JOURNAL OF NUCLEAR RESEARCH AND DEVELOPMENT, NO.

8, DECEMBER 2014

ESTIMATION OF THE FLOW AND TRANSPORT PARAMETERS FOR COLUMN

EXPERIMENTS IN LIMESTONE

ALICE IONESCU

Institute for Nuclear Research Pitesti, Romania

e-mail: alice.ionescu@nuclear.ro

Abstract
The paper presents the derivation of the flow and transport parameters for Tritium and 14C,
from the breakthrough curves of flow-through experiments in two limestone columns of
different particle sizes. The limestone rock, bored from Dobrogea region in Romania, was
investigated at Los Alamos National Laboratories (LANL), as part of collaboration agreement
with the Institute for Nuclear Research Pitesti. Flow parameters obtained from the inverse
modelling of 3H transport with HYDRUS-1D code were further used to estimate transport
parameters for 14C. Transport of 14C is modelled by physical non-equilibrium with equilibrium
non-linear sorption in the immobile region, kinetic sorption in the mobile liquid region and
irreversible sorption, and attachment-detachment model with irreversible sorption. For a better
understanding of the sorption mechanisms, additional information is needed, concerning rock
mineralogical composition, water chemistry, determination of resident concentrations and a
better documentation of the experimental works.

Keywords: 14C, 3H, limestone, column experiment, mobile-immobile, kinetic sorption, inverse
modelling, HYDRUS

Introduction
Demonstration of the safety of disposal of the radioactive
waste is a priority task, in order to ensure safe use of the
nuclear power and public acceptance. The assessment of
the safety of the disposal facilities deep underground
requires estimation of the values of various flow and
transport parameters, for different geological and
geochemical environments, through laboratory and field
experiments. Sorption of contaminants to soil is an
important path for removal of the contaminants from the
groundwater, reducing the risk to the population and biota.
Laboratory flow-through (column) experiments allow
observation of contaminant migration in the presence of
hydrodynamic effects and chemical phenomena, even
under non-equilibrium conditions [1].
14
C is a waste product of the nuclear power industry that is
particularly important because of its high environmental
mobility and bio-availability. Geologically, inorganic 14C
is very mobile, with the exception of calcite-containing
rocks that provide a clear solid-phase sink [5]. The extent
to which 14C in solution may react with the solid phase is
not well known. Sorption of 14C was investigated by
various techniques: column studies, diffusion cells and
batch experiments. 14C could be redistributed between
solid and liquid phases by the isotopic exchange and the
recrystallization mechanisms [4, 5]. Sorption varied
largely among the solids used in these experiments, but
one key finding is that sorption reactions are very slow.
Reaction of the 14C in solution with calcite (one of the
most important mineral fractions in limestone) seems to be
a surface reaction, and it was found that aging of the
mineral grains is affecting greatly the dominant
mechanism for removal of the 14C from solution and the
solid surface available for isotopic exchange.
Nevertheless, the influence of mineral solid surface on 14C
isotopic exchange was reported mainly for synthetic
calcite, and is less important for natural calcite [5]. Under
alkaline conditions, carbonates will precipitate, and will
incorporate exchanged 14C, as it was detected in the
precipitated calcite at the inlet of the columns. Precipitated
14
C will be available for later re-exchange with pore-water,
as the source term for 14C will decrease. The reverse
reactions may be much slower [5]. Another possible sink
for 14C is through variation of the solution pH that might
remove 14C from solution. Investigation of 14C sorption
through laboratory experiments should be done on aged
solids and, before starting the experiment, reaching of
equilibrium between water and solid should be carefully
checked [4].
The objective of this paper is to determine the flow and
transport parameters for 3H and 14C from the experimental
results obtained from flow-through experiments in two
limestone columns subjected to two different flow
regimes. The old rock samples were extracted from an
existing well in the vicinity of Saligny (Dobrogea region),
from the depth of 71 m. In 2005, the samples were sent to
the Los Alamos National Laboratories (LANL) for
preparation and running of the column experiments, as
part of the cooperation with the Institute for Nuclear
Research Pitesti. The experiments were modelled with the
HYDRUS-1D code, and parameters were determined by
inverse modelling from the experimental breakthrough
curves (BTC) [2].

