González et
al., 2016) ceramic industries.
The plot of the values of the tile and brick raw materials on the
Augustinik diagram (Fig. 4A) shows that there is little difference in the
Al2O3/SiO2 ratio or the values of the accessory elements total content
between the brick and tile materials. Al2O3/SiO2 ratios comprise be-
tween 0.15–0.35 for bricks and 0.08–0.27 for tiles. The current domain
of the brick raw materials from the French and Spanish industries falls
within the classical domain of the fired-clay products of the Augustinik
diagram. The roofing tile raw materials are plotted over a larger domain
due to a higher accessory element total content.
4.1.3. The Winkler diagram
The grain-size of the raw materials has a strong influence not only on
their shaping and drying but also on the mechanical properties of the
fired-clay products. The grain-size distribution is classically appraised
on a ternary plot of three sediment grain-sizes (below 2.5 μm for the fin-
est, between 2.5 and 25 μm for the intermediate and above 25 μm for the
coarsest fraction), i.e., the Winkler diagram (Winkler, 1954) (Fig. 4B).
Plots of the tile and brick raw material values fall within the previously
defined domains. The raw tile materials show a higher content of the
finest grain-size (37–56%, mean 44%) than that of the brick ones (30–
55%, mean 37%). The content of the intermediate grain-size is quite sim-
ilar for these two types of products.
4.2. The Durance watershed sediments
4.2.1. Mineralogy
Along the Durance course, two groups of samples are identified
based on their bulk mineralogical composition and clay mineral assem-
blage (Fig. 3). The sample groups correspond to the upstream and
middle courses of the Durance defined by the Serre-Ponçon dam. Data
from the Verdon samples, although similar to those of the Durance mid-
dle course samples, show distinct elements, which will be further
discussed.
The bulk mineralogical composition indicates differences between
the samples from the upstream Durance (upstream of Serre Ponçon
dam), the Durance middle course and the Verdon river (Table 1,
Fig. 3A and B). The bulk mineralogical composition comprises
seven minerals that are present in more than two-thirds of the sam-
ples and constitute at least 96% (mean value) of the mineral assem-
blage (Table 1). The following three components are dominant:
clay minerals, quartz and calcite. The proportions of the first two
512 F. Haurine et al. / Applied Clay Science 132–133 (2016) 508–517

Fig. 3. The mineralogical industrial framework (MIF).

Fig. 4. Elemental composition and grain-size distribution in raw industrial materials (France, Italy and Spain), Durance samples and mixtures (A - Augustinik diagram data from ICP-AES
analysis; B - Winkler diagram, Winkler, 1954).
 F. Haurine et al. / Applied Clay Science 132–133 (2016) 508–517 513

Table 1
Bulk sediment composition of the Durance watershed samples.

Upstream Durance Middle course Durance Verdon

(N = 26) (N = 11) (N = 6)

Mean σ Mean σ Mean σ

Minerals Occurrence (%) (%) (%) Occurrence (%) (%) (%) Occurrence (%) (%) (%)

Clay minerals 100 16 6 100 22 6 100 17 4

Quartz 100 19 2 100 22 4 100 16 3
Calcite 100 25 12 100 36 6 100 59 6
Chlorite 100 17 7 100 9 5 83 2 2
Muscovite 100 8 3 100 4 2 67 2 1
Microcline 100 4 2 92 2 1 100 2 0
Albite 83 6 5 100 3 1 83 2 1
Dolomite 70 5 7 75 ε 1 – – –
Total 100 98 100

