geologija. 2008. Vol. 50. Supplement. P.

69–75
DOI:
© lietuvos mokslų akademija, 2008
© lietuvos mokslų akademijos leidykla, 2008
© Vilniaus universitetas, 2008

Effects of petroleum pollution on clay soil microstructure

Dorota Izdebska-Mucha, Izdebska-Mucha D., Trzciński J. Effects of petroleum pollution on clay soil microstructure. Geologija.
Vilnius. 2008. Vol. 50. No. 3(63). Supplement. P. 69–75. ISSN 1392-110X
Jerzy Trzciński In the paper, microstructural changes of clay soil – glacial till – caused by in-situ pollution with
diesel oil are presented. STIMAN software was used for a quantitative analysis of scanning electron
microscope-based photographs. As a result of pollution, the microstructure underwent substantial
qualitative changes: the packing of particles and clayey microaggregates decreased and part of the
microaggregates disintegrated, edges and corners of some clay particles were warped and the amount
of intermicroaggregate pores and edge-to-face (EF) contacts among clay microaggregates increased.
Diesel oil pollution entailed significant quantitative changes in the till pore space. The amount of mes-
opores, the maximum and average pore area, the maximum, minimum and average pore perimeter and
the maximum and average pore diameter grew markedly while the value of the total pore perimeter
decreased. As indicated by the drop of the microstructural anisotropy index and the amount of fis-
sure pores as well as the growing average form index, the polluted clay became more isotropic. These
changes might be due to the reduction of interparticle forces upon pollution with a fluid characterized
by a dielectric constant lower than water.
Key words: glacial till, petroleum-derived pollution, microstructure, pore space

Received 03 March 2008, accepted 25 April 2008

Dorota Izdebska-Mucha, Jerzy Trzciński. Institute of Hydrogeology and Engineering Geo­

logy, Warsaw University, Żwirki i Wigury 93, 02-089 Warsaw, Poland. E-mail: [email protected],
[email protected]

INTRODUCTION situ with a petroleum-derived substance. These studies are a con-

tinuation of quantitative analyses of porosity changes in glacial
For many years, changes of soil properties resulting from pol- till artificially saturated with petroleum and diesel oil (Izdebska-
lution have been a subject of interest of both Polish and for- Mucha, 2003, 2008) as well as of microstructural studies con-
eign scientists. The saturation of soil by fluids characterized ducted over many years at the Institute of Hydrogeology and
by physico-chemical properties different from water has been Engineering Geology, Faculty of Geology, University of Warsaw
found to have a deteriorating effect on its mechanical and filtra- (e. g., Grabowska-Olszewska, 1976, 1983; Grabowska-Olszewska
tion parameters, plasticity, swelling and others (e. g., Bowders, et al., 1984; Kaczyński, Trzciński, 1997; Trzciński, 2003; Izdebska-
Daniel, 1987; Stephenson, 1989; Barański, 2000; Herzig, 2001; Mucha, Trzciński, 2007).
Korzeniowska-Rejmer, 2001; Garbulewski, Fronczyk, 2004;
Izdebska-Mucha, 2005; Korzeniowska-Rejmer, Izdebska-Mucha, METHODOLOGY
2006; Khamehchiyan et al., 2007).
With respect to changes of engineering-geological para- Soil samples were collected from the area of a fuel terminal
meters, filtration properties in particular, in cohesive soils pol- located in north-eastern Poland. Pollution with diesel oil oc-
luted with organic fluids the microstructural analysis seems to curred in August 2005 in a field with underground fuel tanks
be of particular interest and significance. Results published so (Fig. 1). In the area where a down-flow and stagnation of die-
far have been limited to data obtained from samples after filtra- sel oil took place, petroleum-derived substances migrated
tion tests or suspension studies (e. g., Fernandez, Quigley, 1985; upwards in the soil ground. Determination of hydrocarbon
Berger et al., 2002; Kaya, Fang, 2005). content in soils, carried out in September and October 2005,
Thanks to the use of special software for the scanning elec- revealed the pollution from the ground surface to the ground-
tron microscope (SEM)-based microstructural analysis, quan- water level to exceed 1.5 to 10 times the permissible concent-
titative characteristics of pore space parameters are given in ration (Table 1).
this paper along with qualitative descriptions. The data reflect Soil samples for laboratory tests were collected from two
microstructural changes noted in cohesive soils contaminated in 2 m deep exploration pits, one being located in an area not
70 Dorota Izdebska-Mucha, Jerzy Trzciński

