PETROGRAPICAL PROPERTIES AND INDEX PROPERTIES OF SEDIMENTARY

ARGILLACEOUS ROCKS VIS--VIS SLAKEABILITY CHARACTERISTICS

Imam A. SADISUN1, BANDONO1, Hideki SHIMADA2, Masatomo ICHINOSE2 and Kikuo MATSUI2
1

Department of Geology, Faculty of Earth Science and Mineral Technology

Institute of Technology Bandung, Bandung 49132, Indonesia
2

Department of Earth Resources Engineering,

Graduate School of Engineering, Kyushu University, Fukuoka 812-8581, Japan

ABSTRACT
The objective of this study was to relate the petrographical properties and index properties of sedimentary
argillaceous rocks to their slakeability characteristics. Four different types of rocks that geologically could be
classified as shales, siltstones, mudstones and claystones were studied. They offered visibly marked differences in
petrographical analysis, involving mineralogy and texture/fabric, revealed when they were subjected to X-ray
diffraction (XRD) and scanning electron microscopy (SEM) analyses. Moreover, these differences in petrographical
characteristics were highly corresponding to the index properties which further presented fundamental basis for
evaluating slakeability characteristics. The evaluation obviously showed that expandable minerals, soluble minerals
and released-strain energy as well as diagenetic maturity seemed to be major factors affecting the
slake-deterioration processes. Besides, slaking characteristics of studied argillaceous rocks revealed strong
relationship to index properties, which indicated negative exponential correlation to dry density, positive linear
correlation to both absorption and adsorption, and positive power-law correlation to plasticity index. In this case,
the most important basic property of the argillaceous rocks with regard to their slaking characteristics was plasticity
index.

INTRODUCTION
The importance of sedimentary argillaceous rocks in relation to engineering activities is due to their peculiar
behaviour of when they are contacting with water or being exposed to the atmosphere, they often present a
considerable slaking within a short period of time. A great variety of problems connecting with rock slaking and
attendant structural damages have been faced throughout the globe over recent years. Accordingly, it is necessary to
heighten our awareness of such behaviors which fundamentally affect its physical nature, strength and deformability.
The intent of this paper is to exhaustively establish the petrographical properties and index properties of some
sedimentary argillaceous rocks in relation to their slakeability characteristics. As a case study, some samples were
collected and then named as Ikeshima shales (IKS), Ombilin siltstones (OM), Tanjung Enim Mudstones and
claystones (TE), and Subang Claystones.
PETROGRAPICAL PROPERTIES OF ROCKS
Due to the fact that overwhelming majority of the rocks was consisting of very small grain-sized minerals, X-ray
diffraction analysis (XRD) and scanning electron microscope (SEM) were applied to this study. The results of XRD

495

analysis of each rock sample are shown in Figure 1. The XRD patterns of bulk samples show that, in general, all
studied rock samples are dominated by quartz and clay minerals comprising kaolinite, illite, and smectite (with or
without poorly traced mineral of chlorite), which can also be identified when they were investigated using the SEM.

Figure 1. Typical XRD patterns of each sample including its mineralogical analysis: Q (quartz), P (plagioclase),
Si (siderite), R (rutile), Py (pyrite), K (kaolinite), I (illite), I/S (illite/smectite), S (smectite).
INDEX PROPERTIES OF ROCKS
A variety test of index properties were carried out for all rock samples, consisting of dry density, absorption, and
adsorption, whereas Atterberg limits were carried out in disaggregated materials. The results of index properties
analyses can be resumed as presented in Table 1.
Table 1. Summary of dry density, absorption, adsorption, and Atterberg limits analysis results.
Sample Type

d (g/cm3)

nab (%)

nad (%)

LL (%)

PL (%)

IKS Shale

2.36 - 2.58

5.08 - 14.2

2.16 - 5.87

19.63 - 26.31

8.80 - 15.13

8.05 - 15.79

OM siltstones

2.27 - 2.45

5.91 - 31.97

2.29 - 8.37

29.84 - 53.76

17.79 - 31.11

11.47 - 23.65

TE claystones

2.16 - 2.23

23.85 - 36.81

6.27 - 9.35

51.78 - 67.45

12.77 - 18.07

33.71 - 54.68

TE mudstones

2.25 - 2.37

19.72 - 27.05

6.14 - 9.16

47.81 - 55.08

21.32 - 23.23

26.49 - 31.85

SC claystones

2.03 - 2.31

21.95 - 76.84

6.92 - 19.94

59.56 - 98.31

13.34 - 26.07

43.79 - 72.85

PI

(%)

SLAKEABILITY CHARACTERISTICS OF ROCKS

A modified static slaking index test suggested by Sadisun et al. (2002; 2003) was applied in this study. All slaking
index values of each argillaceous rock type through five cycles were plotted as shown in Figure 2.