are fairly stable (mean values of approximately 18%), while those of
calcite of the Durance middle course and along the Verdon river are
higher (mean values: 25%, 36%, 59%, respectively). Conversely, the
chlorite mean content diminishes from 17% (upstream Durance) to
9% (Durance middle course) and 2% (Verdon river). The other three
minerals (microcline, muscovite and albite) are present in minor
proportions, on average b4%.
Plots of the bulk mineralogical results of the Durance and Verdon
samples on the MIF ternary plots show that the calcite content is very
variable in the upstream samples (10 to 50%) and more homogeneous
for the downstream ones (30 to 50%) (Fig. 3A). The middle course
Durance and Verdon samples present ratios of clay minerals versus
silicates that are comparable to those of the industrial materials. The
ratio from the upstream Durance samples is far lower (Fig. 3A) due to
a high content of silicate minerals other than quartz (chlorite, musco-
vite, microcline and albite) (Fig. 3B).
Clay mineral assemblages (from the b2 μm fraction) indicate large
differences between the upstream and downstream groups of samples
(Table 2). Upstream samples comprise two clay minerals (illite (60%)
and chlorite (40%)), middle course ones present the assemblage of
three clay minerals (illite (33%), chlorite (26%), and mixed-layer illite/
smectite (26%)) plus kaolinite in minor proportion (13%). The clay min-
eral assemblages of the Verdon samples are comparable to those of the
middle course Durance despite the occurrence of smectite in all samples
(23%) and a lower content of chlorite (8%, present in 50% of the
samples).
On the ternary diagrams, the Durance middle course samples and
those from the Verdon are plotted among the brick and tile framework
(Fig. 3C and D). The upstream samples are isolated due to the absence of
swelling clays and kaolinite (Fig. 3C) and to the high content in illite and
chlorite (Fig. 3D).
This contrast in mineralogy along the course of the Durance reflects
the geology of its drainage basin. In the upstream part of its course,
some of the Durance tributaries (Guisane, Gill, Gyronde) drain areas
composed of metamorphic and crystalline rocks of the internal Alps
that constitute the source of the various silicate minerals (illite, chlorite,
microcline, albite) (Fig. 1). Downstream of the Serre-Ponçon dam, the
whole Durance hydraulic network flows over a sedimentary cover com-
posed of limestone, marls and sandstones, in which the clay mineral as-
semblages contain a significant percentage of smectite and mixed-layer
I/S or C/S (Deconinck, 1984). The Verdon river crosses sedimentary
successions dominated by limy to marly facies; the clay mineral assem-
blage is comparable to that of the Durance middle course drainage area.
4.2.2. Brick and tile industry tests
Based on the plot of the Durance samples on the MIF, the tests
specific to the heavy clay industry are conducted on samples from
dam reservoirs that are representative of the upstream (Serre-Ponçon
dam, SP-1 to 3) and downstream (Cadarache, CA-1) domains of the
Durance and the Verdon watershed (Castillon, VE-1; Chaudanne, VE-
2; Sainte Croix, VE-3) (see Fig. 1 for location).
The elemental compositions are within the expected range of the
Al2O3/SiO2 ratio and much higher as far as the accessory element total
content is concerned, except for the VE-3 sample (Fig. 4A). The elemen-
tal compositions of the samples from the Serre-Ponçon dam reservoir
are the closest to the industrial domain for bricks. The shift of the
Cadarache and Verdon samples towards high values of the accessory
element total content is mainly due to their high content of calcite
(CaCO3).
The grain size distribution of all samples reflects sediments that con-
tain a low proportion of coarse grained elements (N 25 μm) (Fig. 4B). De-
spite this grain-size distribution, the Verdon samples are nearly within
the brick domain. The low content of the coarse-grained sediments is
a limitation for the Serre-Ponçon and Cadarache samples that are, how-
ever, close to the brick and tile domains, respectively.
The total carbon content is low, with values ranging from 3 to 8%
(Table 3). Most of the carbon is considered as being associated with
the calcium carbonate, given the small amounts of organic carbon.
In the first ceramic test, the extrusion was only successful for the
Cadarache (CA-1) and Verdon Castillon (VE-1) samples. The Cadarache
specimen bars show a satisfying aspect without deformations while of-
fering a smooth surface, whereas the Verdon-Castillon ones display

Table 2
Clay mineral assemblages (fraction b2 μm) of the Durance watershed samples.

