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Despite the large number of studies concerned with microbially induced carbonate precipitation
(MICP) on soils, little attention has been paid to the effect of the chemical concentration used in the
treatment on the precipitation pattern of calcium carbonate and their influence on engineering
properties of MICP cemented soils. In this study, unconfined compressive strength tests were
conducted on sand samples treated using 0.1, 0.25, 0.5 and 1 M ureacalcium chloride solutions. It
was found that, although the strength of tested samples all increased after MICP treatment, the
magnitude of this increase depended on the concentration used in the treatment and that the use of a
low-chemical-concentration (i.e. urea and calcium chloride) solution resulted in stronger samples.
Permeability test results showed that the use of a high-ureacalcium chloride-concentration solution
resulted in a rapid drop in permeability at the early stage of calcite precipitation, whereas the use of a
low-chemical-concentration solution was found to result in a more gradual and uniform decrease in
permeability. This observed effect of chemical concentration on the strength and permeability of
MICP cemented soils can have implications for the design of MICP for field applications.
KEYWORDS: ground improvement; laboratory tests; microscopy; permeability; soil stabilisation; stiffness
331
332 AL QABANY AND SOGA
reactants (urea and calcium chloride (CaCl2 )) injected to
samples. Results showed that, below a urea and calcium
chloride input rate of 0.042 mole/l per h and for a bacterial
optical density (OD600 ) between 0.8 and 1.2, the chemical
efficiency remained high and the amount of precipitation
was not affected by the treatment chemical concentration.
However, it was found that, although the external appearance
of cemented samples using MICP was similar, the calcium
carbonate precipitation pattern at the pore scale was found
to be affected by the chemical concentration adopted in the
treatment. Cemented samples treated using ureacalcium
chloride concentrations varying from 0.1 M to 1 M were
examined microscopically; some scanning electron micro-
scopy (SEM) images taken in the study are shown in Fig. 1.
In that study, it was found that the use of a solution of lower
chemical concentration in MICP treatment resulted in better
200 m
distribution of calcite precipitation, with a typical crystal (a)
size of 35 m for the 0.25 M samples. For these samples,
calcite crystals had a similar size, were very well distributed
spatially and covered the sand grains contact areas uni-
formly. As the chemical concentration increased, it was
found that both the uniformity of distribution and crystal
size decreased. For example, the calcite crystal size was
found to be as high as 35 m in the 1 M samples. The
precipitation of calcium carbonate in MICP is a complex
process, because many variables such as chemical concentra-
tions, bacterial activity and the presence of organic macro-
molecules such as enzymes could all affect the formation of
the calcium carbonate crystals, as discussed in Al Qabany et
al. (2012).
Following this previous work, the main objective of the
work presented in the current paper is to examine the effect
of using different chemical (namely urea and calcium chlor-
ide) concentration solutions on the increase in strength and
reduction in permeability of MICP cemented sand samples. 200 m
(b)
It is hypothesised that different calcite precipitation patterns
observed at the micro-scale would have an effect on the
overall mechanical and hydraulic properties of the cemented
samples.
EXPERIMENTAL WORK
Bacterial media and chemical concentrations
Sporosarcina pasteurii (American Type Culture Collection
(ATCC) 11859) was used in all tests conducted in this study.
Cells from the frozen stock were grown on ATCC 1376
ammoniumyeast extract (NH4 YE) medium plates (20 g
yeast extract, 10 g of ammonium sulphate ((NH4 )2 SO4 ) and
20 g of agar in 0.13 M Tris buffer in pH 9.0). Bacteria were
then harvested and grown in an ammoniumyeast extract
liquid medium (usually for 2436 h) to an optical density of
0.81.2 (OD600 ) (107 cells/ml) before they were injected 500 m
(c)
directly into the samples. Abiotic (without bacteria) bottles
of media were prepared and incubated under the same Fig. 1. Scanning electron microscopy images of samples going
conditions as control samples to check for contamination through different chemical treatments: (a) 0.25 M at 100 kg/m3 ;
and to ensure that the growth obtained in the remaining (b) 0.5 M at 73.5 kg/m3 ; (c) 1 M at 70 kg/m3
inoculated liquid media was indeed only S. pasteurii.
