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Clay mineral characterization through the methylene blue test: Comparison

with other experimental techniques and applications of the method

Article  in  Canadian Geotechnical Journal · December 2004

DOI: 10.1139/t04-060

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1168

Clay mineral characterization through the

methylene blue test: comparison with other
experimental techniques and applications of the
method
Antonella Chiappone, Stefania Marello, Claudio Scavia, and Massimo Setti

Abstract: This article illustrates an experimental study of clay mineral characterization conducted with the aid of the
methylene blue “stain” test, which yields a semiquantitative evaluation of the activity of a geomaterial based on the
type and quantity of clay minerals contained in it. The properties of clay minerals are described briefly, with special
regard to their swelling behaviour in the presence of water. The testing method is described with reference to the pro-
cedures and interpretation criteria specified in the Association française de Normalization (AFNOR) and American So-
ciety for Testing and Materials (ASTM) standards. The results are then presented of a testing campaign conducted to
assess the applicability of the methylene blue test for the characterization of geomaterials through a comparison with
other testing methods. Additional tests were performed on stratigraphic sequences to identify the levels containing
higher proportions of active clay minerals, based on their tendency to swell on coming into contact with water. This
characterization technique was applied to marly–arenaceous formations of the Langhe region (Piedmont, Italy), where
planar sliding instability phenomena have often been observed following abundant rainfall, and marly–arenaceous for-
mations of Monferrato (another region in southeast Piedmont, Italy), where studies of a geological–structural nature
have often revealed traces of postsedimentary tectonic phenomena.
Key words: methylene blue stain test, marl, clay mineral, swelling phenomenon, planar sliding instability.
Résumé : Cet article illustre une étude expérimentale de la caractérisation des minéraux argileux conduite au moyen de
l’essai de coloration au bleu de méthylène qui fournit une évaluation semi-quantitative de l’activité d’un matériau géo-
logique sur la base des types et de la quantité des minéraux argileux qu’il contient. Les propriétés des minéraux argi-
leux sont décrites brièvement particulièrement en regard de leur comportement en gonflement en présence d’eau. La
méthode d’essai est décrite en se référant aux procédures et aux critères d’interprétation spécifiés dans les normes de
l’AFNOR et de l’ASTM. Ensuite, on présente les résultats d’une campagne d’essais réalisée dans le but d’évaluer
l’applicabilité de l’essai au bleu de méthylène pour la caractérisation des matériaux géologiques en les comparant avec
d’autres méthodes d’essais. Des essais additionnels ont été réalisés sur des séquences stratigraphiques pour identifier
les niveaux contenant des proportions de minéraux argileux actifs sur la base de leur tendance au gonflement lorsque
mis en contact avec l’eau. Cette technique de caractérisation a été appliquée aux formations quasiment sableuses de la
région de Langhe (Piedmont, Italie), où on a souvent observé des phénomènes de glissements le long de plans à la
suite de pluies abondantes, et aux formations marneuses sableuses de Monferrato (une autre région du sud-est du Pied-
mont), où des études orientées vers la structure géologique ont souvent révélé des traces de phénomènes tectoniques
post-glaciaires.

Mots clés : essai de coloration au bleu de méthylène, marne, minéraux argileux, phénomène de gonflement, instabilité
de glissement le long de plans.

[Traduit par la Rédaction] Chiappone et al. 1178

Introduction plies in particular to fine-grained materials, such as clay. In

geotechnics, it is vitally important to understand the interac-
The physical–mechanical properties of some geomaterials tion between water and a geomaterial; this interaction is a
are significantly affected by the presence of liquids; this ap- function of the content of the geomaterial, particularly the

Received 5 February 2002. Accepted 3 May 2004. Published on the NRC Research Press Web site at http://cgj.nrc.ca on
9 December 2004.
A. Chiappone. Geodes s.r.l., Corso Galileo Ferraris 80, 10129 Torino, Italy.
S. Marello and C. Scavia.1 Department of Structural and Geotechnical Engineering, Politecnico di Torino, Corso Duca degli
Abruzzi 24, 10129 Torino, Italy.
M. Setti. Department of Earth Science, Università degli Studi di Pavia, Via Ferrata, 1I, 27100 Pavia, Italy.
1
Corresponding author (e-mail: Claudio.scavia@polito.it).

