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Geoderma 167-168 (2011) 360–368

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Geoderma
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / g e o d e r m a

Impact of lime and mineral fertilizers on mechanical strength for various soil pHs
Véronique Chaplain a,⁎, Pauline Défossez b, Ghislaine Delarue a, Jean Roger-Estrade c, d, Anthony R. Dexter e, f,
Guy Richard e, Daniel Tessier a
a
INRA, UR 251 PESSAC: Physico-chimie et Ecotoxicologie des Sols Contaminés, F-78026 Versailles, France
b
INRA, UR 1263 EPHYSE, F-33140 Villenave d'Ornon, France
c
AgroParisTech, UMR 211 Agronomie, F-78850 Thiverval-Grignon, France
d
INRA, UMR 211 Agronomie, F-78850 Thiverval-Grignon, France
e
INRA, UR 272 Sols, Ardon, F-45075 Orléans 2, France
f
IUNG-PIB, ul. Czartoryskich 8, 24-100 Pulawy, Poland

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

Article history: Application of lime and fertilizers might impact soil properties by affecting their physico-chemical
Received 21 January 2011 parameters. The focus of the Versailles 42-plots experiment that was started in 1929 has always been to
Received in revised form 18 July 2011 determine in fallow conditions the impact of mineral fertilization over time on the physico-chemical
Accepted 7 August 2011
properties of a loamy soil. This paper's aim is to assess the impact of long-term mineral fertilization on
Available online 28 September 2011
mechanical strength and soil stability. Soil samples of similar texture and bulk density were taken from the
Keywords:
42-plots site, with pH ranging from 3.5 to 8.2. Aggregate stability followed the procedure of Le Bissonnais
Compression behavior (1996). Compression tests were performed in drained conditions and short loading time (300 s). Remolded
Aggregate stability and saturated soil samples were used to focus on the impact of chemical changes due to repeated fertilization.
Mineral fertilization The pre-compression stress values Pc were derived from compression curves using various model fits
Acid soils according the shape of curve. Chemical discrepancies among soils provided from pH, organic matter and
Interfacial properties diversity of treatments. The decrease of pH reduced the cationic exchange capacity (CEC) value due to the
protonation of variable charges and retention of positively charged hydroxyl-Al polymers. Exchangeable
aluminum represented up to 90% of the CEC in acid soils as calcium ions represented from 80 to 98% of CEC
with increasing pH of neutral and alkaline soils. Compression curves showed different global shapes according
pH values and the contrasted behavior of acid soils when compared to other ones. The Pc values of highly acid
soils were much greater than other treatments (greater than 150 kPa compared with 30 kPa). Nevertheless
their Pc values decreased down to 40 kPa, when soils were air-dried before compression. Meanwhile the
deformation rate decreased when the pH dropped. This lower deformation cannot be explained by kinetic
aspects and was not sensitive to drying. So the hypothesis of a set of yield stress avoiding drainage of the
water phase and limiting soil compression was proposed. Aggregate stability tests revealed the unstable
nature of all plots especially with the highly acid soils. The size distributions of fragment were very similar for
all three tests with a narrow distribution in elementary particle class suggesting the predominance of
dispersion in fragmentation process. But we found opposite results for this soil by comparing mechanical
strength and water stability of aggregates. This contrast raised the question of the crucial role of the air-drying
step on aggregate stability measurements. A small increase of aggregate stability was observed in neutral and
alkaline soils due to calcium bridges when compared to reference plot. Such effect was not observed in
compression behavior of remolded soils. Future studies will require the use of structured soil samples; in
particular for neutral and alkaline soils to gather evidence of the effects of calcium bridges on soil stability and
mechanical strength. Our results showed the need to consider interfacial processes in the soil stability and
compression behavior and the great interest of the 42-plots experiments at INRA Versailles to relate chemical
and physical soil properties.
© 2011 Elsevier B.V. All rights reserved.

1. Introduction

The critical role of soil structure in soil quality has been recognized
for many years because it affects transport phenomena as well as
⁎ Corresponding author at: INRA, Pessac Rd 10, F-78026 Versailles, France. Tel.: + 33
biological activity inherent to soil organic matter dynamic (Six et al.,
1 30 83 37 04; fax: + 33 1 30 83 32 59. 2004), or to the fate of organic contaminant (Mamy et al., 2011). The
E-mail address: chaplain@versailles.inra.fr (V. Chaplain). structure of soil depends on soil texture and organic matter (Carter,

0016-7061/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.geoderma.2011.08.003
V. Chaplain et al. / Geoderma 167-168 (2011) 360–368 361