Fig. 1. Location of sampling sites: a – map

of underground fuel tank field in the fuel
terminal area; b – photo of a part of the
area polluted with diesel oil. UP – unpol-
luted till, P – till polluted with diesel oil.
Red line shows the limits of diesel oil spill

Tab l e 1. Hydrocarbon content in polluted glacial tills affected by pollution and the other in a polluted area. Two
glacial till horizons were found to occur in the vertical section
Hydrocarbon Hydrocarbon >C12
C6–C12 content content of these artificial exposures (Fig. 2). According to the Geological
Samp­ mg/kg of dry mg/kg of dry Total Map of Poland at a scale 1 : 50 000 (Rabek, Świerszcz, 2003),
ling Soil mg/kg
weight weight these tills were formed during the upper stadial of the Vistula
depth type of dry
m measu­ permi­ measu­ permi­ weight Glaciation.
red ssible1 red ssible1 Microstructural studies presented in this paper were com-
pleted on till samples from the lower horizon B. The hydrometer
Сlayey till sedimentation test and sieving analysis revealed the till to con-
(horizon
0.3 A, see 392.79 500 32147.85 3000 32540.64 tain 1% of gravel, 53% of sand, 25% of silt and 21% of clay frac-
Fig. 2) tion on the average. The mineral composition resulting from the
XRD diffraction analysis is as follows: illite, kaolinite, smectite,
Sandy till quartz and accessory minerals (Fig. 3).
(horizon Till samples of undisturbed structure in the form of mono-
2.0 B, see 1456.6 500 3938.2 3000 5394.8
Fig. 2) liths were taken, of which approximately 1 cm3 cubes were
cut. These were subsequently freeze-dried and subjected to
1
Journal of Laws No. 165, pos. 1359. SEM-based quantitative microstructural analysis (Trzciński,
 Effects of petroleum pollution on clay soil microstructure 71

2004). The microstructure of non-polluted (NP) till and that MICROSTRUCTURAL CHARACTERISTICS OF
polluted with diesel oil (P) was analysed on images with mag- NON-POLLUTED TILL AND TILL POLLUTED
nifications ranging from 100 to 6 500 times. The SEM used in WITH DIESEL OIL
these studies was the Jeol JSM 6380LA model, and the quanti-
tative procedures were conducted in accordance with the in- Qualitative description of the microstructure. The glacial till ex-
struction for the respective STIMAN software (Sokolov et al., amined has a matrix microstructure (according to classification by
2002). The studies were accomplished at the Laboratory of Sergeyev et al., 1980; Grabowska-Olszewska et al., 1984). Taking
Scanning Electron Microscopy and Microanalysis, Institute of into account the relative packing of structural elements, the till
Hydrogeology and Engineering Geology, Faculty of Geology, non-polluted with diesel oil was classified into subtype B – medium
University of Warsaw. packed (according to classification by Trzciński, 2003). The matrix
microstructure consists of a clayey mass, the so-called matrix (thin
arrow in Fig. 4a) with individual sandy (lower arrow in Fig. 4b)
and silty (upper arrow in Fig. 4b) grains embedded in it. The clayey
matrix is aggregated and composed of microaggregates (bold right
arrow in Fig. 4c) which together with grains form clayey-silty and
clayey-sandy aggregates. The grain surface is covered with clay film.
The contacts among the microaggregates are of the face-to-face FF
(thin upper arrow in Fig. 4c), edge-to-face EF (thin lower arrow in
Fig. 4c) or edge-to-edge EE (lower thin arrow in Fig. 4d) type. There
is a lack of visible orientation of structural elements. The pore space
is composed mainly of intermicroaggregate pores (left bold arrow
in Fig. 4c), interparticle pores (bold arrow in Fig. 4d) and subor-
dinate interaggregate pores (bold arrows in Fig. 4a) according to
porosity classification by Grabowska-Olszewska et al. (1984).
Significant microstructural changes were noted between till
P and till NP, a comparison of their features being presented in
Table 2.