Can. Geotech. J. 41: 1168–1178 (2004) doi: 10.1139/T04-060 © 2004 NRC Canada
Chiappone et al.
content of clay minerals, which may cause swelling. The
quantity and quality of clay minerals in soil are usually
determined through powder methods, X-ray diffractometry
(XRD), and Brunauer–Elmet–Teller (BET) analyses, which
provide information on the specific surface of the particles.
Such techniques are quite costly and time consuming, and
therefore new experimental techniques are being defined and
tested to meet the need for faster and cheaper methods for
the characterization of clay minerals. This article, concern-
ing a method based on the use of methylene blue, begins
with a brief description of the characteristics of clay miner-
als and their role with regards to swelling phenomena. The
methylene blue technique is illustrated with reference to two
applicable standards specified by the Association française
de Normalization (AFNOR) and the American Society for
Testing and Materials (ASTM) and is compared with other
experimental techniques. Laboratory tests were performed
according to these methods on geomaterials sampled from
the marly–arenaceous geological formations of the Langhe
and Monferrato areas in the southeastern Piedmont region of
Italy, where instability phenomena caused by planar sliding
are known to occur and where important evidence of post-
sedimentary tectonic deformation phenomena is present.
These tests, whose results are presented in the article, were
performed in the laboratory of the Direction Départementale
de l’Equipement – Isère – Service des Routes, Grenoble,
France, and the Laboratory of Geotechnique of the Depart-
ment of Structural and Geotechnical Engineering, Politec-
nico di Torino, Torino, Italy. XRD analyses were performed
at the Department of Earth Science, University of Pavia,
Pavia, Italy.
Properties of clay minerals
Clay minerals often represent a major component of the
sedimentary geomaterials making up the Earth’s crust. Their
origin can be traced to different processes (Velde 1995; Wil-
son 1999), such as alteration, i.e., transformation of other
(primary) materials; in situ deposition, or redeposition after
transport (“detritus”); and new formation arising from diage-
netic and (or) hydrothermal processes.
In terms of grain size, the term clay covers various miner-
als (mostly silicates) with grain size <2 µm, as well as
quartz, feldspar, carbonates, iron oxides–hydroxides, etc.
The term clay minerals defines the minerals belonging to the
phyllosilicate group (silicates with planar structure).
In the main types of sedimentary geomaterials (sand, silt,
clay, and marl), clay minerals are generally present as tiny
particles (smaller than 2 µm), and for this reason they are
identified by means of appropriate analytical tools (Wilson
1987), such as powder X-ray diffractometry (XRD) (Moore
and Reynolds 1997) or scanning (SEM) and transmission
(TEM) electronic microscopes, sometimes used in conjunc-
tion with microanalytical devices.
From the crystal–chemical viewpoint, clay minerals can
be viewed as hydrated aluminium silicates, whose crystalline
structure is based on a combination of coordinated polyhe-
drons (tetrahedrons and octahedrons) arranged along planes
(Brindley and Brown 1980; Chamley 1989). Tetrahedrons
(T) are generally coordinated by silicon atoms, with oxygen
atoms arranged at the four vertices of the tetrahedron.
1169
Octahedrons (O) are generally coordinated by aluminium
and (or) magnesium atoms, with oxygen atoms and OH
groups at the six vertices of the octahedron. Coordinating at-
oms may undergo different isomorphic substitutions: Si4+
can be replaced by Al3+ or Fe3+ in tetrahedron sites and Al3+
by Mg2+, Fe2+, and Mn2+ in octahedron sites (Brindley and
Brown 1980; Weaver and Pollard 1973). Clay minerals (e.g.,
talc and pyrophyllite, kaolinite and serpentine, mica,
smectite, vermiculite, chlorite) are classified depending on
the way the sheets (T–O, T–O–T, T–O–T–O) making up the
various structural units are stacked and based on the isomor-
phic substitutions taking place in the coordinating atoms. A
particular group of clay minerals are the mixed layers (or
interstratified clays), which are characterized by a vertical
stacking sequence of two or more types of single layers (T–
O, T–O–T, T–O–T–O). The alternation of layers can be
regular or irregular; for example, illite–smectite (I/S) is a
frequent irregular mixed layer.
The presence of isomorphous substitutions between atoms