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PETROGRAPHICAL PROPERTIES VERSUS SLAKEABILITY CHARACTERISTICS

Based on the petrographical characteristics, it is possible that the slake-deterioration of studied rocks is due to
specific mineralogical/textural relationship. It has already well known that the rocks containing smectite and pyrite
minerals may disintegrate when they are exposed to the air and water, such as stated by Taylor and Spears (1970),
Hopkin and Deen (1984), and Bratti and Broch (1995).
In order to recognize the influence of smectite on slake-deterioration, a correlation analysis was carried out between
the percentages of expandable mineral and slaking indexes. From a slaking index-smectite content relationship plot
shown in Figure 3, it can be identified that the slaking indices increase with the increase of the smectite content.
This relationship could be better recognized upon subdividing studied argillaceous rocks into individual rock type
(i.e. IKS, OM, TE-Md, TE-Cl, and SC). In this case, the different trend of the relationships might be caused by the
other factors which simultaneously affecting slake-deterioration processes.
IKS
OM
TE-Md
TE-Cl
SC

100

Slaking Index (%)

80

60

40

20

0
0

3
4
Number of Cycle

Figure 2. Typical slaking indexes of each sedimentary argillaceous rock.

60

Slaking Index (%)

50
40
30
20

IKS
OM
TE-Md

10

TE-Cl
SC

0
0

10

20

30

40

50

Smectite Content (%)

Figure 3. Plot showing the distribution of slaking index values of

each studied rock in different smectite content.

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Meanwhile, when pyrite-bearing rocks are exposed or moistened, pyrite will be oxidized to ferrous sulphate (FeSO4)
and free sulfuric acid (H2SO4). If any calcium carbonate (CaCO3) is present, free sulfuric acid resulting from the
oxidation of pyrite may alter into sulfate (gypsum/CaSO4.2H2O), promoting a slow increase in volume, and hence,
in rock cracking. In this study, a further test was carried out to understand the slaking behavior of pyrite bearing rock
in distilled water and CaCO3 solution in a different concentration. TE-4 and SC-2 were selected as case study for
this test as they were relatively high content of pyrite, which were 27.25% and 13.58%, respectively (Figure 4). It
can be recognized that the slaking indexes in CaCO3 aqueous solutions are always higher than that in distilled water,
and likewise, the observed slaking indexes significantly increase as the CaCO3 concentration increased. In this case,
the increase of slaking index values of TE-4 reached 23% and 51% in the CaCO3 concentration of 5% and 10%,

100

100

80

80

Slaking Index (%)

Slaking Index (%)

while SC-4 was 12% and 19%.

60
40
Distilled Water
5% CaCO3
10% CaCO3l

20
0

60
40
Distilled Water
5% CaCO3
10% CaCO3

20
0

Number of Cycles

Number of Cycles

Figure 4. Results of modified slaking index test in distilled water and CaCO3 solutions
for: a) TE-4 (left) and b) SC-2 (right) samples.
In spite of the two specimens being equal in percentages of smectite and pyrite minerals, they occasionally exhibit a
difference in the values of slaking indexes. This may indicate that the argillaceous rock structure/fabric contained a
certain degree of strain energy (dissipation energy), which also affects the slake-deterioration processes. In this case,
the extension or release of any discontinuity planes seemed as the dominant factor controlling the slaking. It was
revealed by a closure phase of cracking or fissuring that developed when the rock was initially exposed to the
atmosphere. These processes were occasionally hard to detect by the naked eye without using at least a 10X
magnification loupe for hairline cracks that were mostly developed. The cracks would further result in increases of
permeability and exposed rock surface area in where any expandable allowed reaction with water. Moreover, the
increase of permeability by developed cracks was also a main factor triggering capillary forces. Bjerrum (1968)
noted that the sedimentary argillaceous rocks with high diagenetic maturity usually would give low potential on
stored-energy release due to the strong adhesion between particle bond and known as diagenetic bond. Taking all
these above into consideration, it is not unreasonable to understand that the inherent release energy significantly
contributed in the slaking processes.
For the comparative stages of diagenesis of studied rocks could be expressed by the disappearing of smectite layers
in the illite/smectite mixed-layered phases, it was interesting to analyze the relationship between illite/smectite ratio
and slaking index (Figure 5). This relationship shows that the Ikeshima shales that contain the highest diagenetic

498

maturity generally possessed the lowest slaking indexes. These results were in agreement with our expectation due
to the fact that the diagenetic processes will result in increase of induration and decrease on potential to release
strain energy.
Meanwhile, some Subang claystones contained soluble minerals of calcite and siderite, which mainly occurred as
very small crystals of pore-filling materials. To verify the importance of these minerals in slaking behavior, the
sample of SC-2 containing of 10.70 % calcite and 12.31 % siderite was selected again and submitted to the
slaking index test in the HCl solutions of different concentrations (Figure 6). The results are quite similar to the use
of the CaCO3 solution where slaking indexes increase with an increasing concentration of HCl solution. In this case,
in the 0.5 M and 1 M HCl solution of distilled water, the observed slaking indexes increased 12% and 20%,
respectively. This demonstrates the grave importance of calcite soluble minerals in the slaking behavior of
argillaceous rocks, particularly in the acid condition.
70
IKS
OM
TE-Md
TE-Cl
SC

60

Slaking Index (%)

50
40
30
20
10
0
0.0

1.0

2.0

3.0

4.0

5.0

Illite-Smectite Ratio

Figure 5. Relationship between illite/smectite ratio and slaking index.