Quantitative description of the pore space. Substantial differen­

ces were observed in the morphometric and geometric parameters
between NP and P tills (Table 3). The porosity value remains un-
changed, but the coefficient of variation is higher for NP till and
the minimum value is higher for P till. The amount of pores is
smaller in P till and the maximum value is much higher in NP till.
An analysis of the morphometric parameters (area, peri­
meter, diameter) provided the following information. There
was no significant change of the total pore area in P till, whereas
the maximum and average pore area parameters clearly shifted
towards the higher values. The minimum pore area value remai­
Fig. 2. Exploration pit where polluted soil was sampled. A – upper till horizon, thick- ned unchanged. The total pore perimeter was lower, but the ma­
ness about 1.3 m, brown-red clayey till with few pebbles, B – lower till horizon, ana- xi­mum, minimum and average values of this parameter were
lysed brown sandy till higher for P till. Elevated maximum and average pore diameter
parameters were found for P till, but the minimum pore diameter
value was unchanged. The distribution of pore size substantially
changed. The amount of micropores decreased, while mesopores
proved more abundant in P till.
In addition, the geometric (shape, anisotropy, degree of
orientation) parameters also changed. The average form index
value grew in P till. Observations of the pore shape revealed a
smaller amount of fissure pores and an elevated share of aniso-
metric and isometric pores. The microstructural anisotropy in-
dex value decreased markedly for P till.

INTERPRETATION AND DISCUSSION OF THE

RESULTS

Fig. 3. XRD analysis of glacial till from unit B. Samples sedimentated on glass slides. The results (Table 3) revealed that, compared to NP till, the aver-
Sm – smectite, Ill – illite, Kln – kaolinite, Qtz – quartz age porosity value for P till remained unchanged. The low value
72 Dorota Izdebska-Mucha, Jerzy Trzciński

Fig. 4. Matrix microstructure of glacial till: a and c – UP – unpolluted till; magnification 200×, b and d – P – till polluted with diesel oil; magnification 3300×. Detailed descrip-
tion in the text

Tab l e 2. Comparison of microstructural features of non-polluted till (NP) and till polluted with diesel oil (P). Types of contacts: FF – face-to-face, EE – edge-to-
edge, F – edge-to-face
NP till P till
The clayey matrix is relatively strongly aggregated The clayey matrix is significantly less aggregated
Clay particles forming aggregates and microaggregates are densely Clay particles forming aggregates and microaggregates are more
packed loosely packed, and some microaggregates are disintegrated

Some clay particles on the microaggregate surface have distinctly

Clay particles and microaggregates tightly adhere to each other along warped edges and corners (Fig. 3d – thin upper arrows) forming a
their surfaces forming a smoother surface rougher surface (compare Figs. 3a and 3b)

Clayey film tightly adheres to the surface of grains, particularly Clayey envelopes do not adhere tightly to the grain surface
to the silty ones

Among clayey microaggregates predominant are contacts of Among clayey microaggregates predominant are contacts of
the FF and EE types the EE type
The amount of intermicroaggregates equals that of interparticle pores Intermicroaggregate pores are predominant (compare Figs. 3c and 3d)

of the coefficient of variability for P till and its high value for larger pores resulted in an increase of the maximum and average
NP till points to a more uniform distribution of porosity in the pore area, the maximum, minimum and average pore perimeter,
polluted soil. There was a noticeable drop of the pore amount in the maximum and average pore diameter and in a considerable
P till, coupled with a much lower maximum value of this param- drop of the total pore perimeter value in P till. The lack of chang-
eter which, in the absence of changes of the porosity, could sug- es in the minimum pore area and pore diameter indicates that
gest significant qualitative and quantitative changes in the pore pores formed in P till were not smaller than those in NP till.
space of the polluted soil. These changes found confirmation in The variability of geometric pore parameters is reflected in
the distribution of morphometric parameters. The amount of changes of their shape and orientation. The growth of the form
micropores decreased with the growth of the number of mes- index in P till results from the growing amount of pores more
opores in P till. The redistribution of pore space in favour of isometric in shape, which is confirmed by a decreasing amount
 Effects of petroleum pollution on clay soil microstructure 73