with different valence causes alterations to the electronic
charges in the structural units, as borne out by the presence
of negatively charged “sites” along the outer surface of the
structural units, and a subordinate role is played by the posi-
tively charged sites located along the edges of the structural
units. The surface electric charges of these sites are compen-
sated for by external cations and (or) anions, which may be
attracted in a more or less stable manner and exchanged with
the electrolytes contained in the aqueous solutions circulat-
ing in the material; this mechanism is referred to as ionic ex-
change capacity, which can be either cationic of anionic.
A peculiar feature of some clay minerals (smectite, ver-
miculite) is their capability of expanding in the presence of
water and (or) organic liquids: they are commonly referred
to as expandable (swelling) clay minerals.
The variation in basal “spacing” depends on the quantity
and nature (valence and hydration potential) of the ex-
changeable cations contained in the structural spaces be-
tween layers. Smectite containing Ca or Mg in these spaces,
in fact, swells less than that containing Na; conversely, the
volume of structural space may decrease when the water
molecules and (or) organic molecules entrapped are elimi-
nated by heat and (or) pressure (e.g., loading pressure). This
phenomenon is referred to as intracrystalline swelling. An-
other swelling phenomenon, “osmotic swelling,” is associ-
ated with the so-called double-diffuse layer situated on the
outer surface of clay particles which is made up of water
molecules and electrolytes. The thickness of this layer is de-
termined by the forces of mutual attraction among the water
molecules, the electrolytes diffused in the latter, and the ac-
tive sites located on the outer surface of the clay particles
(the nature of the electrolytes plays a significant role).
The swelling phenomenon, which can be detected and
measured on the scale of the crystalline structure, is also re-
flected on a larger scale, as borne out by the landslides
caused by the presence of swelling minerals.
Water molecules can be characterized by different degrees
of mobility and density depending on their position relative
to the outer surface of the mineral particles. We can distin-
guish the following “types” of water: (i) adsorbed water cov-
ers the outer surface of clay particles in very thin layers, of
the order of 100 Å (1 Å = 0.1 nm), is kept in place by very
© 2004 NRC Canada
1170
strong electrostatic forces, and in natural conditions cannot
be removed; (ii) saturation water is situated at a greater dis-
tance from the outer surface of the clay particles and is re-
tained by polar forces and can be removed quite easily; and
(iii) interstitial water is mostly contained in pores and can
also be removed quite easily. The geotechnical (mechanical,
hydraulic) behaviour of clay materials in the presence of wa-
ter is therefore the outcome of interactions among solid clay
particles, water molecules, and dissolved electrolytes
(Güven and Pollastro 1992), in addition to any organic mol-
ecules that may be present.
The various types of clay minerals can be roughly classi-
fied as follows: (i) inert — chlorite, illite, and kaolinite with
cationic exchange capacity (CEC) of 3–25 mequiv./100 g,
specific surface area of 10–100 m2/100 g, liquid limit (LL)
of 50–120, and plasticity index (IP) of 20–60; and
(ii) active — smectite and vermiculite with CEC of 80–
150 mequiv./100 g, specific surface area of 100–
700 m2/100 g, LL of 100–700, and IP of 80–600.
With the aid of scanning electronic microscopy (SEM) it
is possible to examine the morphology of individual clay
particles and their mutual arrangement (or fabric). Different
types of fabric have been identified, including compact, scat-
tered, flocculated, oriented, etc. (Henning and Storr 1986).
Modern systems, such as environmental scanning electron
microscopy (ESEM), enable us to make dynamic observa-
tions in varying humidity and pressure conditions.
The study of clay geomaterials often entails complex and
costly analyses. Relatively simple procedures, such as the
one proposed in this study, may prove effective and expedi-
tious to obtain indications on the behaviour of clay geo-
materials.
Methylene blue stain test: the French
standard, AFNOR, and the American
standard, ASTM
In this investigation the following standards have been