18
A. IONESCU: ESTIMATION OF FLOW AND TRANSPORT PARAMETERS FOR COLUMN EXPERIMENTS IN LIMESTONE

Materials and method release of 14C from Column 3 shows a second higher
Description of the column experiments (setup and maximum at about 3.87 PV. The second maximum is not
breakthrough curves) visible for Column 2, which shows instead a wider
Details of the column experiments were presented in flattened release curve. In Run 2, the BTCs of 14C are
another paper [3], therefore only a brief description is bi-modal, with a first lower peak, almost merged with the
depicted here. After crushing and sieving, limestone was second higher peak. The bi-modal BTC is more visible for
packed in two columns of different particle size ranges: the finer grained Column 2, whilst for Column 3 the two
75 – 500 μm, respectively 500 – 2000 μm. The columns peaks are almost fuzed. For both columns, 14C release
were saturated with synthetic water having an ionic show extended tailings.
strength of 26.5 mM/l and a pH of 8.7. Initially, a pulse of
contaminants of approximately 0.4 PV was injected at the
bottom of the columns, at a fast flow rate for a given
period of time, followed by several pore volumes of water
at the same flow rate. Another pulse was injected
afterwards, at a much lower flow rate, and after the source
was exhausted, the columns were flushed with synthetic
water. The eluted fluid was collected at the top of the
columns, and the concentrations were measured by liquid
scintillation spectrometry.

Table 1 summarizes the physical dimensions and

hydrological properties of the cores. Total porosity was
estimated through weighting of the dry and wet cores.

Table 1 Physical and hydrological properties of the

limestone cores, [3]
Parameter Column 2 Column 3
Length, L [cm] 46.16
Grain size [μm] 75 - 500 500 - 2000
Area [cm2] 6.13 6.24
Bulk density, ρb [g/cm3] 1.414 1.285
Porosity, θ [-] 0.53 0.55
Run 1 Run 2 Run 1 Run 2
Average flow rate, Q [ml/h] 2.87 0.716 2.863 0.733
Pulse duration, T0 [h] 20.38 81.36 19.91 79.41

Fig. 1 displays the resulting breakthrough curves from

column 2 (a) and column 3 (b). The BTCs of H-3 show a
very small first maximum of the relative concentration of
about 2.4·10-5, immediately after the onset of the injection
(visible on logarithmic scale), at 0.08 PV for Column 2,
respectively at 0.6 PV for Column 3.
The onset of the first release took place before the first
sampling. At higher flow rates in Run 1, the second (and
much higher) peak of the non-sorbing tracer 3H arrives a
little bit faster from the fine-grained column 2, after about
1.14 PV. At lower flow rates (Run 2) the peak of 3H arrive
at the column end faster from Column 3 (at 1.12 PV),
compared to Column 2 (at 1.15 PV).
The time of the peak from Column 3 is at 1.18 PV. For
both columns, 3H BTCs shows extended low-amplitude
tailings. The tailing is only visible on a log scale, and
suggests manifestation of some degree of physical non-
equilibrium.
The peak of 14C arrives faster from the coarser-grained
Column 3, irrespective of the flow rates, showing higher
maximum relative concentrations. For higher flow rates
(Run 1), the 14C time of peak in Column 3 is at 3.3 PV,
while the time of peak for Colum 2 is at 4.1 PV. The
19
Fig. 1 Breakthrough curves of 3H and 14C
from Column 2 (a), respectively Column 3 (b).
Treatment of experimental results
Physical non-equilibrium solute transport is accounted for
by assuming a two-region, dual-porosity type formulation
that partitions the liquid phase (i.e., the total water content
θ) into mobile (flowing, inter-aggregate), θmo, and
immobile (stagnant, intra-aggregate), θim, regions with θ =
θmo+θim. Water flow is assumed to be uniform and the
immobile water content to be constant with time, therefore
the mobile-immobile water concept (physical non-
equilibrium) is applied only to solute transport. Chemical
non-equilibrium model assumes that the sorption sites S
can be divided into two fractions: sorption on one fraction
of the sorption sites is assumed to be instantaneous (S1),
while kinetic sorption S2, usually modelled as a first-order
rate process, occurs on the second fraction (Two-Site
Model).
 JOURNAL OF NUCLEAR RESEARCH AND DEVELOPMENT, NO. 8, DECEMBER 2014