Bacteria were only introduced to the samples either during
packing (where sand was poured in bacterial solution di- (NaHCO3 ) per litre of deionised water for stabilisation of
rectly into rigid cells to facilitate sand compaction for small the pH of the solution before injections. 0.25, 0.5 and 1 M
samples) or in an initial injection (where sand was packed ureacalcium chloride concentrations were used in order to
dry into the cells followed by injection of two pore volumes assess the effect of using different chemical concentrations
of deionised water to ensure saturation of the samples, then on the change in permeability with cementation, and 0.1 M
injection of one pore volume of bacterial solution). This was ureacalcium chloride concentration was added to this range
followed by chemicals only in all subsequent injections. The for the strength tests. Chemical retention time in the samples
test liquid media used for chemical injections contained an (time between injections) was determined based on the con-
equimolar amount of urea and calcium chloride, in addition clusion of a previous study to ensure full chemical reaction
to 3 g nutrient broth as a nutrient source for bacteria, 10 g (Al Qabany et al., 2012) and the retention times adopted
ammonium chloride (NH4 Cl), and 2.12 g sodium bicarbonate were 6, 12 and 24 h for the 0.25, 0.5 and 1 M ureacalcium
EFFECT OF CHEMICAL TREATMENT USED IN MICP ON PROPERTIES OF CEMENTED SOILS 333
chloride solutions, respectively. Different chemical treat- large number of samples to be treated at the same time. UCS
ments used in the study are summarised in Table 1. The tests are commonly used to characterise the strength property
total amount of chemicals introduced to any specimen in of cemented soils; a total of 60 samples were tested in this
different experiments was based on chemical stoichiometric study. Much of the experimental work with cemented soils
calculations, and the amount of precipitation targeted in each reported in literature has been carried out using this type of
sample varied from 40 to 160 kg calcium carbonate per test (Consoli et al., 2009), which allowed comparison of data.
cubic metre of sand. This was assuming that all injected A Wykeham Farrance constant-displacement mode UCS
urea and calcium chloride precipitated as calcium carbonate, machine was used for testing. After MICP-induced cemented
which was verified by measuring the amount of precipita- samples were created in the same manner as for the per-
tion. This was done by adding hydrochloric acid (HCl) and meability tests, they were taken out of the moulds and any
calculating the weight difference of the sample before and irregularities at the two ends of the samples were removed
after dissolving the precipitated calcium carbonate. to ensure that they could be uniformly loaded. Samples were
loaded at a rate of 1.14 mm/min (BS EN 123903:2002
(British Standards Institution, 2002)). During testing, they
Permeability tests were placed in plastic bags to preserve all the pieces of the
A rigid wall permeability test set-up was used for measur- samples after they were broken. After the completion of the
ing permeability during the bio-cementation process. In total, tests, the amount of calcite cementation was measured.
30 samples were tested and samples had different amounts
of calcite precipitation produced by different ureacalcium
chloride concentrations (0.25 M, 0.5, 1 M). British standard RESULTS
grade D silica sand was used in all tests conducted in this Samples extracted from the rigid cells (shown in Fig. 2)
study (d50 165 m, d90 250 m, maximum void ratio were found to be fully cemented and also had very high
0.9875 and minimum void ratio 0.585). The sand was efficiency, a similar finding to previous studies (Al Qabany,
placed inside rigid cells (D 100 mm, L 250 mm) by dry 2011). The chemical efficiency, which is defined by the
pluviation. The dry relative density was varied between 0.2 percentage of injected urea and calcium chloride that pre-
and 1 to examine the density effect and a confining pressure cipitate as calcium carbonate, was found to vary from 70%
of 20 kPa was applied to the samples. Permeability measure- to 100% for all samples treated by 0.25 and 0.5 M urea
ments were carried out during various stages of chemical calcium chloride solutions. In contrast, the samples treated
injections, such that change in permeability was measured at by 1 M ureacalcium chloride solution had significantly
different amounts of precipitation. Permeability value was lower efficiencies of around 20%. This may be attributed to
obtained by measuring the pressure difference across the the crystal morphology of the precipitated calcium carbo-
sample at constant flow conditions. Injections were made nate, as discussed in a previous study (Al Qabany et al.,
from the bottom of the sample using a peristaltic pump and 2012). The use of chemical concentrations of 1 M and larger
the effluent solution was allowed to overflow at the top of in MICP treatment was found to result in the precipitation
the cell during injections, such that the effluent level was of a less stable form of calcium carbonate (namely vaterite),
constant at all times. Porous stone was placed at both ends which may be flushed out during injections after precipita-
of the sample in order to ensure uniform flow through the tion. This form of calcium carbonate (as confirmed by
samples. When the permeability of soil becomes small, rigid energy dispersive X-ray (EDX) analysis) was reported to be
cells may not be suitable, because the flow along the wall vaterite based on its spherical shape observed microscopi-
can be bigger than the flow through the soil sample. How- cally. Also, van Paassen (2009) reported the spherical-shaped
ever, as shown in the results, this was not found to occur calcium carbonate resulting from MICP to be vaterite based
because the chemical efficiency of the samples was consis- on X-ray diffraction (XRD) analysis.