Tab l e 3. Quantitative microstructural parameters of non-polluted till and till polluted with diesel oil
Non-polluted till1 Polluted till2
Coefficient Coefficient
Min. Max. Average Standard of varia­ Min. Max. Average Standard of varia­
value deviation tion (%) value deviation tion (%)
Porosity n (%) 19.2 30.8 24.9 4.64 19 21.5 26.8 24.4 2.12 9
Number of pores N × 103 178 1503 730 456 62 265 752 420 195 46
Total pore area St × 103 (µm2) 446 2866 2102 882 42 1979 2530 2276 210 9
Maximum pore area Smax (µm2) 9356 130565 92301 48697 53 43782 375622 140862 135013 96
Minimum pore area Smin (µm2) 0.07 0.07 0.07 0.00 0 0.07 0.07 0.07 0 0
Average pore area Sav (µm2) 1.91 4.65 3.15 0.96 30 3.36 8.99 6.09 2.04 34
Total pore perimeter Pt ×10 (µm)
3
1105 7932 4027 2298 57 2240 4267 2689 884 33
Maximum pore perimeter Pmax (µm) 2320 15131 9900 4554 46 8089 27827 15032 7920 53
Minimum pore perimeter Pmin (µm) 1.23 1.41 1.37 0.08 5.52 1.32 1.58 1.41 0.12 8.68
Average pore perimeter Pav (µm) 5.28 6.53 5.73 0.53 9 5.68 8.52 6.74 1.28 19
Maximum pore diameter Dmax (µm) 109 408 326 118 36 236 692 392 179 46
Minimum pore diameter Dmin (µm) 0.30 0.30 0.30 0.0 0 0.30 0.30 0.30 0.00 0
Average pore diameter Dav (µm) 0.70 0.92 0.80 0.08 10 0.8 1.13 0.93 0.15 15.7
Micropores 0.1 < ∅ < 10 µm (%) 24.6 46.9 31.6 9.2 29 17.3 30.8 21.4 5.5 26
Mesopores 10 < ∅ < 1000 µm (%) 53.1 75.4 68.5 9.2 13 69.2 82.7 78.6 5.5 7.04
Maximum form index Kfmax (–) 0.922 0.981 0.950 0.022 2.36 0.908 0.982 0.948 0.032 3.39
Minimum form index Kfmin (–) 0 0.046 0.008 0.019 245 0 0.023 0.005 0.010 224
Average form index Kfav (–) 0.34 0.429 0.398 0.032 8.12 0.399 0.458 0.421 0.028 6.53
Isometric pores a/b < 1.5 (%) 10.8 13.2 12.2 1.0 8.4 9.5 17.4 12.4 3.1 25
Anisometric pores 1.5 < a/b < 10 (%) 84.8 88.3 85.9 1.3 1.48 80.8 88.9 86.4 3.2 3.73
Fissure-like pores a/b > 10 (%) 0.6 3.0 2.0 1.0 51 0.2 2.7 1.3 1.0 77
Anisotropy coefficient Ka (%) 0.78 20.8 11.2 7.6 68 2.2 11.7 6.0 3.7 63
1
Number of tests 6.
2
Number of tests 5.
∅ The equivalent diameter of pore.
a/b The ratio of the two most different dimensions of pore.

of fissure pores and more abundant isometric and anisometric of some of the clay particles were warped, and the size of pores
pores. The change of shape into more isometric is responsible was redistributed in favour of mesopores.
for a significant drop of the microstructural anisotropy index in Changes in the pore space of cohesive soils polluted with
P till. Because of the subsequent reorientation of particles and organic fluids have been also recognized by, e. g., Fernandez,
microaggregates the contaminated soil becomes more isotropic. Quigley (1985), Anandarajah (2003) in samples previously sub-
The pollution of the soil ground with diesel oil caused a jected to filtration studies. They have reported the formation of
substantial microstructural transformation of the glacial till in macropores and fissures responsible for the increased perme-
question, which should be related to changes in the chemis- ability of the soils examined.
try of the pore fluid. Diesel oil is a mixture of hydrocarbons,
a non-polar fluid characterized by a low dielectric constant
value ε = 2.1. According to double layer theory, a decrease of
the ε value in the pore fluid entails a reduction in the thick-
ness of this layer (Verwey, Overbeek, 1948; Mitchell, 1993).
Studies by Kaya, Fang (2000, 2005) have confirmed that the
lower the ε value, the bigger the drop of the electric potential
on the clay particle surface and of interpaticle forces, repulsion
forces in particular (Fig. 5). The data presented imply that, as a
consequence of partial exchange of water to diesel oil coupled
with the reduction of repulsion forces among the clay parti-
cles, bonds between the structural elements of the soil were Fig. 5. Schematic diagram of electric potential vs. double-layer thickness of clay par-
weakened, part of the microaggregates disintegrated, part of ticle in water and diesel oil (according to Fernandez, Quigley, 1985 – partly changed),
the clayey films were detached from the grain surface, edges ε – dielectric constant
74 Dorota Izdebska-Mucha, Jerzy Trzciński