When both sorption sites are kinetic, these reactions can
proceed at different rates (the Two Kinetic Sites Model).
Additionally, irreversible sorption S3 may constitute a first
order sink in the liquid phase. Mass balance for the total
sorbed concentrations and for each sorption site is
expressed through:
S = S1 + S2 + S3
S1 = f M K f C m
Dm is the dispersion coefficient in the mobile zone, qm is
the volumetric fluid flux density in the mobile region, φm
and φim are sink–source terms that account for various
zero- and first-order or other reactions in both regions; f is
the fraction of sorption sites in contact with the mobile
water content, α is the mass transfer coefficient, and Γs is
the mass transfer term for solutes between the mobile and
(1)
immobile regions [2].
(2)

dS 2 Results
= α 2 ( (1 − f M ) K f C β − S 2 ) (3) Determination of the flow parameters
dt Tritium transport was modeled first with a local
∂S3 θ equilibrium model (LEA), assuming that all the porosity is
= β 3C (4)
∂t ρ available for flow. Dispersivity αL was optimized first.
The r2 value for regression of the observed versus fitted
where fM is the fraction of exchange sites assumed to be in values was 84.3% (results not shown), and the resulting
equilibrium with the solution phase; α2 is the first-order BTC could not match the maximum of the released
rate constant; Kf is the (Freundlich) adsorption isotherm concentration. When total porosity was introduced in the
coefficient; β is the (Freundlich) exponent and ρ is the optimization process for Column 2, r2 increased to 99.34%
bulk density. If both sites are kinetic (attachment- and the modeled BTC matched the experimental data, with
detachment concept), the reversible attachment- the exception of the tail which was not reproduced.
detachment processes are described through:
∂Si θ Physical non-equilibrium (MIM) was considered next,
= β i C − γ i Si , i = 1, 2... (5) considering that only a part of the total porosity is
∂t ρ available for flow. The optimized parameters were
where βi and γi are the attachment and, respectively, immobile porosity θim, dispersivity αL, and the mass
detachment rates corresponding to the sorption positions 1 transfer rate α. The r2 value increased to 99.7%, and the
and 2. If immobile porosity is considered, this part will be tail was reproduced reasonably well. Direct simulation of
inaccessible to flow and exchange processes. the BTC from Column 3, using the optimized parameter
values obtained for Column 2 showed a very good
Solute transport in the mobile zone takes place by agreement with the experimental data, with r2 of 98.5%.
advection-dispersion, whilst a diffusion-type transfer Further parameter optimization resulted in increasing of
between the mobile and immobile zone controls the the r2 value to 99.4%. The MIM model gave higher
amount of solute. Mass transport is described by the immobile porosity and dispersivity values in finer-grained
following equations: soil in Column 2, in agreement with the longer effective
transport paths due to increased tortuosity. In both cases,
∂ (θ m Cm ) ∂ ( Sm ) the shoulder appearing in the experimental data at later
+ fρ =
∂t ∂t times was not obtained. The values of the optimized
(6) parameters are shown in Table 2.
∂ ⎛ ∂C ⎞ ∂
= ⎜ θ m Dm m ⎟ − ( qm Cm ) − Φ mo − Γ S
∂x ⎝ ∂x ⎠ ∂x The MIM model was checked for Column 2 by performing
additional calculations for each part of the experiment.
∂ (θim Cim ) ∂ ( Sim ) The resulting BTCs showed better agreement with the
+ (1 − f ) ρ = − Φ im + Γ S , experiment, the r2 increased to 99.99% for Run 1,
∂t ∂t (7)
respectively to 99.85% for Run 2. While for the immobile
Γ S = α ( Cm − Cim )
porosity and dispersivity the fitted values were similar to
where Cm and Cim are the concentrations in the mobile and those obtained in the optimization of the entire
immobile zones, Sm and Sim represent the adsorbed experiment, the mass transfer coefficients were
concentrations in the mobile and immobile zones, significantly different.