2004; Dexter, 2004a, 2004b). It is also affected by practices including physical properties including bulk density, water interaction, geometric
crop rotations, effects of grasses, tillage, wetting–drying, chemical mean diameter of water-stable aggregates, compression behavior after
amendments especially organic ones (see for instance Bronick and Lal, 10 years of successive applications (Intrawech et al., 1982). Tensile
2005). This work concerns the impact of mineral fertilizers and lime strength, (TS) of aggregates was measured on soils having received
on mechanical strength and water-stability of soil, both properties various fertilizers (Munkholm et al., 2002). Results showed that soils
being related to soil structure. treated with mineral fertilizers (NPK) had properties intermediate
The soil structure is basically characterized by the bulk density and between those of soils having received manure amendments, and
the dual nature of porosity divided into micro and macro pores. unfertilised soils. However the observed effects depend greatly on the
However, due to the complexity of soils and the multiplicity of processes water regime and the wet–dry cycle (Munkholm et al., 2002). The
involved in soil structure, the bulk density changes with the observation impact of NPK treatments on TS seems to be related to the dispersive
scale as described by the hierarchical concept (Braudeau and Mohtar, clay contents. This discrepancy in wet conditions might be related to
2009; Dexter, 1988; Hadas, 1987). Structure of small size samples differences in the nature and amount of bonding materials. Many
(typically less than 1 mm) are dominated by high short range variations parameters affect soil stability so, that a specific impact of NPK
of the micro porosity and could be characterized by a specific fractal treatment is hard to demonstrate. It is often low, when compared to
dimension. When the size of the samples is increased up to the the impact of other parameters, such as the presence of crop residues or
mesoscopic scale (typically from 1 mm up to 10 cm) both micro and management practices (Simansky et al., 2008). Soil aggregate stability
macro porosity participate to the global porosity (Bartoli et al., 2005). decreased with NPK treatment in the case of an acidic Alfisol under an
The fractal dimension at this scale could differ from those determined at annual soybean–wheat crop rotation (Hati et al., 2008). At a small rate,
smaller scale (Bartoli et al., 2005). Fractal properties applied at a specific liming can result in dispersion of clays, but the aggregation progresses,
range cannot be directly applied to predict soil physical properties at when the rate increases due to the contribution of Ca2+ cations.
another scale range. Those structural properties are either directly Contrasted effects of liming on aggregate stability were reported (Castro
observed or deducted from physical properties such as water retention and Logan, 1991; Roth and Pavan, 1991; Tama and El-Swaify, 1978). The
and hydraulic conductivity but rarely in mechanical behavior (Van major effects of fertilizers on soil physical properties are to improve crop
Damme, 1995). Such structural properties demonstrate the need to yields and to act on organic matter both in nature and content. But
consider the scale's complementarity in studying physical properties of addition of lime or fertilizers on soils has also a direct impact by
soil. Microstructure appears to be responsible for most of the soil modifying the chemical composition of the soil solution, its ionic
physical properties and can be well described by a single soil physical strength and in some cases soil pH. In particular, soil acidification from
parameter S (Dexter, 2004a, 2004b). Soil structure and soil–water long-term use of nitrogen fertilizers has been reported (Schroder et al.,
interaction are closely related (Braudeau and Mohtar, 2009). 2011; Stroia et al., 2011), with consequences on plant growth. All
The water-stability can be namely approached by dispersion of physico-chemical parameters influence the dispersion/flocculation
elementary particles and dried-aggregate breakdown by slaking and processes and are then expected to influence mechanical strength and
micro-cracking processes. At clays scale, the higher is the dispersive clay soil stability. Indeed chemical fertilization was found to reduce
content in water, the more unstable is the soil considered (e.g. de mechanical properties of a paddy soil (Li and Zhang, 2007).
Oliviera et al., 2005). At the aggregate scale, the higher is the mean The aim of this paper is to assess the impact of long-term mineral
weight diameter of slaked aggregate fragments, the more stable is the fertilizers and lime on mechanical strength and water stability of
soil considered (Le Bissonnais, 1996). Soil strength can be namely aggregates. For that we compared compression curves in saturated
approached by internal cohesion of saturated aggregates (small scale) conditions and dried aggregate stability in water. Soil samples were
and compression behavior usually measured at a larger core scale. taken from the 42-plots experiment in INRA Versailles, whose aim is to
Uniaxial compression curves show the relationship between stress test the long-term impact of mineral treatments on physico-chemical
applied on a soil sample and volumetric parameters such as strain, void properties of soils. Mechanical tests were performed using remolded
ratio or porosity. They have two main mechanical parameters: (i) the soil samples at a given bulk density and water saturation. Therefore, soil
pre-compression stress, Pc, beyond which plastic deformation occurs, structure can be considered as homogeneous. Results will be discussed
(ii) the slope of the virgin compression line, VCL, namely the com- as a function of chemical changes induced by repeated fertilization
pression index Cc. Pc and Cc are considered an indicator of the soil's load considering both chemical composition of water phase and interfacial
support capacity and soil resistance to compression respectively. High properties of soil.
strength of a soil structure is associated with high values of Pc.
These different approaches have been compared only infrequently.
However the macroscopic behavior of the soil is usually related to the 2. Materials and methods
behavior of individual aggregates (Blanco-Canqui et al., 2005). Soils
with high tensile strength values of aggregates offer higher mechan- 2.1. Experimental site and soil characteristics
ical resistance as a whole (Perfect and Kay, 1994). Pc values are related
to the ratio of aggregate density to bulk density of soils (Rücknagel et The 42-plots experiment in INRA, Versailles uses a loamy soil in
al., 2007). Recent detailed analysis shows that particle size and dry fallow conditions. It has been managed by the French National Institute
aggregate size distribution weakly impacts soil compression proper- for Agricultural Research (INRA). The 5 m 2 plots have received fertilizers
ties (Keller et al., 2011). or amendments every year. Ten reference plots without any treatment
Few studies have dealt with long-term effects of mineral fertilization are randomly located through the site, and 16 different treatments are
on soil stability, because most studies focused on the effect of fertilizers tested in duplicate plots. All plots are dug to 20 cm depth twice a year
on crop production and organic content of soil. Most of long-term and are systematically weeded to suppress plant cover. Since 1929, soils
experiment site involve plants that limit the impact of fertilizers. So the samples have been regularly taken from all plots, air-dried, ground and
aggregate stability was found to be not significantly affected by cropping sieved b2 mm. This collection is stored in dark conditions for further
systems and fertilizer level (Subbian et al., 2000). The increase in water analysis. The choice of treatments, at the beginning of the experiment,
stable aggregation results from increased crop yields and organic matter was made in order to be able to distinguish the effects of associated ions.
returns (Haynes and Naidu, 1998). Adding fertilizers also has direct For example, the ammonium fertilizers were respectively associated
physico-chemical effects, influencing soil aggregation with conse- with sulfate, phosphate, nitrate or chlorohydrate anions. Simple
quences on bulk density (Haynes and Naidu, 1998). The application of observation of the site shows the effect of mineral fertilization on soil
various N sources reduced the soil pH, but did not significantly affect soil structure and soil–water interactions. It also shows the influence of
362 V. Chaplain et al. / Geoderma 167-168 (2011) 360–368