Broken lines represent upper and lower trend limits.

Slaking Index (%)

100
80
60
40

Distilled Water
0.5 M HCl
1 M HCl

20
0
0

Number of Cycles

Figure 6. Results of modified slaking index test in distilled

water and HCl solutions for SC-2 sample.

499

INDEX PROPERTIES VERSUS SLAKEABILITY CHARACTERISTICS

Bivariate regression techniques were carried out to identify any index properties, or combinations of variables, that
might affect in slakeability characteristics. The results showed that lower slakeability characteristic was associated
with a higher degree of induration, as indicated by dry density and absorption values. Figure 7a shows a strong
negative exponential correlation between slaking index and dry density values of studied argillaceous rocks with
statistically regression coefficient of 0.85 at the 95% confidence level. The equation for the regression line is:
Is1 = 5E+06e-5.5d

(1)

Meanwhile, a plot of the relationship between slaking index and absorption values is shown in Figure 7b. The
regression line fits the data well indicated by a regression coefficient of 0.86, although a few of data scatters can be
identified, particularly from Subang claystones. This scatter suggests that absorption value is not sensitive to
differences in the slakeability of the Subang claystones. The equation for the regression relationship can be
expressed by:
Is1 = 0.96 nab + 4.40

(2)

A similar trend to the above correlation was identified when the adsorption values were plotted against slaking index
values, as shown in Figure 7c. The relationship derived from this correlation gives the general trend equation:
Is1 = 0.79 nad + 2.24

(3)

with statistically regression coefficient of 0.78 at the 95% confidence level. The relatively strong relationship to both
absorption and adsorption to slaking index values makes good sense for the water is the most important agent in
slake-deterioration processes.
The regression analyses indicated plasticity index as the most important basic property of studied argillaceous rocks
with respect to their slaking characteristics. Bivariate regression between plasticity index and slaking index showed
a strong correlation between two parameters, indicated by regression coefficient of 0.90 at the 95% confidence level.
Plot of the regression is shown in Figure 7d. The equation for the regression line can be expresses as:
Is1 = 5 PI1.18

(4)

CONCLUSIONS
Detailed petrographical analyses subjected to XRD and SEM showed evidence that all studied sedimentary
argillaceous rock samples were dominated by quartz and clay minerals but they showed some differences in term of
qualitative analysis of minerals as well as features of microstructures. On the basis of petrographical analyses, the
illite-smectite ratio within mixed-layered phases and the occurrence of dispersion particle structures of clay minerals
were enabling to be put in the practical use as a good indicator to differentiate relative degree of induration among

500

the studied argillaceous rocks. Meanwhile, based upon basic physical analyses, the comparative differences in dry
density and absorption of the rocks could be indicative of their related degree of induration.
80

a.

IKS
OM
TE-Md
TE-Cl
SC

IKS
OM
TE-Md
TE-Cl
SC

60
Slaking Index (%)

Slaking Index (%)

100

10

b.

40

I s1 = 0.69 n ab + 4.40

20

I s1 = 5E+06e -5.5 d

R2 = 0.86
n = 20

R = 0.85
n = 20

2.2

2.4

2.6

2.8

20

40

Dry Density (g/cm )

70
I s1 = 2.79 n ad + 2.24

IKS
OM
TE-Md
TE-Cl
SC

100

c.

R2 = 0.78
n = 20

50

Slaking Index (%)

Slaking Index (%)

60

40
30

IKS
OM
TE-Md
TE-Cl
SC

20
10

60

80

Absorption (%)

d.

10

I s1 = 0.37 PI 1.18
R2 = 0.90
n = 20

10

15

20

25

30

Adsorption (%)

10

100

Plasticity Index (%)

Figure 7. Regression of slaking index and: a) dry density, b) absorption, c) adsorption,

and d) plasticity index. Broken lines represent 95% confidence limits.
The evaluation on slaking characteristic of studied argillaceous rocks, on the basis of petrographical characteristics,
obviously showed that expandable minerals, soluble minerals, and released-strain energy as well as diagenetic
maturity seemed to be major factors affecting the slake-deterioration processes. Besides, slaking characteristics of
studied argillaceous rocks revealed strong relationship to their basic physical characteristics, which indicated
negative exponential correlation to dry density, positive linear correlation to both absorption and adsorption, and
positive power-law correlation to plasticity index. In this case, the most important basic property of studied
argillaceous rocks with regard to their slaking characteristics was plasticity index.
ACKNOWLEDGEMENTS
The authors are grateful to the Management of Matsushima Colliery of Ikeshima Coal Mine and Ombilin-Tanjung
Enim Collieries of Bukit Asam Coal Mine for providing the samples used in this study. Any opinion expressed in
this paper are those of authors themselves and not necessary those of the mines.

501

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