Table 2 Summary of the optimization results for Tritium

Parameter / Mean Absolute Akaike information

Model
θ θι μ αΛ α r2 Error (MAE) criterion (AIC)
LEA (C 2) 0.47257 - 0.29495 - 0.9934 0.00158 -3514
±σ 0.523E-3 - 0.762E-2 -
MIM (C 2) - 0.05441 0.27789 4.55E-5 0.9969 0.00112 -3658
±σ - 3.59E-4 5.93E-03 1.03E-5
MIM (C 3) 0.041229 0.14803 4.366E-5 0.9939 0.00139 -3545
±σ - 4.459E-4 5.135E-3 1.561E-5
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A. IONESCU: ESTIMATION OF FLOW AND TRANSPORT PARAMETERS FOR COLUMN EXPERIMENTS IN LIMESTONE

Mass transfer coefficient decreased with decreasing of the
flow rate from 0.2⋅10-3 h-1 to 0.6⋅10-4 h-1, suggesting that it
is a lumped parameter, describing other processes, which
are influenced by the flow regime. In any of the
simulations the shoulder was not reproduced. This
behavior might indicate that in the assumed immobile pore
domain water actually flows, but at a much lower rate
compared to the mobile zone. Longitudinal dispersivity
and mass transfer rate coefficient decreased with particle
size increasing and decreasing of the pore water velocity,
in agreement with existing observations [6, 7].
The comparison between the experimental BTCs and the
modeled release curves for is shown in Fig 2.

Fig.2 Tritium optimized relative concentration vs. time for local equilibrium (LEA) and MIM models in
Column 2 (a), respectively Column 3 (b)

The optimized immobile porosity θim, dispersivity αL, and
the mass transfer rate α are fixed in the following
optimization of the mass transfer of 14C.
Determination of the transport parameters for 14C4
For the modelling of the transport of 14C the following
concepts were tested:
• MIM-Freu-Irrev: Physical non-equilibrium with two-
site sorption and irreversible sorption. Instantaneous and
kinetic sorption occurs in the mobile domain, while in the
immobile zone it is assumed that sorption is instantaneous.
In the mobile zone some irreversible sorption may occur,
to account for removal of 14C exchanged with precipitated
calcite that might occur given the water high pH;
• 3S3R-att: Irreversible sorption and one-site kinetic
sorption, considering attachment to and detachment from
the sorption site with or without physical non-equilibrium.
• 3S5R-att: Irreversible sorption and two-site kinetic
sorption, considering attachment to and detachment from
the sorption site with or without physical non-equilibrium.
The first kinetic site might represent sorption in the high
flow rate, while the second kinetic site describes sorption
in the low flow rate part of the experiment.
The parameter values resulting from the optimizations are
given in Table 3, and the optimized BTCs in Figs 3 and 4.

Fig. 3 Experimental and optimized relative concentration vs. time for physical non-equilibrium two-site models
in Column 2 (a), respectively Column 3 (b); Mass transfer rate was not fitted in MIM-Freu-Irrev-0