considered: the French Norme Française NF P 94-068
(AFNOR 1993) and the American C837-99 (ASTM 1984).
An experimental campaign on clay materials with differ-
ent mineralogical properties and grain-size distributions was
carried out to identify those which lent themselves best to
the application of this technique and hence should be used to
fine-tune the testing method. The experimental program was
conducted according to the procedures set forth in the afore-
mentioned standards and according to a number of “spuri-
ous” procedures designed to achieve a controlled variation in
the testing parameters specified in the standards: this was
done to pinpoint the effects of such parameters on the accu-
racy of the test results and to verify the applicability of this
technique to the mineralogical properties and grain size of
the materials.
Principles of the methylene blue stain test
The methylene blue stain test makes it possible to quan-
tify the ionic absorption capacity of a soil by measuring the
quantity of methylene blue necessary to cover the total (ex-
2
From the French “à la tache.”
3
The recommended quantities are 30–60 g in very clayey to clayey soils and 60–120 g in medium to slightly clayey soils.
Can. Geotech. J. Vol. 41, 2004
ternal and internal) surface of the clay particles contained in
the soil. This testing technique works on the basis of the
chemical reactions triggered by an excess in negative elec-
tric charges in the clay particles and (or) the ionic exchange
phenomena taking place between the easily exchangeable
cations of the clay and the methylene blue cations released
by methylene blue during its decomposition in water. The
particles having the largest specific surface and the greatest
negative charge are those of clay minerals, which therefore
are the ones that can be most readily “exchanged.” Further-
more, the absorption capacity of a soil, its clay content being
the same, is a function of the type of clay mineral contained
in the soil. The absorption capacity increases as a function
of clay particle specific surface and charge.
Based on this principle, different testing techniques have
been developed using methylene blue electrolytes (e.g., tur-
bidimetric tests). The most widely used technique, thanks to
its simplicity and effectiveness, is the so-called stain test de-
fined in the French standards.2 The testing procedures de-
scribed in this paper are based on the provisions of the
aforementioned AFNOR and ASTM standards.
Both standards define an index reflecting the “activity” of
a soil. The AFNOR (1993) standards use a “blue value of
soil” index (VB), providing a semiquantitative evaluation of
the activity of a soil and qualitative indications of the type of
clay minerals contained in the soil. The ASTM (1984) stan-
dards define a similar “methylene blue index” (MIB).
The parameters that may affect ion absorption phenomena
(the quantity of clay materials contained in a geomaterial be-
ing the same) can be subdivided into two groups: (i) factors
associated with the mineralogical properties of a material
(such as the nature of the minerals present and their specific
surface); and (ii) factors associated with the environment in
which the test is performed (acid or basic environment).
Procedure and interpretation of the methylene blue test
according to the AFNOR and ASTM standards
For the methylene blue test, the AFNOR and ASTM stan-
dards require a set of devices as listed in Table 1 and shown
in Fig. 1. The testing procedures and the criteria for the in-
terpretation of test results are described in the following sec-
tions.
AFNOR
The quantity of material to be tested is determined as a
function of clay content;3 the material is pestled in a mortar
and dried in an oven at a temperature of 105 °C for 12 h.
The specimen prepared in this manner is placed in a con-
tainer with 500 mL of distilled water, dispersed in the water,
and maintained in suspension by means of a stirrer. With a
burette, unit doses (5 mL) of the methylene blue solution,
with a concentration of 10 g/L, are added to the suspension.
After adding each unit dose, a small quantity of the suspen-
sion is collected with a rod and a small drop is made to fall
onto standard filter paper; this produces a dark blue stain,
surrounded by a colourless wet area (Figs. 2, 3).
Further unit doses of the solution are then added and more
drops are deposited on the filter paper until a light blue halo
© 2004 NRC Canada
Chiappone et al. 1171

