1.

Introduction

Understanding the microstructural behavior of soildistribution, connectivity and shape of

pores, and the size and arrangement of particlesis vital in determining the macroscopic soil
properties. The spatial distribution of voids and geometric arrangement of particles in a soil
mass reflects the imprints of the geologic processessedimentation, deposition and
transportation of a soil material; depositional conditionsterrestrial, marine or glacial
environment; and weathering history. As summarized in Table 1, various types of
microstructural approach have been used extensively in characterizing the macroscale
behavior of geotechnical phenomena, such as determining the properties of natural clays (e.g.
Delage 2010; Delage et al. 1982; Delage et al. 1984; Gumanste et al. 2014; Hattab et al.
2014; Hemes et al. 2013; Houben et al. 2014; Oztoprak and Pisirici 2011; Pusch 1969; Zbik
and Frost 2009; Zhang et al. 2004; Zhang et al. 2012); understanding the deformation
behavior of clayey samples under different loading conditions (e.g., Bai and Smart 1997;
Dudoignon et al. 2001; Griffiths and Joshi 1989; Hattab and Fleureau 2010; Hicher et al.
2000; Martin and Ladd 1975; Sachan 2007); interpreting the behavior of clays during
hygroscopic evolution (e.g., Beckett and Augarde 2013; Desbois et al. 2009; Lin and Cerato
2014; Lubelli et al. 2013; Rao and Revanasiddapa 2005; Wei et al. 2013); and studying the
behavior of clays upon compaction (e.g., Kuila and Prasad 2013; Romero 2013).
Despite the advancement in the novel microstructural experimental techniques, prior
to the in-depth analysis, preparing a good-quality and undisturbed soil sample is one of the
crucial steps in evaluating accurately the behavior and properties of the soil sample. Sample
disturbance is an ever-present problem in geotechnical investigation as the foregoing may
produce result that does not completely reflect the properties previously existing in the
sample of interest. In the past, tremendous efforts have been paid by researchers to minimize
the sample disturbance. For instance, Gillott (1976); Kang et al. (2003); Sides and Barden
(1971) and; Smart and Tovey (1982) studied various kinds of drying methods, e.g., freeze,
oven and critical point drying, in order to figure out the optimal solution to remove the
moisture content within a soil sample, yet at the same time maintaining the inherent integrity
of soil structure. Also, many literatures (e.g., Chiou et al. 1990; Echlin 2009 and; Gillott
1976) have suggested methods in creating an undisturbed observation plane for viewing
under the scanning electron microscope, in term of choices of equipment and environmental
condition for cutting. All these efforts aim to produce representative samples therefore the
microscopic information remains undisturbed and significant in characterizing the
engineering behavior of soils.
The aforementioned description illustrates how a soil specimen, after performing a
series of experiments, is handled for microstructural analysis. Nevertheless, some procedural
factors such as the step of removing loadings applied on the soil sample before drying have
been hitherto neglected or considered to have minimal disturbance to the sample. Ironically,
stress relief as a result of unloading may induce elastic rebound of particles and the onset of
swelling (Mitchell and Soga 2005; Budhu 2011), hence the specimen prepared for the
subsequent microstructural analysis may not reflect the actual distribution and arrangement of
fabrics at the original loading state. In addition to that, other issues such as the uniformity and

homogeneity of soil samples, and preserving soil samples with known orientation for analysis
are also critical in evaluating accurately the evolution of microstructure, yet are rarely
discussed in the literature. In fact, attention to detail should cover from the beginning of
preparing soil samples to the final stage of microstructural analysis in order to produce results
that are comparable, presentable and interpretable. Summarizing, this paper aims to provide a
framework in preparing clay samples for pore-size measurement and fabric characterizations,
which may help to standardize the future studies of the microstructure of soil.
This paper begins with a description of a tailor-made 3D-printed portable oedometer,
which is used to preserve the loading applied during quick cooling of clay samples. The
features of essential components and the assembly process of the experimental setup will be
presented. Then, as guided by Table 2, the experimental details of sample preparationpreconsolidation, one-dimensional (1D) consolidation and freeze drying of clay samples will be
delineated. The microstructural analysis, which is grouped into two categories, i.e. pore-size
measurement using the mercury intrusion porosimetry (MIP) and nitrogen adsorption
isotherm (NAI) tests; and fabric characterization using the scanning electron microscopy
(SEM) approach will be discussed. Preliminary results will be presented to show that the
result of sample prepared from the standardized framework suggested is satisfactory and
comparable.
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Reasons of selecting freeze drying

Reasons of selecting MIP for pore-size measurement?
Reasons of selecting SEM for fabric characterization?

Among all the visualizing methods, SEM is selected due to its ease in preparing sample and
ability in producing images with high resolution for direct observations of tiny clay particles.