tently high at all levels of cementation and hence there was Figure 3 shows the reductions in permeability with in-
no chemical loss as a result of non-uniform flow. Visual crease in the amount of calcium carbonate precipitation for
observation of cemented samples also showed no difference three different concentrations. Although the degree of reduc-
along the cross-section of the samples. After completion of tion was variable, even for samples treated with the same
the tests, the amount of calcite cementation was measured. chemical concentration, large reduction occurred at the
beginning of the precipitation. This indicated that larger
pores where the chemical solution was accessible were
Unconfined compressive strength tests reducing their pore sizes by the development of calcite
Unconfined compressive strength tests were conducted on precipitation (see Discussion section).
oven-dried samples with different amounts of calcite precipi- As shown in Fig. 3, permeability tests were performed on
tation produced by solutions of different ureacalcium chlor- samples with different relative densities (RDs). Both loose
ide concentrations (0.1, 0.25, 0.5 and 1 M). Tests were and dense samples showed reduction in permeability with
performed on samples of two different sizes: (a) D 100 mm increase in the amount of calcium carbonate precipitation.
and L 250 mm and (b) D 35.4 mm and L 100 mm, However, for most samples with RD greater than 0.7, the
where the smaller size had a simpler set-up and enabled a decrease in permeability was not as significant as the more
loosely packed samples (i.e. over 90% reduction for many
samples of RD 60%). Furthermore the rates of permeabil-
Table 1. Chemical treatments used in the study ity reduction on samples with higher RDs were greater than
those with low RDs. This implies that MICP as a permeabil-
Chemical concentration Frequency Normalised ity reduction method is more effective for loose samples
(retention time): input rate: than for dense samples. Nevertheless, there was large scatter
h mole/l per h and uncertainty in the results obtained, so further study is
required to improve the consistency of the treatment.
0.1 M urea and calcium chloride 3 0.033
In Fig. 4, the measured permeability values at different
0.25 M urea and calcium chloride 6 0.042
0.5 M urea and calcium chloride 12 0.042 levels of calcium carbonate precipitation are normalised with
1 M urea and calcium chloride 24 0.042 the initial permeability value before the MICP treatment,
and the normalised permeability values are plotted against
334 AL QABANY AND SOGA
000020
RD 026 RD 057
RD 065 RD 069
RD 074 RD 074
000015 RD 075 RD 082
Permeability: m/s
RD 083 RD 091
000010
000005
0
0 1 2 3 4 5 6 7 8 9 10
Calcium carbonate: %
(a)
000020
RD 054 RD 062
RD 067 RD 071
000015 RD 078 RD 100
RD 081 RD 083
Permeability: m/s
RD 100 RD 100
RD 100 RD 100
000010 RD 100 RD 100
000005
0
0 1 2 3 4 5 6 7 8 9 10
Calcium carbonate: %
(a) (b)
000020
RD 083
RD 080
RD 083
000015 RD 088
Permeability: m/s
RD 090
000010
000005
0
0 1 2 3 4 5 6 7 8 9 10
Calcium carbonate: %
(c)
10
09
025 M 05 M
08 1M
Normalised permeability
07
06
05
04
(b) 03
02
Fig. 2. Cemented sample after extraction from rigid cells for
(a) 0.25 M chemical treatment and (b) 1 M treatment 01
0
the amount of calcium carbonate precipitation for samples 0 1 2 3 4 5 6 7 8
Calcium carbonate: %
with initial relative density between 0.75 and 0.85. For most
samples, permeability was reduced to between 10% (for Fig. 4. Decrease in normalised permeability with calcium carbo-
0.25 M samples) and 30% (for 1 M samples) of its initial nate precipitation for three chemical concentrations
EFFECT OF CHEMICAL TREATMENT USED IN MICP ON PROPERTIES OF CEMENTED SOILS 335
3000
value. It was also found that the higher the concentration of 01 M treatment
the chemical solution was, the faster the reduction in per-
Unconfined compressive
2500 025 M treatment
meability happened before it became constant. On average,
1800
1600 RD 0809
Unconfined compressive
1400 RD 0708
strength, UCS: kPa
1200 RD 0607
1000 RD 0506
800
600
(b) 400
200
Fig. 7. Schematic diagram of pore clogging as a result of MICP 0
using (a) a low chemical concentration and (b) a high chemical 0 20 40 60 80 100 120 140 160 180 200
concentration Calcium carbonate precipitation: kg/m3
(a)
3000
RD 091
Unconfined compressive
2500 RD 0809
strength, UCS: kPa
low overall chemical efficiency were obtained for these 2000 RD 0708
samples, as reported in Al Qabany et al. (2012). RD 0607
When a low-concentration solution was used for the MICP 1500
treatment, precipitation took place at pore throats (contact
points) where there was an abundance of bacteria and 1000
nutrients, as reported by DeJong et al. (2010). This is 500
supported by the fact that, for most of these samples,