Upstream Durance Middle course Durance (N = 11) Verdon

(N = 26) (N = 6)

Mean σ Mean σ Mean σ

Minerals Occurrence (%) (%) (%) Occurrence (%) (%) (%) Occurrence (%) (%) (%)

Kaolinite – – – 82 13 7 100 19 8
Illite 100 60 8 100 33 10 100 19 8
Chlorite 100 40 8 100 26 8 50 8 –
Smectite – – – 45 2 3 100 23 15
Mixed-layer I/S 9 ε 1 91 26 10 100 20 9
Mixed layer C/S – – – – – 50 5 5
Total 100 100 94
514 F. Haurine et al. / Applied Clay Science 132–133 (2016) 508–517
Table 3
Carbon content of the dam reservoir sediments.
Carbon content TCC1 σTCC OCC2
(%) (%) (%)
Upstream Durance (SP, N = 3) 3.88 0.07 0.46
Downstream Durance (CA, N = 1) 5.78 0.17 0.80
Verdon (VE, N = 3) 7.30 0.16 0.64
1
- Total Carbon Content; 2 - Organic Carbon Content.
some cracks on the edges of the specimen bars despite an overall good
surface aspect (Fig. 5).
The remaining ceramic tests, which necessitate the use of good
quality specimen bars, were only conducted on the two successfully ex-
truded samples. The linear drying shrinkage at controlled room temper-
ature remains limited as follows: 5.4% (CA-1) and 3.4% (VE-1) (Fig. 6).
The low angle of the colloidal-drying slope indicates a gradual drying
of the colloidal water in both samples, a behaviour that is favourable
to industrial production, as is the high value of the interstitial water con-
tent (17.6–19.1%). The large amount of working moisture (approxi-
mately 25%) does not constitute a limitation. Drying difficulties seem
unlikely based on the shape of the Bigot's curves (Fig. 6).
Results of thermo dilatometric analysis and thermogravimetric/
thermo differential analysis (TGA/TDA) are in accordance with the ob-
servations made during characterization (linear shrinkage with temper-
ature, chemical reactions such as decarbonatation and organic matter
combustion) and do not bring any further understanding of the sedi-
ment behaviour. The firing tests, performed on the Cadarache and
Verdon Castillon samples that produced appropriate specimen bars,
show a limited firing shrinkage (Fig. 7) of b5% up to 1100 °C. The shrink-
age increases above 1100 °C, indicating that the start of the fusion
process that is effective at 1200 °C with the collapse of the sample.
Water absorption slightly increases during firing, from 3 to 5% at
1100 °C for the Cadarache sample and is stable at approximately 14.5%
for the Verdon Castillon sample. Above this temperature of 1100 °C,
the water absorption drops to 0% in relation to the melting of the
material.
The flexural strength is approximately 5 MPa for the dried
specimen bars and approximately 30 MPa for the specimens fired
at 950 °C (Fig. 8). This value is far above the 10 MPa value classically
considered as appropriate by the brick and tile industry when tested
in laboratory conditions.
Fig. 5. Specimen bars from the Cadarache and Verdon reservoir sediments at given stages of firing (from 850 to 1150 °C).
σOCC
(%)
0.02
0.08
0.04
Fig. 6. Drying linear shrinkage at controlled room temperature (Bigot's curve) for the
Cadarache (CA-1) and Verdon (VE-1) samples along with different mixtures based on
the Cadarache sample.
5. Discussion
5.1. The potential of the Durance reservoir sediments for the heavy clay
industry
The differences observed in the mineralogy, the major element
content, the grain size distribution and the physical properties of the
Durance sediments provide a basis to discriminate among the following
three geographic areas: the upstream Durance (UD), the Durance mid-
dle course (MD) and the Verdon (VE).
The UD samples present a mineralogy that is clearly distinct from
that of the industrial assemblages as follows: a high content of silicate
minerals (chlorite, albite, muscovite) and of illite and calcite and a low
proportion of swelling clay minerals. The high carbonate and silicate
mineral contents constitute a limitation to the tile and brick industry,
as they reduce the plasticity of the moist material, as observed during
the failed plastic extrusion of the Serre-Ponçon sample.
The mineralogy, the major element content and the grain-size distri-
bution of the MD and VE samples are quite similar to those of the indus-
trial samples, except for the carbonate content, which is markedly
higher, and the lack of coarse grain-size elements. The plastic extrusion
of both samples did succeed despite the high carbonate content, which
induced cracks on the VE samples. Both the MD and VE samples present
physical characteristics that are of interest to the brick and tile industry
 F. Haurine et al. / Applied Clay Science 132–133 (2016) 508–517
Fig. 7. Linear shrinkage and water absorption at different firing temperatures for the
Cadarache (CA-1) and Verdon (VE-1) samples along with different mixtures based on
the Cadarache sample.
in terms of drying properties (shrinkage and pore water content), fire
shrinkage and tensile bending strength.
5.2. Towards an industrial use
Most of the reservoir sediments of the Durance watershed present
characteristics close to those of the industrial mixtures, especially the
Cadarache one. We explored several ways to overcome the main prob-