nitrogen source on this impact and the role of the chemical nature of Table 2
cation (or anion) associated with fertilizer. Exchangeable cations 42-plots site Versailles 2000: H1 (0–20 cm)/H2 (25–40 cm).

The changes from the initial soil in 1929 and the reference plots in Plot Treatment CEC (Co)a b
Ca2+ b
Mg2+ Al3+ (KCl)b
1999 are (i) a decrease of soil pH from 6.3 to 5.6 (ii) a decrease of organic
H1/H2 H1/H2 H1/H2 H1/H2
carbon from 1.62 ± 1.2 to 0.7 ± 0.2 in% w/w due to the absence of plants
1 (NH4)2HPO4 6.2/8.0 0.2/0.3 0.2/0.4 6.4/7.8
(iii) a decrease of the cationic exchange capacity, (CEC) in cmol+ kg− 1
2 NH4NO3− 7.6/9.8 0.4/0.2 0.2/0.1 6.6/8.5
from 14.8 ± 0.8 to 8.7 ± 0.3 (Pernes-Debuyssier, 2003). The textures of 3 No 8.7/10.2 5.1/7.3 0.7/0.8 2.2/1.4
the reference soil measured in 1929 then in 1999 are respectively in 3 (1929) 15.3/NDc 13.3/ND 1.4/ND b 0.05
w/w%: clays 19.4 (18.4); fine silt 19.5 (19.5); coarse silt 38.7 (37.1); fine 4 superP 11.3/14.2 9.7/12.4 0.4/0.8 0.06/b0.05
sand 19.5 (21.7) and coarse sand 2.9 (3.3). Texture of others plots 5 CaCO3 13.3/14.7 13.1/14.4 0.2/0.4 b 0.05
6 CaO 13.6/14.7 13.3/14.6 0.3/ND b 0.05
showed overall the small impact of treatments on the particle size
a
distribution (Chaplain et al., 2008; Pernes-Debuyssier, 2003). The first Cationic Exchange Capacity (Cobaltihexamine method).
b
Ca2+, Mg2+, Al3+, in cmol+.kg− 1.
noticeable result of fertilizers applied on others plots is the impact on c
Not Determined.
soil pH that varies from very acid (3.5) to alkaline (8.2) depending on
the fertilizer or amendment type. Small variations in particle size
distribution between the treatments were also reported (Chaplain et al., placed inside the cylindrical cell used for mechanical measurements and
2008; Pernes-Debuyssier, 2003). then saturated on a porous membrane for 24 h. Soil cores were then
In this work, we choose five different treatments for which soil pH used for compression tests. If required core samples were put at an
ranged from 3.5 to 8.2 as the bulk density of undisturbed structured initial water potential of pF 2.5 by equilibration in a 5 bar Ceramic Plate
aggregates were quite similar from 1.42 to 1.52 Mg.m− 3 (Chaplain et al., Extractor (Soil Moisture Equipment Corp., model 1600) for one week.
2008). These plots were selected in order to minimize discrepancy in soil Shrinkage during the preliminary wet–dry cycle was systematically
structure at small scale and focus on the chemical changes induced by controlled by the height of the core given by the position of the captor of
treatment. All analyses were carried out on b2 mm air-dried samples. displacement at the beginning of the compression test (Hill and Sumner,
The treatments, the soil pH in water, the clay fraction and the total 1967; Panayiotopoulos, 1996). The bulk density 1.45 Mg.m− 3 was
organic content, (TOC) values were reported in Table 1 for all selected chosen to limit the initial shrinkage during core preparation and to
plots and both horizons used in this study: H1 correspond to the 0– permit sufficient deformation during the compression tests (Chaplain et
20 cm and H2 to 25–40 cm. The pH was measured in water by the French al., 2011). The bulk density value was also close to the bulk density of
standard method AFNOR (NF X31-103) (AFNOR, 1996). The clay fraction undisturbed aggregates.
b2 μm was extracted from soil, without destruction of organic matter, by
mechanical dispersion and sedimentation (Pernes-Debuyssier and 2.2.2. Compression curves
Tessier, 2002). The organic content was determined by elemental Uniaxial compression curves were measured for the soils using a
analysis (C&N Fison Carlo Erba). The CEC value was determined using hydraulic oedometer apparatus in drained conditions. The cell was a
the cobaltihexamine method. Values are reported for both horizons in cylinder of 50 mm diameter and 20 mm height providing lateral
Table 2 together with earth alkaline ions, exchangeable Al3+ extracted constraint. Successive uniform vertical stresses were applied: 1, 2, 5,
by a KCl solution (see Pernes-Debuyssier and Tessier, 2002, for a more 10, 15, 30, 50, 100, 200, 300, 600, 800, and 1000 kPa. Each load was
complete description of analysis). The change in pH values induced applied for 5 min, which is an intermediate time between typical
strong variations in the chemical properties of soil, in response to the geotechnical and agricultural loading times. The vertical deformation
chemical diversity of the inputs. and internal pressure in the case of saturated soil samples, were
measured each 10 s for the duration of each load. The void ratio was
calculated using a particle density value given in Table 3. The real
2.2. Compression tests density of particles is identical in all the samples collected on a same plot
except for the reference plot where a lower value (2.63 Mg.m− 3) was
2.2.1. Samples and core preparation measured in horizon 25–35 cm (Pernes-Debuyssier, 2003). Compres-
Soil monoliths were collected in 2008 in the 25–35 cm horizon, wet sion curves showed the variation of void ratio measured at the end of
sieved minimizing the drying of soils before compression tests. Other each load with the logarithm of external stress. At the end of
monoliths were collected in the 0–20 cm horizon in 2002. Soils were air- compression, the external pressure was progressively decreased with
dried, ground and sieved b2 mm and stored in the dark until 2008, the same loading time following the same but reversed successive
when mechanical tests were performed. Remolded and water saturated pressures. Again the vertical deformations were measured each 10 s for
cylindrical soil samples were used to ensure homogeneous and similar the duration of each load to draw the unloading curves. At the end of
soil structure among soils and focus on the impact of chemical changes. each unloading test, the soil sample was weighed to determine its water
Samples were made of successive layers of sieved soil and water, with a content.
maximum water content of 20% by weight. After that, soil samples were Normalized deformation was calculated from compression and
relaxation curves according to the following equation (Baumgartl and
Köck, 2004):
Table 1
Physico-chemical data of soils of 42-plots site 2000: H1 (0–20 cm)/H2 (25–40 cm).
eT = ðe−ef Þ=ðe0 −ef Þ ð1Þ
Plot Treatment Clay % w/w pH TOCa % w/w
H1/H2 H1/H2 H1/H2