Table 1. Devices necessary for the methylene blue test.

AFNOR ASTM
Mixer, 400–700 rpm, with tongue (diameter 70–80 mm) Mixer
— pH meter
Beaker, 3000 mL, diameter 155 mm Beaker, 600 mL
Glass stirring rod, diameter 8 mm Glass stirring rod
Burette Burette, 25 mL
Filter papera Filter paper
a
White filter paper with ash content <0.01%, surface mass 95 g/m2, thickness 0.2 mm, filtration ve-
locity 75 s, and retention diameter 8 mm.

Fig. 1. Methylene blue test apparatus. Fig. 3. Example of a methylene blue stain test.

is seen to form inside the wet area and around the blue stain.
This reflects the presence of an excess quantity of methylene
blue that is no longer absorbed by the clay mineral and re-
mains in suspension. At this point, no more methylene blue
is added and the suspension is checked at 1 min intervals to
determine the stability of the light blue halo; if the halo per-
sists after 5 min, a sufficient quantity of methylene blue has
been added. Otherwise, the titration process is continued un-
Fig. 2. Methylene blue stain test (from Chiappone 1999a,
til the halo becomes stable enough.
1999b): (a) blue stain surrounded by a colourless wet area (nega-
Testing time ranges from about 15 to 60 min as a function
tive outcome of test); (b) blue stain surrounded by a light blue
of the content of the clay minerals contained in the sample.
halo (positive outcome of test).
There is a certain degree of subjectivity in deciding whether
the titration process has come to an end, making for an error
of ±1 unit dose (5 mL of methylene blue solution). The
greater the number of doses added, the smaller is the relative
error, which is given by the ratio between a single dose and
the sum of the doses added.
As mentioned previously, the index supplied by this test-
ing method is referred to as the blue value of the soil (VB,
in g/100 g) and is given by
[1] VB = V × 0.01 × 100/W
where V is the volume (in cm3) of the methylene blue solu-
tion used, 0.01 is the concentration (g/cm3) of the methylene

© 2004 NRC Canada

1172
blue solution used, and W is the dry weight (in g) of the
specimen.
Thus, the blue value represents the quantity of methylene
blue adsorbed by the clay minerals contained in the aqueous
suspension: the greater the quantity of clay minerals con-
tained in the soil, the greater the quantity of methylene blue
adsorbed. Furthermore, the blue value makes it possible to
determine the total active (internal + external) specific sur-
face (Sa, in m2/g) of the particles that can be reached by wa-
ter: having determined the blue value and the concentration
of a solution (0.01 g/cm3), and knowing that a molecule of
methylene blue has a surface area of 130 Å2 (1 Å = 0.1 nm),
the following formula can be applied:
[2] Sa = (VB/100)(N/WMB)(130 × 10–20) = 21VB
where N is Avogadro’s number (6.02 × 1023), and WMB is the
molecular weight of methylene blue. The specific surface
Sa = 21VB if the molecular weight of methylene blue is
373 g, and Sa = 24VB if the molecular weight is 320 g.
The total active surface ranges from 20 to 800 m2/g for
clay minerals and from 1 to 4 m2/g for inert minerals.
Accordingly, in addition to reflecting the percent clay
content of the sample, the blue value is also indicative of the
types of minerals present; in particular, it is affected by the
percentage of montmorillonite (a clay mineral in the
smectite group). If fine fractions consisting of different mix-
tures of clay minerals are analysed, the blue value increases
with an increase in the montmorillonite content.
For the fraction made up of elements smaller than 2 µm,
the blue value is defined as the index of activity of the clay
fraction in soil (ACB):
[3] ACB = 100VB/C2
where ACB is the index of activity (in grams of methylene
blue in a 100 g clay fraction), VB is the blue value for the
sample (in grams of methylene blue in 100 g of dry soil),
and C2 is the clay content (particles smaller than 2 µm).
As in the case of the blue value, the index of activity also
increases with an increase in the montmorillonite content, its
value being low for scarcely active or inert clay fractions.
Hence, the index of activity is an excellent indicator of the
capability of a soil (and that of its clay fraction, in particu-
lar) to retain water.
Lautrin (1989) proposed a classification of soils as a func-
tion of their index of activity (Fig. 4): a low value is be-
lieved to be representative of stable soil (nonswelling, with
high resistance to shear), and high values are thought to
indicate that the properties of the soil may change in the
presence of water.
ASTM
The applicable ASTM standard is based on the same prin-
ciples illustrated in connection with the stain testing proce-
dure specified in the AFNOR standard. The procedure is
based on the mechanism of chemical adsorption triggered by
a “deficit” in the electric charges of the particle, i.e., an ex-
cess quantity of negative charges tends to be reequilibrated
by the cations released by methylene blue upon being dis-
solved in water.
Can. Geotech. J. Vol. 41, 2004
Fig. 4. Blue activity diagram (modified from Lautrin 1989).
Classes as follows: 1, not clayey soil; 2, soil with interactive
clay fraction; 3, soil with not much active clay fraction; 4, soil
with normal clay fraction; 5, soil with active clay fraction; 6,
soil with very active clay fraction; 7, soil with noxious clay frac-
tion.
The ASTM and AFNOR testing procedures differ in terms
of the quantity of material to be analysed and the concentra-
tion of the methylene blue solution. Furthermore, the ASTM
procedure has to be performed in controlled pH conditions
(in an acid environment). The test is performed on 2 g of
material (weighed dry after oven drying at 105 °C for 12 h).
The sample is placed in a 600 cm3 beaker with 300 mL of
distilled water and kept in suspension with a stirrer. The test
must be performed in an acid environment (pH of between
2.5 and 3.8); accordingly, the pH must be measured and
corrected, as necessary, through the progressive addition of
0.1 N sulphuric acid until the pH is stabilized at the desired
value. The rest of the procedure is as described for the
AFNOR method, except that the unit dose of methylene blue
to be added during the titration process is different, i.e.,
1 mL of 0.01 N solution.
The outcome of the test is taken to be positive when the
light blue halo surrounding the blue stain persists for at least
4–5 min.
The ASTM standards define the blue index (MIB, in
mequiv./100 g) as follows:
[4] MIB = EV100/W
where E is the milliequivalents of methylene blue per milli-
litre (= 0.01), V is the volume (in mL) of the solution used in
the titration process, and W is the weight (in g) of the dry
sample.
Thus, the blue index can be determined from the follow-
ing formula:
[5] MIB = 0.5V
© 2004 NRC Canada
Chiappone et al. 1173