lems (e.g., the high CaCO3 content and the fine grain-size distribution),
e.g., the addition of some shortening agent to the Cadarache sample,
which presents the most favourable mineralogical composition.
Adjustment of the grain-size distribution is classically performed in
the brick and tile industry by adding a material of a given grain-size dis-
tribution (quartz sand or grinded calcined clay wastes). Two mixtures
are made by adding some quartz sand of a given grain-size of 0.1 mm
(20 and 30% of the final composition, respectively). Another mixture is
achieved by adding grinded calcined clay, with particle sizes evenly
Fig. 8. Flexural resistance of the Cadarache sample and of the different mixtures obtained
from three point bending tests.
515
distributed between 40 and 400 μm (20% of the final composition). A
fourth mixture is based on the addition of sediment from Serre-Ponçon
(42%) to that from Cadarache (50%) with some grinded calcined clay
(8%), following a first try with a mixture composed of 50% of the two
reservoir sediments, a mixture that could not be extruded. The increase
in the coarser grain-size of the mixture results in a plot of the first three
mixes within the tile domain on the Winkler ternary plot and of the last
one close to the brick domain (Fig. 4B).
In complement to the grain-size adjustment, the addition of quartz
sand significantly lowers the percentage of clay minerals and calcite in
the mixtures (Fig. 3), the Al2O3/SiO2 ratio and the values of the accesso-
ry elements (Fig. 4A). The addition of grinded calcined clay (initial com-
position within the clay-brick domain) slightly lowers the values of the
variables on the Augustinik diagram (Fig. 4A). Its effect on the mineral-
ogical composition is less important because it is composed of minerals
that are stable at the firing temperatures. The mixing of sediments from
two reservoirs, with the addition of some grinded calcined clay, results
in a mineral composition that is very close to that of the tile and brick
domains (Fig. 3). The projection of the mixture grain-size distribution
on the Winkler diagram is slightly displaced towards the Brick domain
(Fig. 4B).
The drying shrinkage is reduced for all four samples, being at its low-
est for mixtures 1 and 2, i.e., the addition of quartz sand (Fig. 6). The
pore water content is also lowered down to values ranging from 14%
(CA-1 + 30% sand) to 16% for the other mixtures with quartz sand
and grinded calcined clay, whereas it is increased to 19% for mixture 4
(SP-2, CA-1 with some grinded calcined clay). Similarly, the firing
shrinkage is lowered to nearly nothing with the CA-1 SP-2 mixture
(Fig. 7). The behaviour above 1100 °C is maintained for all samples.
The mechanical behaviour is less altered with the addition of cal-
cined clays than with the addition of sand, which induces a lowering
of the value below 10 MPa (Fig. 8), classically admitted as the threshold
for industrial materials in laboratory conditions.
These results show that even if the original natural material is not
suitable for the brick and tile industry, new raw materials that are with-
in the expectations of the brick and tile industry can be elaborated by
mixing sediments from different dam reservoirs or by adding some
shortening agents (sand or calcined clay from recycling).
5.3. The pollutant issue
The upstream part of the Durance course is a fairly pristine moun-
tainous environment; some organic pollution is associated with the
seasonal tourist activities. Downstream of the Serre Ponçon dam, the
Durance valley is occupied by orchards that may cause pollution due
to pesticides and organics. From Sisteron downstream to Château-
Arnoux, pollution due to chlorinated solvents remains a major problem
for drinking water. In the Verdon basin, pollution is limited to the organ-
ic pollution during seasonal peaks.
Metal and organic pollutants in the sediments from the dam reser-
voir (Serre-Ponçon, Cadarache and Sainte-Croix) are regularly mea-
sured within the scope of the Durance observatory (SMAVD). Analyses
are conducted on the b 2 mm sediment grain size of the fine grained
sediments (95% grain size below 500 μm). The content of metals listed
in the Regulatory law of 2006 (As, Cd, Cr, Cu, Hg, Ni, Pb and Zn) is far
below the critical value (Table 4). The content of organic pollutants
(PAH and PCB) is related to that of organic matter (Samara et al.,
2009), as indicated by the high values of PCB given for the Ste.-Croix res-
ervoir sediments at the end of the summer touristic season when the
yearly average values (b5) are below the critical value (Table 4). Most
of the organic pollutants are inerted during firing (Xu et al., 2013).
The sediment concentrations (CA-1 and VE-1) of sulphur (S) and
fluorine (F) are high, while those of in Chlorine (Cl) are below the indus-
trial range of values (Table 5). The emission values at 1100 °C are slight-
ly above (CA-1 sample) and below (VE-1 sample) the upper limit of the
industrial materials because part of the sulphur is fixed during firing.
516 F. Haurine et al. / Applied Clay Science 132–133 (2016) 508–517