CONCLUSIONS of Geotechnical and Geoenvironmental Engineering. 129.

163–172.
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The authors wish to thank Ms. M. Klimarczyk and Mr. P. Pilipczuk 12. Izdebska-Mucha D. 2005. Wpływ zanieczyszczeń ropo­
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26. Trzciński J. 2004. Combined SEM and computerized im­ między cząstkami ilastymi po zanieczyszczeniu gruntu cieczą o niższej
age analysis of clay soils microstructure: technique & niż woda wartości stałej dielektrycznej.
application. In: Jardine R. J., Potts D. M., Higgins K. G.
(eds.). Advances in Geotechnical Engineering. The Skempton Дорота Издебска-Муха, Ежи Трчиньски
Conference. London: Thomas Telford. 654–666.
Влияние загрязнения нефтепродуктами на
27. Uppot J. O., Stephenson R. W. 1989. Permeability of
микроструктуры связных грунтов
clays under organic permeants. Journal of Geotechnical
Engineering ASCE. 115. 115–131. Резюме
28. Verwey E. J., Overbeek J. T. G. 1948. Theory of the stability of Показаны изменения микроструктуры моренных суглинков при
lyophobic colloids. Amsterdam – New York: Elsevier. 205 p. загрязнении нефтепродуктами в условиях in situ. Исследования
проводились сканирующим электронным микроскопом. Для
Dorota izdebska-Mucha, Jerzy Trzciński ко­ли­чественного анализа микроскопических снимков исполь-
зовалась компьютерная программа STIMAN. Под воздействием
Naftos produktų teršalų poveikis rišlių
загрязнения микроструктура моренных суглинков изменилась:
gruntų mikrostruktūrai
уменьшилась плотность упаковки частиц и микроагрегатов гли-
Santrauka ны, часть микроагрегатов разрушилась, углы и ребра загнулись,
Straipsnyje pateikiami mikrostruktūriniai moreninio priemolio poky- увеличивались поры и количество контактов ребро–плоскость
čiai, atsirandantys dėl naftos produktų teršalų poveikio in situ sąlygo- (EF) между агрегатами глин. Соответственно увеличились число
mis. Tyrimai atlikti nuskaitančiu elektroniniu mikroskopu. Kiekybinei мезопор, максимальный и средний диаметр, максимальный, ми-
mikroskopinių nuotraukų analizei panaudota STIMAN kompiuterinė нимальный и средний периметр пор. Уменьшилось значение об-
programa. Veikiant teršalams moreninio priemolio mikrostruktū- щего периметра пор. Загрязненный суглинок стал более изотроп-
ra pakito: sumažėjo dalelių ir molio mikroagregatų glaustumas, dalis ным. На это указывают уменьшение коэффициента анизотропии
mik­roagregatų suiro, kampai ir briaunos užlinko, padidėjo porų tarp микроструктуры и увеличение среднего значения коэффициента
mikroagregatų dydis bei kontaktų briauna – plokštuma (EF) tarp mo- формы пор. Указанные изменения могли произойти из-за редук-
lio mikroagregatų. Dizelinio kuro teršalai sukėlė nemažus kiekybinius ции глинистых частиц под воздействием жидкости с меньшим
priemolio porų pokyčius: padidėjo mezoporų kiekis, maksimalus ir значением диэлектрической константы.