Table 2. Blue values (VB) and blue indices (MIB) determined from the tests.
VB (g/100 g)
MIBe (mequiv./100 g;
Sample AFNORa Type 1b Type 2c Type 3d ASTMe ASTM)
PI, clay 3.00 2.90 2.97 (pHi = 8, pHf = 3.5, 2.70 2.80 8.75 (pHi = 8, pHf = 3.5,
H2SO4 = 36 mL) H2SO4 = 36 mL)
BE, bentonite 18.90 19.50 19.50 (pHi = 8, pHf = 3.5, 17.70 15.99 50.00 (pHi = 8, pHf = 3.5,
H2SO4 = 10 mL) H2SO4 = 12 mL)
MoB16, marl 2.49 2.75 2.75 (pHi = 7, pHf = 3.5, 2.40 2.33 7.30 (pHi = 8, pHf = 3.5,
H2SO4 = 14 mL) H2SO4 = 19 mL)
C3, marl 2.78 2.85 2.35 (pHi = 7, pHf = 3.5, 2.29 2.80 8.75 (pHi = 8, pHf = 3.5,
H2SO4 = 14 mL) H2SO4 = 28 mL)
Note: H2SO4, millilitres of acid used for pH control; pHf, value corrected with acid injections; pHi, initial pH as recorded at start
of test.
a
Solution: 10 g/L concentration; suspension: material 45 g (dry weight); distilled water: 500 mL.
b
Solution: 10 g/L concentration; suspension: material 2 g (dry weight); distilled water: 300 mL.
c
Solution: 10 g/L concentration; suspension: material 2 g (dry weight); distilled water: 300 mL; pH control: sulphuric acid 0.1 N.
d
Solution: 0.01 N (3.1986 g/L concentration); suspension: material 2 g (dry weight); distilled water: 300 mL.
e
Solution: 0.01 N (3.1986 g/L concentration); suspension: material 2 g (dry weight); distilled water 300 mL; pH control: sulphuric
acid 0.1 N.