21
 JOURNAL OF NUCLEAR RESEARCH AND DEVELOPMENT, NO. 8, DECEMBER 2014

Table 3 Summary of the optimization results for 14C in Columns 2 and 3

Column 2 f Kf β fM α2 α β3 r2
MIM-Freu-Irrev-0 0.27367 0.54243 1.2504 1.55E-4 0.028 0.46E-4 8.10E-4 0.7362
±σ 2.7E-17 2.7E-17 1.3E-2 1.08E-1 5.7E-3 (fixed) 1.25E-4
MIM-Freu-Irrev-1 7.34E-1 4.76 8.8E-1 9.01E-6 9.2E-2 1.9E-3 5.01E-4 0.9756
±σ 1.96E-2 1.84E-1 4.2E-3 3.78E-3 7.5E-3 1.3E-4 4.59E-5
Kinetic models Smax,2 β2 γ2 Smax,1 β1 γ1 βs r2
MIM-3S3R-att 1.9E-1 4.7E-2 8.77E-4 0.8779
±σ 1.2E-2 3.2E-3 2.57E-5
3S3R-att 1.6E-1 4.6E-2 9.01E-4 0.8777
±σ 1.0E-2 3.1E-3 2.66E-5
MIM-3S3R-att-B 4.9E+4 2.53E-1 4.3E-2 3.17E-3 0.9349
±σ fixed 1.64E-2 2.6E-3 1.60E-4
3S3R-att-B 4.4E+4 2.16E-1 4.3E-2 7.50E-4 0.9357
±σ fixed 1.30E-2 2.5E-3 1.94E-5
3S5R-att 3.95E-3 2.0E-3 3.0E-1 9.8E-2 4.8E-4 0.9415
±σ 1.78E-4 2.9E-4 2.6E-2 8.8E-3 4.2E-5
MIM-3S5R-att-B 1.8E+4 3.94E-2 4.7E-4 3.7E+4 4.45E-1 1.1E-1 2.02E-3 0.9879
±σ fixed 2.24E-3 1.3E-4 fixed 3.39E-2 1.0E-2 2.73E-4
3S5R-att-B 4.89E+3 1.59E-2 7.8E-4 4. 9E+4 4.11E-1 1.1E-1 1.68E-4 0.9858
±σ fixed 9.17E-4 1.4E-4 fixed 3.75E-2 9.7E-3 4.56E-5
Column 3 f Kf β fM α2 α β3 r2
MIM-Freu-Irrev-0 6.47E-1 5.31 8.8E-1 4.02E-2 7.57E-2 4.4E-5 8.6E-4 0.9578
±σ 1.2E-17 1.15E-17 4.3E-3 1.78E-1 1.49E-2 fixed 2.04E-5
MIM-Freu-Irrev-1 7.25E-1 4.02 8.9E-1 9.77E-4 1.33E-1 1.6E-3 4.6E-4 0.9867
±σ 1.32E-2 9.30E-2 1.7E-3 1.32E-1 1.96E-2 6.9E-5 3.7E-5
Kinetic models Smax,2 β2 γ2 Smax,1 β1 γ1 βs r2
MIM-3S5R-att 4.11E-3 3.3E-3 4.26E-1 1.7E-1 5.2E-4 0.9625
±σ 1.45E-4 2.6E-4 3.39E-2 1.4E-2 2.8E-5
3S5R-att 3.81E-3 3.3E-3 3.71E-1 1.67E-1 5.32E-4 0.9622
±σ 1.36E-4 2.6E-4 2.88E-2 1.33E-2 2.93E-5
MIM-3S5R-att-B 3.1E+4 2.96E-2 2.5E-4 5.6E+4 6.13E-1 2.2E-1 1.96E-3 0.9876
±σ fixed 1.55E-3 5.2E-5 fixed 3.04E-2 1.3E-2 1.92E-1
3S5R-att-B 4.5E+3 1.16E-2 4.8E-3 7.6E+4 6.18E-1 2.5E-1 4.64E-4 0.9843
±σ fixed 9.95E-4 3.2E-4 fixed 6.21E-2 2.7E-2 2.16E-5

Non-equilibrium two-site sorption model using the mass
transfer rate α obtained from the optimization of Tritium
gave a poor prediction of the observed breakthrough curve
of C-14 in Column 2, with overestimated tailing and lower
peak concentrations in the fast flow part, respectively
underestimated tailing in the low flow part (cf. Fig. 3).
Better outcome was obtained when α was introduced in
the optimization, and again the mass transfer rate
coefficient was lower in Column 3, in agreement with the
lower pore water velocities in this experiment (Fig. 3b).
The tailing in Run 2 was matched, but the maximum of the
concentration in Run 1in the optimized curve was higher
and delayed, compared to the experimental data. The
values of the optimized distribution coefficients Kf are in
agreement with the reported evidence [4, 6]. Mass transfer
rate for 14C is significantly higher, compared to Tritium,
indicating slower transport rates due to sorption.
Mass transfer rates α and first-order kinetic coefficient α2
are higher in Column 2, thus showing a decrease with
decreasing of the pore water velocities. Also, fraction of
sites at equilibrium fM decreased with increasing of the
particle sizes. Overall, MIM model failed in describing the
tailing parts of the BTCs.
For the physical non-equilibrium two-site models, index 0
stands for not fitted mass transfer rate coefficient, and
index 1 for fitted mass transfer rate coefficient. For the
two kinetic sites models, index MIM means that physical
non-equilibrium was considered (θim ≠ 0), while the
models without this index, all the porosity is assumed to
be available for kinetic sorption reactions. Supplementary,
models coded with index B consider Langmuirian
blocking to simulate reductions in the attachment
coefficient due to filling of favourable sorption sites.