Table 4 Industrial mixtures can be obtained either by incorporating some open-

Metal and organic pollutants in the dam sediments. ing agents (quartz or grinded calcined clay wastes) to correct the grain
Serre Ponçon3 Cadarache4 Sainte Croix5 Critical value6 size distribution and lower the carbonate content or by mixing sedi-
Metals - analysis conducted on the b2 μm fraction - (mg “element”/kg MS)
ments from the upstream and middle courses of the Durance, along
As 10.60 b5.0 9.9 30 with the addition of some calcined clay wastes. The specimen bars
Cd bQL b0.8 bQL 2 made with these mixtures present linear drying, firing shrinkages and
Cr 87.40 11.20 42.1 150 water absorptions in accordance with the use in brick production; the
Cu 28.70 16.27 11.9 100
mechanical strength is well satisfying.
Hg 0.04 b0.4 bQL 1
Ni 44.20 18.36 19.9 50 This methodology shows that the potential of upgrading reservoir
Pb 17.20 9.23 9.0 100 sediments in the tile and brick industry can be appraised from the
Zn 85.1° 47.35 39.9 300 MIF. The use of reservoir sediments is greater when considering a mix-
Organic pollutants - (μg/kg MS)7 ture of sediments from different sites or inert materials, including
Durance watershed grinded calcined clay wastes. The recovery of reservoir sediments
PAH totala 0,98 0.68 would contribute to reducing the raw material consumption, increasing
PCB totalb b5 22.80 the brick and tile industry wastes recycling, offering a new recovery
QL – quantification limit, NA – non-available. route for the reservoir sediments, reducing their impact on the hydro-
3
(Mazoyer, 2014b); 4(CEA, 2012); 5(Mazoyer, 2014a); 6 (Mancioppi et al., 2010); 7
power plants or watering supply, and lowering their management
(Launay, 2014).
a costs (dredging and dispersal following dredging).
PAH total corresponds to the sum of the 16 PAH of the US-EPA.
b
PCB total corresponds to the sum of the 7 regulatory congeners.

The emission values for the fluorine remain high because fluorine is not
inerted during firing. The need to install fuel gas treatment systems or
the risks of corrosion for the industrial furnace walls can be easily re-
duced by the mixing procedure.
5.4. Sediment availability
Acknowledgement
The results presented in this paper are a part of the first author's
PhD thesis. This work benefited from an ANRT support (convention
N ° 2012-093). The authors wish to thank François Thery (EDF) for
giving access to the Cadarache sample and the brick and tile industries
for providing the industrial raw materials.

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