The blue index determined in this manner4 is correlated
with the blue value (VB) by means of eq. [1], keeping in
mind that in this case the concentration of the blue solution
is 3.1986 × 10–3 g/cm3 (instead of 10 × 10–3 g/cm3):
[6] VB = V × 3.1986 × 10–3 × 100/W
where 3.1986 × 10–3 is the concentration of the solution
(in g/cm3).
As pointed out previously, the basic difference between
the two procedures lies in the quantity of material to be
used; this is due to the fact that the ASTM testing procedure
is carried out on high clay content samples, i.e., on a mate-
rial that is quite homogeneous (in terms of grain size), and
even a small sample is representative of the material.
Applications and comparisons between the
two standards
A testing campaign has been conducted at the Laboratory
of Geotechnique, Politecnico di Torino (Torino, Italy), ac-
cording to the procedures specified in the two standards in
question to assess their applicability. This was done by eval-
uating the effects of the following variables on the outcome
of the tests: (i) quantity of material employed (as a function
of sample heterogeneity), (ii) concentration of the methylene
blue solution, and (iii) addition of an acid compound to the
suspension (to maintain pH between 2.5 and 3.8).
The four samples tested had different grain-size distribu-
tions and clay contents. In this way it is possible to test “ho-
mogeneous” materials (mostly clayey) and “heterogeneous”
materials (mostly marly, i.e., fine-grained clastic sediments,
which represent an intermediate stage between carbonatic
rocks and clay, with a carbonate content ranging from 35%
to 65% and a noncarbonate component accounted for, in
most cases, by a sizeable amount of clay minerals).
4
In this case, the blue index given has been obtained from tests rated as positive after 5 min of persistence of the light blue halo.
5
Bentonite refers to clay formed through in situ alterations of volcanic ashes, whether marine or continental. This clay is mostly, or totally,
made up of smectite (Bosellini et al. 1989).
The following samples were tested: (i) homogeneous ma-
terials, including clay (5% sand, 36% silt, 59% clay) from
Pisa (sample PI) and bentonite5 (5% sand, 95% clay) from
Sardinia (sample BE); and (ii) heterogeneous materials, in-
cluding marl from Monastero Bormida (sample MoB16) and
marl (5.55% sand, 61.45% silt, 33% clay) from Monforte
d’Alba (sample C3). These four samples were subjected to
the following: (i) tests according to the AFNOR standard;
(ii) tests according to the ASTM standard; (iii) type 1 tests
performed on the quantity of material provided for in the
ASTM standard (2 g) with methylene blue solution in the
concentration required by the AFNOR standard (10 g/L),
without controlling the pH value; (iv) type 2 tests performed
on the quantity of material provided for in the ASTM stan-
dard (2 g) with methylene blue solution in the concentration
required by the AFNOR standard (10 g/L), controlling the
pH value and correcting it with 0.1 N sulphuric acid; and
(v) type 3 tests performed on the quantity of material pro-
vided for in the ASTM standard (2 g) with methylene blue
solution in the concentration required by the ASTM standard
(0.01 N, corresponding to 3.1986 g/L), without controlling
the pH value.
From the foregoing it can be seen that in addition to the
two testing procedures specified in the standards, three addi-
tional spurious procedures were used, giving a total of 20
tests. Table 2 shows the results in terms of blue value (VB)
and blue index (MIB), and Table 3 shows the relative errors
associated with the different procedures.
From a comparative analysis of the results, the following
can be seen:
(1) In three cases out of four, the blue values (VB) obtained
from the tests performed according to the AFNOR test-
ing method are higher than those obtained from the tests
performed according to the ASTM procedure; in partic-
ular, the difference between the results seems to be

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1174 Can. Geotech. J. Vol. 41, 2004

Table 3. Relative errors (%) associated with the five different testing procedures.
AFNOR vs. AFNOR vs. Type 1 vs. AFNOR vs. Type 3 vs.
Sample type 1 type 2 type 2 ASTM ASTM
PI, clay 3.33 1.00 2.36 6.67 3.57
BE, bentonite 3.08 3.08 0.00 15.40 9.67
MoB16, marl 9.45 9.45 0.00 6.42 2.92
C3, marl 2.45 15.47 17.34 0.71 18.21

Table 4. Results of tests performed on samples of marly material taken from the landslide site at
San Benedetto Belbo (CN), Località Borgaletto, at and in the proximity of the sliding surface.
C2 C3.9 C5 IP Sm VB ACB
Sample location (%) (%) (%) (%) AC (%) (g/100 g) (g/100 g)
Top of sliding surface 20 31 37 20 1.00 20 1.06 8.00
Within sliding surface 24 40 46 25 1.04 32 2.07 11.03
Bottom of sliding surface 19 32 38 18 1.35 31 2.02 11.06
Note: Samples from Simeoni (1998). C2, clay content for elements smaller than 2 mm (AGI, British Stan-
dard, and MIT); C3.9, clay content for elements smaller than 3.9 mm (modified after Udden’s classification
(Wentworth 1922)); C5, clay content for elements smaller than 5 mm (according to ASTM classifications D422
and D653 and AASHTO classification T88); IP, plasticity index; AC, Skempton’s (1953) activity index; Sm,
smectite content; VB, blue value; ACB, blue activity value.