1 (NH4)2HPO4 14/18 3.6/4.0 0.9/0.5 Where e0 and ef are respectively the initial and final void ratio values
2 NH4NO3− 17/19 4.5/4.1 0.7/0.5 for each test.
3 No 18/18 5.6/5.8 0.7/0.7
3 (1929) 19/NDb 6.3/ND 1.6/NDb
4 superP 17/22 7.1/7.2 0.5/0.4 Table 3
5 CaCO3 14/22 8.2/8.1 0.6/0.4 Particle density 42 plots site in Versailles 2000 (10–20 cm).
6 CaO 17/21 8.2/8.1 0.6/0.4
Plot 1 2 3 4 5 6
a
Total Organic Carbon.
b Particle density, in Mg.m− 3 2.63 2.62 2.67 2.61 2.65 2.65
Not determined.
V. Chaplain et al. / Geoderma 167-168 (2011) 360–368 363

The global deformation rate is assimilated to the difference in bulk compression curves using the sum of the standard errors in parameters
density between the start and the end of the compression test, divided of the model fit. Fitting was done using Sigmaplot and Excel statistical
by the initial bulk density. tools according to the ordinary least squares method.

2.2.3. Determination of mechanical parameters 3. Results and discussion


The method and model fit used to determine the virgin compression
line, (VCL), and calculate mechanical parameters differed according the 3.1. Effects of treatments in chemical properties of soils
global shape of compression curves: rounded, bi-linear or S-shape ones.
The classical Casagrande method was used with rounded compression The discrepancies in physico-chemical properties given in Tables 1
curves by a fourth-grade polynomial fit to determine the position of the and 2 measured between both horizons are less than the standard
point of maximum curvature as described in Cavalieri et al. (2008). A deviation estimated in reference soils. Only a small decrease of clay
bisector was drawn between the tangent at this point and a horizontal content is suspected in (Plot 1 and Plot 5) when compared to the
line. The pre-compression stress Pc was defined as the intercept reference soil. The clay mineralogy was not affected by treatment
between this bisector and VCL (Arvidsson and Keller, 2004). In the (Pernes-Debuyssier et al., 2003). A change in particle size distribution of
cases of bi-linear and S-shaped compression curves, the Pc value was the the clay fraction is also described in Plot 1 for which finest particles less
intercept of VCL with a horizontal curve taken at e0. The VCL was simply than 0.4 μm are lost (Pernes-Debuyssier and Tessier, 2004). Flocculation
obtained by linear regression in the second part of curve in the first case. by soluble Al3+ could explain the disappearance of the b0.4 μm fraction.
As it was the tangent to the compression curve at inflexion point in the Because of the longevity of the site, soil samples taken respectively in H1
second case. The Gompertz's model fit was applied to S-shape curves to (in 2000) and H2 (in 2008) horizons can be considered as similar in
determine the position of the inflexion point. Pc values were calculated terms of particle size distribution and mineral characteristics. Chemical
from the model parameters as described in Gregory et al. (2006) and discrepancies among soils provide from the pH of soil, organic matter
Keller et al. (2011). and diversity of fertilizers including the effect of anions in the case of
ammonium treatments (Plots 1 and 2).
2.3. Aggregates stability in water The decrease in pH reduces the CEC value due to the protonation of
variable charges and retention of positively charged hydroxyl-Al
The aggregate stability was measured according to the unified polymers. Exchangeable aluminum represented up to 90% of the CEC
methodology proposed by Le Bissonnais (1996) on 3–5 mm air dried at the low acid pH. In neutral and alkaline soils, calcium ions represent
aggregates AFNOR (NF X31-515) (AFNOR, 2005). This method is a from 80 to 98% of the CEC with increasing pH. Both clays and organic
combination of three tests, that take into account two basic mechanisms matter contribute to the adsorption of NH4+ (Gouveia and Eudoxie,
responsible for the fragmentation of aggregates under the action of 2002; Liu et al., 2008). The adsorption was also pH-dependent as
water, namely: slaking (tests I and III) and mechanical breakdown of negative charges of soil promote the affinity of soil towards NH4+ (Liu et
saturated aggregates (test II). In the former case, fragmentation is due to al., 2008) and usually fixation increased with pH. The retention of
the compression of air trapped in the aggregates following immersion in cations in acid soils including forest soils cannot be described by simple