precipitation was more distributed throughout the entire 0
sample and no sudden clogging occurred. 0 20 40 60 80 100 120 140 160 180
Calcium carbonate precipitation: kg/m3
(b)
Effect of density on UCS increase with calcium carbonate Fig. 8. Unconfined compressive strength plotted against calcite
Unconfined compressive strength test results demonstrated precipitation based on relative density for a single chemical
that the magnitude and the rate of UCS increase with treatment: (a) 0.5 M; (b) 0.1 M
EFFECT OF CHEMICAL TREATMENT USED IN MICP ON PROPERTIES OF CEMENTED SOILS 337
01 M treatment Ivanov et al. (2010)
Comparing strength from ureolytic MICP to other soil
improvement techniques 025 M treatment Ismail et al. (2002b)
When the UCS test results produced in this study were 05 M treatment Aberdeen soil
compared with those reported in previous studies, it was (Muhunthan & Sariosseiri, 2008)
found that similar patterns of increasing strength were 1 M treatment Everet soil
(Muhunthan & Sariosseiri, 2008)
obtained. Fig. 9 shows that the 0.5 M sample data are 4000
similar to those produced by van Paassen (2009) who used 3500
the same concentration solution but different experimental
Unconfined compressive
set-up. Whiffin et al. (2007) created cemented samples using 3000
10 000 (van Paassen, 2009) of soil, and high variation is expected when these factors are
8000 changed, in particular at low cement content conditions.
In addition to Portland cement, Ismail et al. (2002b)
6000
tested soil samples cemented by mixing gypsum or treated
4000 by chemically induced calcite precipitation (as opposed to
microbially induced). They found that, in order to achieve
2000
the same UCS value obtained from mixing Portland cement,
0 a larger amount of gypsum and a smaller amount of calcite
0 100 200 300 400 500 600
were needed. For example, 3.5% calcite, 8% Portland
Calcium carbonate precipitation: kg/m3
cement and 10% gypsum were required for UCS value of
Fig. 9. Unconfined compressive strength plotted against calcium 500 kPa, whereas 7% calcite, 15% Portland cement and 20%
carbonate precipitation for MICP in the present study compared gypsum were required for UCS value of 2500 kPa. It is
to van Paassen (2009) (0.5 M) expected that calcite precipitation using MICP would be
similar to the chemically induced case because in both cases
3000 calcite precipitation takes place out of an aqueous solution
1 M treatment (Whiffin et al., 2007)
that permeates into the soil matrix, and no hydration takes
Unconfined compressive
2500 025 M treatment place inside the samples, unlike gypsum and Portland
strength, UCS: kPa
1500
Implication for engineering applications
1000
The findings from this study show that different micro-
500 scale precipitation distributions from different chemical
treatments result in different macro-scale permeability and
0 strength values, which potentially has implications for how
0 20 40 60 80 100 120 140
MICP could be applied in engineering practice. Larger
Calcium carbonate precipitation: kg/m3
concentrations resulted in the precipitation of relatively
Fig. 10. Unconfined compressive strength plotted against calcium larger calcium carbonate crystals along with inhomogeneous
carbonate precipitation for MICP in the present study (0.25 M) precipitation patterns, which led to a faster decrease of
compared to Whiffin et al. (2007) (1 M) permeability with precipitation, and overall weaker UCS
338 AL QABANY AND SOGA
values compared with samples treated using lower urea MICP treatment. A solution with low chemical concentration
calcium chloride concentrations. may produce a more uniform precipitation pattern and
Different permeability reduction patterns that can be stronger samples for a given amount of calcite precipitation.
obtained by varying the concentration of the chemical solu- However, this means that more volume of fluid injection is
tion can be useful when determining whether the reduction required compared to the case of using a solution with
in permeability needs to be distributed over a large area or higher chemical concentration, which in turn may increase
possibly only at specific localised locations. With the use of operation costs. Further work is needed to find an optimal
a low-concentration solution, more consistency in permeabil- condition that not only gives targeted engineering properties
ity reduction is ensured and the possibility of flow channel for soil improvement but also requires less operational
development is potentially smaller. Furthermore, it would complexity in the field.
result in a uniform precipitation distribution, whereas a
high-concentration solution may be used when a relatively
rapid reduction in permeability is needed and a complete
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