22
A. IONESCU: ESTIMATION OF FLOW AND TRANSPORT PARAMETERS FOR COLUMN EXPERIMENTS IN LIMESTONE
One-site kinetic sorption models failed to reproduce the
tailings in both columns. Two-site kinetic sorption models
were able to reproduce the BTC in the low flow part of the
Fig. 4 Experimental and optimized relative concentration of C-14 for two-site kinetic models
in Column 2 (a), respectively Column 3 (b)
Consideration of blocking mechanism led to an
improvement in matching of the peak in the fast flow
regime (Run 1) and of the breakthrough time, but
overestimated the tailing in the low flow regime.
Further consideration of the physical non-equilibrium
results in earlier arrival of the first peak, reducing of the
maximum concentration in both flow regimes and
underestimation of the tailing in the low flow part (Run 2).
Interaction with the second kinetic site is characterized by
relatively fast attachment and slow detachment, while
Conclusions
The paper presents the derivation by inverse modelling
with HYDRUS code of the flow and transport parameters
of Tritium and 14C from flow-through experiments in
packed limestone columns, involving different grain sizes
and flow regimes.
Application of physical non-equilibrium model for 3H
transport resulted in a very good reproduction of the
experimental breakthrough curves. This approach could
not explain the very early breakthrough, although of very
limited amplitude.
Dual permeability concept with MIM would probably be
more successful in modelling of this feature, provided the
time of breakthrough could be estimated. For that,
sampling should have been done more often around the
injection times. The fitted dispersivity and mass transfer
coefficients behaviour were in agreement with existing
observations.
Determination of the transport parameters for 14C was
done with two types of models: physical non-equilibrium
(MIM) with two-site sorption in the mobile zone,
respectively two kinetic sites for sorption.
23
experiment, but overestimated the peak in the fast flow
range, resulting in earlier arrival and broader curve (as can
be seen in Fig.4).
interaction with the first kinetic site is characterized by
fast attachment and detachment rates. In each column,
attachment and detachment rates decrease with increasing
of the residence time from Run 1 to Run 2.
At the low flow rates in Run 2, where the pore water
velocities in both columns are almost similar, the
attachment is higher in the finer soil of Column 2, due to
the higher percentage of fines and longer residence times.
At higher flow rates in Run 1, the attachment decreases
with particle size increasing, possibly due to decreasing of
the contact time and of surface available for exchange.
For the MIM model, better agreement was obtained when
mass transfer coefficient was introduced in the
optimization process. The values of the optimized
distribution coefficients Kf are in agreement with the
reported evidence.
The most complex models used, namely two-site kinetic
models, reproduced better the experimental breakthrough
curves, especially when blocking was considered. None of
the approaches considered in this work could describe
what appear to be bi-modal BTCs or the very small early
breakthrough.
Confirmation of results of the optimizations and of the
hypothesis involved in the modelling (i.e., calcite
precipitation, variations of the solution pH), and suitability
of the dual permeability approach requires more accurate
information, that could be obtained through detailed record
keeping, finer sampling intervals around the onset of the
injection, monitoring of the water chemistry while the
experiment unrolls and subsequent measurements of the
resident concentrations and mineralogical analysis and
investigation of the rock to confirm precipitation.
 JOURNAL OF NUCLEAR RESEARCH AND DEVELOPMENT, NO. 8, DECEMBER 2014
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