water. Tests I and III correspond to fast and slow wetting processes exchange phenomena. The need of a new perspective was reported in a
respectively. In the latter case (test II) slaking is prevented by a recent review (Ross et al., 2008). In solution both NH4+ and Al 3+ may
preliminary wetting of aggregates in ethanol before immersion in water. interact with organic matter, especially with aromatic cycles with
Fragmentation is obtained by stirring. After the fragmentation treat- possible drastic changes in the organic matter conformation (Keiluweit
ment, the granulometric distribution of the remaining aggregates was and Kleber, 2009; Schlautman and Morgan, 1993).
determined by dry-sieving. Seven classes were defined: N2 mm; 1–
2 mm; 0.5–1 mm; 0.2–0.5 mm; 0.1–0.2 mm; 0.05–0.1 mm; b0.005 mm. 3.2. Mechanical behavior of soil samples at short loading time
A detailed description of the procedure is also given in Li and Zhang
(2007). The mass of the aggregate samples was 5 g per test. Tests started The mean compression curves at saturation are drawn in Fig. 1
by an oven-drying step at 40° for 24 h. Results are expressed in% weight for highly acid soils (Plot 1) and acid soils (Plot 2) and then com-
of the total weight (% w/w) for each size class and by the ratio pared with the reference soils (Plot 3) in full line. These curves
[b50 μm]/[0.1–1 mm] value. Samples and measurements were made in showed all different global shapes observed among soils. The highly
2000 in the 0–25 cm horizon. acid soils are characterized by rounded compression curves but
unfortunately no local maximum in curvature is found by fitting.
2.4. Statistical analysis
0,9
The spatial variability of physico-chemical properties was esti-
mated on the reference plots to limit the number of analyses. For that,
ten samples dating from 1929 of any reference plots were taken into 0,8
the collection and 10 samples collected in 2000 into a single reference
Void ratio, e

(Plot 3). Measurements performed on the initial samples gave a 0,7 Highly acid
relative standard deviation of 7% for TOC and CEC values. This variability
slightly increased with time. The variability within a single plot gave a
relative standard deviation of 3% for TOC and CEC and 5.8% for the clay 0,6
Reference
fraction. The impact of treatment is determined by comparing the
difference between mean values among plots and reference soils on one 0,5
hand and the standard deviation previously measured on reference
Acid
plots on the other hand.
0,4
All mechanical and aggregate stability tests were performed as three 1 10 100 1000 10000
replicates with the same initial conditions. Results represent mean
External pressure, kPa
values; standard deviation is also reported. The number of replicates
being too low to use complex statistical tools, the set of results of Pc Fig. 1. Compression curves at water saturation. Remolded soil samples 1.45 Mg.m− 3
values is given. Standard error in the Pc value was estimated from each collected in the (25–35 cm) horizon in 2008: ▲ Plot 1; Δ Plot 2; ● Plot 3.
364 V. Chaplain et al. / Geoderma 167-168 (2011) 360–368

Such gradual transition between the elastic and plastic deformation A


1,0
were observed (Keller et al., 2011 and references inside). To limit
the uncertainty associated with the graphical estimation, we per-
formed additional measurements in unsaturated conditions with

Normalized void ratio, e*


0,8
Plot 1 (Rücknagel et al., 2010). The compression curves obtained
obeyed a bi-linear model and determination of Pc was easy. Values of
0,6
Pc are thought to be a good indicator of mechanical behavior in
saturated conditions because the water content measured at pF 2.5
is very close to saturation. In acid soils, a bi-linear shape of compres- 0,4
sion curves led to an accurate determination of Pc. The compression
curves for the other plots are S-shaped. The set of Pc values are
0,2
reported for all plots in Table 4. The regression coefficient values
were always greater than 0.998 and for each fit, the sum of variation
coefficient of parameters was around 10%. Overall we found the 0,0
greater mechanical stability of the highly-acid soils (Plot 1), when 1 10 100 1000 10000
compared with other soils of similar texture, density and water External pressure, in kPa
content but various pH for which Pc values were lower than 40 kPa.
Furthermore, we observed that the Pc values of Plot 1 seem to be B 1,0
very sensitive to the value of e0. Indeed they ranged from 113 to

Normalized void ratio, e*


220 kPa when the e0 value varied from 0.867 to 0.817. The small 0,8
number of replicates avoids a rigorous and quantitative comparison
among others soils although the normalized compression curves in
0,6
Fig. 2A distinguish their mechanical behavior. We can just highlight
the small Pc value of Plot 5 equal to 15 ± 3 kPa. Increasing exchange-
0,4
able calcium increased the shear strength of wet aggregates (Dexter
and Chan, 1991). The use of remolded soils certainly limits in this
work such impacts. The normalized unloading curves in Fig. 2B 0,2
clearly show the similar behavior of all plots including Plot 1.
The mean deformation rate during compression is expressed as a 0,0
1 100 10000
function of pH in Fig. 3. It is rather constant from alkaline pH to low
acid ones and then continuously decreases in more acid soils. The External pressure, in kPa
short value (300 s) of the duration of each step during the compres-
Fig. 2. Normalized compression curves (A) and relaxation curves (B). From
sion test could explain such a decrease with highly acid soils, if the experiments in Fig. 1 ▲ Plot 1; Δ Plot 2; ● Plot 3; ο Plot 4; □ Plot 5; ■ Plot6.
“equilibrium” in e value is not reached. The internal pressure measured
during compression increased up to a plateau region (data not shown)
for all soils except the acid ones (Plot 2). But the value of pi at this plateau region also varied among soils: it was low (about 10 kPa), in highly acid
soils (Plot 1), zero for acid soils (Plot 2) and around 25–40 kPa for all
Table 4 others soils, including the reference one. Those results illustrate the
Precompression stress values from Fig. 1: 42 plots site Versailles 2008, 25–35 cm. importance of kinetic aspects in compression tests.
Plot Initial void ratio Pc, in kPa Model
3.3. Kinetic aspects in compression tests
Plot 1
Unsaturated 0.817 220 Bi-linear
Id 0.830 155 id
We detailed here the kinetic aspects of each step of the compression
id 0.845 143 id test by calculating, each time, the normalized void ratio. The normalized
id 0.851 165 id deformation e* measured 30 s after the beginning of each step, is
id 0.867 113 id represented in Fig. 4 as a function of the pressure applied at each stage
Plot 2
for acid and alkaline plots and compared to the reference plot. For all
0.800 19 Bi-linear
0.806 19 id plots, e* reached a minimum value when the external pressure is
0.849 15 id 600 kPa and again increases, when the external pressure is still
Plot 3 increased. In any case, the e* values are lower in acid plots than in
0.811 27 Gompertz
0.820 26 Id
0.823 26 Id 0.4
0.843 20
Plot 4
0.774 16 Gompertz
0.3
Deformation rate

0.783 14 Id
0.787 20 Id
0.2
0.792 16 Id
Plot 5
0.817 18 Gompertz
0.1
0.867 11 Id
0.871 17 Id
0.902 13 Id
0
Plot 6
3 5 7 9
0.822 22 Gompertz
pH
0.826 23 Id
0.842 25 Id
0.843 30 Id Fig. 3. Deformation rate as a function of soil pH. Remolded soil samples 1.45 Mg.m− 3
collected in (25–35 cm) horizon in 2008. From experiments in Fig. 1.
V. Chaplain et al. / Geoderma 167-168 (2011) 360–368 365

Normalized deformation e *, after 30 s


Fig. 5A and B shows for all plots, the typical time variations of pi* when
1.0
the external pressure was 600 and 1000 kPa respectively. Again
kinetic results differ among soils. The internal pressure measured in
0.8
acid soils (Plot 2) quickly fell to zero for any steps as well as the rapid
change in deformation shown in Fig. 4. Other neutral and alkaline soils
0.6 clearly show that equilibrium is not reached suggesting a long-time
Alkaline
variation with likely consequences on long-time deformation. Some
0.4 Reference curves (Plots 4 and 6) seem to have an asymptotic value (full line)
Acid whereas others (Plots 3 and 5) seem to decrease linearly with time up
0.2 to zero. However experiments using larger time measurements are
required to discuss this point because some plateau region were also
0.0 observed in the decrease of pi with time showing the non-linearity
10 100 1000 10000 and complexity of processes involved in the decreasing of internal
External pressure, in kPa pressure. The case of the highly acid soils was still different. Indeed an
asymptotic value (10 kPa in both cases) was observed in two opposite
Fig. 4. Normalized deformation 30 s after the beginning of each step. Remolded soil
manners: a decrease or increase of pi with time. The time dependence
samples 1.45 Mg.m− 3 collected in the (25–35 cm) horizon ▲ Plot 1; ● Plot 3; □ Plot 5.
From experiments in Fig. 1. of void ratio reveals the time required for exudation of pore fluids. It
depends on the hydraulic conductivity of soil and its change during
compression but also on the ionic interactions at the water solid
alkaline plots. Such differences in kinetics illustrate the influence of interface. The short time variations of pi may be related to the change
interfacial properties on compression process even at the short time of macro porosity induced by compression as long time variations
scale studied here. may be rather linked to the change in the microstructure. The real
The internal pressure usually increased up to a maximum pimax contribution of ionic interactions is very little understood.
and then decreased (there was just one exception with Plot 1) in These time variations of deformation and internal pressure may
response to the application of the constant external pressure. For each have consequences on the mechanical parameter values. In our
soil, the pimax, value varied with the value of external pressure applied experiments, acid plots change shape much faster than neutral or
with a maximum when the external pressure was equal to 600 kPa. basic ones. Similar results were described in literature, showing that
This maximum point also corresponds to the maximum of deforma- variation in loading time from 10 to 120 min by step, did not affect the
tion in Fig. 4. To enhance comparison between soils, we defined the pre-compression stress values with acid soils around pH 5.5 (Peng et
normalized internal pressure pi* by the ratio between the internal al., 2004). Some other results show that very short loading times
pressure at time t and pimax. Values were calculated for each step, (30 s) influence the Pc value, compared to a static load approach of
10 min (Krümmelbein et al., 2008). No effects were noticed between
30 and 120 min on mechanical parameters (da Veiga et al., 2007) in
acid and neutral soils. Duration of 30 min is often the selected option
A in literature (Keller and Arvidsson, 2007). In our work, long-time
Normalized internal pressure

1 variations are expected, especially with neutral and alkaline soils. An


increase of the duration of step might well highlight differences in
0.75 P = 600 kPa mechanical behavior of basic plots, compared to plots having a pH
close to neutrality, with a probable decrease of mechanical resistance
to compression. Additional experiments are then required but such
0.5
long time variations were previously observed on granular materials
(Rabia et al., 2010).
0.25 At the end the lower deformation of acid soils (Fig. 3) cannot be
attributed to a kinetic aspect. The water content of soil sample (Plot 1) at
the end of compaction is high 26± 0.1 g/g when compared to others
0
0 100 200 300 (21.6 ± 0.2 in plot 2 and 20.1 ± 0.3 g/g in others). The water was
Time, s confined inside the soil sample where drainage is fast but limited. The
incompressibility of soil water should limit the global deformation of
B soil sample during the compression tests. Two hypotheses can be put to
explain the limited drainage. The first proposes a non-linear flow of the
Normalized internal pressure

1
water phase and the set of a yield stress below which water phase did
not flow. The second is related to the evolution of soil structure during
0.75
compression. It suggests that the closing of conducting pores can be
described as a percolation model, for which closing of a few pores can
0.5 induce a significant reduction of hydraulic conductivity. The former
hypothesis appeared as the most probable. In the case of acid soils (Plot
P = 1000 kPa 2) both time variations could suggest the efficiency of drainage to
0.25
reduce internal pressure and the absence of microstructure changes on a
larger time scale.
0
0 100 200 300 3.4. Aggregate stability in water
Time, s
The values of the [b50 μm]/[0.1–1 mm] ratio are given in Fig. 6 for
Fig. 5. Temporal variation of the normalized internal pressure at constant load (A) 600 kPa
and (B) 1000 kPa respectively during experiments described in Fig. 1. Red lines (acid soils:
each test and all plots. They confirm unstable feature of all soils as
full lines Plot 1; dashed line Plot 2), black ones (neutral soils: dashed line Plot 3; full line already mentioned in Pernes-Debuyssier and Tessier (2004) from the
Plot 4) and green lines (alkaline soils: full line Plot 5; dashed line Plot 6). N200 μm size fraction remaining after the stability tests. The highly acid
366 V. Chaplain et al. / Geoderma 167-168 (2011) 360–368

2.5
a narrow pore size distribution, with a mean value that depends on
bulk density. However the low internal cohesion measured at satu-
Ratio [<50 µm]/[0.1-1mm]

2.0 ration in test II, seems to be in contradiction with the higher mechan-
ical stability observed at the core scale.
1.5 In neutral and alkaline soils, dispersion process is counteracted by
the presence of calcium ions, which promote flocculation of clay, the
exchangeable Mg promoting the CaCO3 dissolution. Calcium bridges
1.0
have crucial impacts on the formation and stability of aggregates with
consequences on hydraulic conductivity (Wuddivira and Camps-Roach,
0.5 2007). They increased the stability of structured aggregates of Plot 4 to
Plot 6 and confirm the need to perform mechanical tests using undis-
0.0 turbed soil cores.
Plot 1 Plot 2 Plot 3 Plot 4 Plot 5 Plot 6

Fig. 6. The ratio [b50 μm]/[0.1–1 mm] values in % w/w. obtained during three aggregate 3.5. Effects of drying on mechanical properties
stability tests: dotted test I, horizontal lines test II, dense dotted test III for all Plots as
indicated on the Fig. The normalized compression curves are drawn in Fig. 8. The repeated
wet–dry cycles of the top surface and the long term storage of soil
soils (Plot 1) appeared as the most unstable soil, due to its overall samples (8 years) lessens the differences in mechanical behavior
highest value for this ratio in every test. All others plots (Plots 2–6) between plots and affects the global shape of compression curves of
showed a decrease of the ratio values from tests I and III indicating the acid soils: from a round to bi-linear shape for highly acid soils (Plot 1)
contribution of interfacial properties in fragmentation process. But and from a bi-linear to S-shape for (Plot 2). Mechanical behavior of other
overall, the discrepancies observed among soils are of very low soils is still characterized by an S-shape compression curve. The global
magnitude, when compared to the reference soil. Except Plot 1, all shape of compression curves is mainly determined by the coupling
soils presented a broad size distribution of fragments in test II indicating between mechanical deformation of the solid phase (related to aggre-
a relative high level of cohesion in saturated conditions. To enhance our gation) and drainage (related to hydraulic conductivity through the
understanding of the atypical mechanical behavior of Plot 1 we have porosity) (Horn, 2003). For a given soil, compression curves changed
drawn on Fig. 7 the size distribution of fragments of aggregates over the from an S-shape, round and bi-linear compression curves with increas-
entire range of textural classes for all three tests. This figure shows first, ing values of the bulk density. The rounded shape appeared at water
very similar distributions between tests and second, a narrow distri- saturation, when drainage is the limiting factor (Chaplain et al., 2011). In
bution towards the finer fraction. Those two juxtaposed characteristics this paper, the bulk density was maintained constant the pH being the
are usually associated with the predominance of dispersion in the variable parameter. Discrepancies in the global shape of curves reveal
fragmentation process (Amezketa, 1999; Le Bissonnais, 1996). Alumi- discrepancies between hydraulic conductivity mainly attributed to
num polymers also showed a high efficiency in aggregates stability due interfacial properties due to the relative homogeneity of structure of
to their high point of zero charge. In oxisols, the clay dispersion induced remolded soils at core scale. The changes in the global shape of com-
by low input energy was also pH dependent, its minimum value pression curves induced by air-drying reveal that air-drying improves
corresponding to the zero points of charge which varied from 3.5 to 7 in the drainage of both acids soils.
that study (Bartoli et al., 1992a, 1992b). Organic matter also participates The set of Pc values is given for all plots in Table 5, with a variation
to the stability of micro-aggregates. A positive effect is attributed to coefficient value of about 10%. Overall, we note the drastic decrease of Pc
the formation of a hydrophobic coating around aggregates, reducing from typically 200 to 40 kPa with highly acid soils (Plot 1). The mechan-
wetting rate and consequently the sensitivity to slaking. The hydro- ical parameters of others soils are quite unchanged when compared to
phobic/hydrophilic nature of organic matter was then implied in aggre- no-air-dried soils. Drying is known to enhance soil hydrophobicity
gate stability. The determination of anionic exchange capacity of soils (Klitzke and Lang, 2007) according a temperature dependent process
should be helpful to understand behavior of acid soils. (Bayer and Schaumann, 2007). Furthermore the conformational
Furthermore a significant correlation between median pore dia- changes in soil organic matter during drying result from a competition
meter and median aggregate size were established (Lebron et al., between electrostatic and polar interactions in a given physico-chemical
2002). Nasr and Selles (1995) stipulated that the distribution of soil environment (Chassenieux et al., 2000). Then changes in pH both affect
structural units controls the pore size distribution. The soil structure the soil hydrophilic/hydrophobic balance and the impact of drying. The
of Plot 1 was probably particularly homogeneous and characterized by change in water affinity of solid surfaces after drying may affect the

1.0
60
Normalized void ratio, e*

0.8

40 Plot 1
w/w, in %

0.6

0.4
20

0.2

0
0.0
m

m
m

1 10 100 1000 10000


2

.1

5
1-

5-

0.

0.

0
>

-0

0.
2-

1-
0.

05

0-

External pressure, kPa


0.

0.

0.

Fig. 7. Granulometric distribution in % w/w. for the three tests; dotted test I, horizontal Fig. 8. Normalized compression curves for air-dried soils ▲ Plot 1; Δ Plot 2; ● Plot 3;
lines test II, dense dotted test III Plot 1 2000 (10–20 cm). o Plot 4; □ Plot 5; ■ Plot6.
V. Chaplain et al. / Geoderma 167-168 (2011) 360–368 367

Table 5 soils and more generally of the role of chemical properties in soil
Precompression stress values in Fig. 8 42-plots site Versailles 2000 (0–20 cm). structure stability and mechanical strength with both agronomic and
Plot Initial void ratio Pc, in kPa Model environmental consequences.
Plot 1
0.819 59 Bi-linear
0.825 46 id
Acknowledgments
0.834 40 id
0.839 50 id This work was carried out with the financial support of the «ANR—
0.856 49 id Agence Nationale de la Recherche—The French National Research
Plot 2
Agency» under the «Programme Agriculture et Développement
0.805 44 Gompertz
0.809 40 id Durable», project «ANR-05-Padd-0.13». The authors would like to
0.817 32 id thank the French Programmes GESSOL2 from the Ministry in charge of
0.823 36 id Environment and ADD from the National Research Agency for their
0.834 44 id support to the DST project (Soil degradation due to compaction) in
Plot3
0.835 38 Gompertz
which the work has been done. Authors would like to thank Dr A.
0.844 45 id Pernes-Debuyssier and SNST Scories France for the financial support
0.857 37 id of her thesis in 2003. The authors thanks both reviewers for their
Plot4 constructive comments and Dr. J-M. Thomas for helpful and con-
0.772 46 Gompertz
structive discussions on long-term experimental sites. Authors would
0.785 27 id
0.800 46 id like to thank S. Breuil and J-P. Pétraud for maintaining the 42-plots site
Plot 5 in INRA, Versailles.
0.771 43 Gompertz
0.79 38 id
0.802 43 id References
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