greater in clay samples, and especially in sample BE
(bentonite), which required a decidedly high quantity of
methylene blue solution for the titration process. The
higher quantity of solution adsorbed by sample BE
seems to be in good agreement with the results obtained
by Cuisset (1980), who compared the blue values sup-
plied by electrophoretic tests with those obtained from
blue stain tests and ascertained that the values supplied
by the latter were overestimated compared with the ex-
act values determined with the electrophoretic proce-
dure; this overestimate increases with increasing clay
content in the geomaterial.
(2) The comparison between the blue values obtained from
type 1 and type 2 tests (conducted without and with pH
control, respectively) revealed that the influence of the
environment (neutral – slightly basic6 or acid) in which
the tests are performed is minimal (the error is 2.36%
for sample PI, 0% for samples BE and MoB16, and
17.34% for sample C3). Similar results were obtained
by comparing the values supplied by type 3 tests and
ASTM tests (for samples PI and MoB16, in fact, the
error was limited to 3.57% and 2.92%, respectively,
whereas for sample C3 the error was 18.21%). The
quantity of material employed instead seems to affect
the test results to an appreciable extent: whereas for
samples PI and BE (homogeneous material) the error
was limited to approximately 3% (as seen by comparing
the results of types 1 and 2 with the results obtained us-
ing the AFNOR method), for samples MoB16 and C3
(heterogeneous material) the error increased appreciably
(9.45% to 15.47%). This suggests that the quantity of
material to be tested is a function of grain size.
We can draw the following conclusions: (i) the procedure
described in the ASTM standard is suitable to obtain infor-
mation on the clayey fraction only, (ii) the procedure de-
6
The measurement of pH at the beginning of the tests always yields values of between 7 (neutral environment) and 8 (slightly basic environ-
ment).
scribed in the ASTM standard is suitable for tests performed
on fine-grained homogeneous materials, and (iii) the proce-
dure described in the AFNOR standard should be used to
perform tests on heterogeneous material and to obtain infor-
mation on whole material.
Comparisons between the methylene blue
stain test and other experimental
techniques
The applicability of the methylene blue tests for the
geotechnical characterization of materials was assessed by
comparing the results obtained from methylene blue stain
tests with those obtained from other kinds of tests currently
in use.
The samples tested consisted of marly materials taken
from Oligo-Miocene formations (marl–sand layers) typical
of the Langhe region (southeast Piedmont, Italy) at sites in-
volved in the landslide phenomena triggered by the floods of
November 1994.
In view of the modest clayey content of the samples (Ta-
ble 4), the methylene blue stain tests were performed
according to the AFNOR procedure (see the section titled
Procedure and interpretation of the methylene blue test
according to the AFNOR and ASTM standards), and the
results were compared with those obtained on the same
materials using the following techniques: grain size and
hydrometer analyses, determination of Atterberg’s limits, X-
ray diffractometry, and tests for the determination of swell-
ing pressure.
Table 4 compares the results obtained from the methylene
blue stain tests with those obtained from grain size and hy-
drometer analyses, determinations of Atterberg’s limits, and
X-ray diffractometry. For the latter, Table 4 only shows the
results obtained in terms of active clay mineral content (in

© 2004 NRC Canada

Chiappone et al. 1175

this case, smectite); for the grain size and hydrometer analy- Fig. 5. Blue values versus swelling pressures for samples from
ses it shows the results for clay content. Since XRD revealed the following landslide sites: San Benedetto Belbo (CN),
the presence of smectite elements (Table 4) exceeding the Località Borgaletto; Monastero Bormida (AT), Località Cascina
2 µm threshold (commonly assumed as the limit of the silt– Armandi; and Somano (CN), Località Fontana del Boglietto.
clay transition7 for geotechnical purposes), clay contents for
elements smaller than 3.9 µm (the silt–clay transition limit
used in sedimentology8) and smaller than 5 µm9 are also
given.
The results shown in Fig. 5 reflect the correlation between
the blue values (VB) and the swelling pressures determined
on the same materials.10
From the foregoing results the following is evident:
(1) The results of methylene blue stain tests make it possi-
ble to characterize the material in an exhaustive manner
by taking into account both the quantity and type of
clay minerals present. The clay content being the same,
in fact (samples from the top and bottom of the sliding
surface, see Table 4), the blue value varies as a function
of active clay mineral content (smectite, in this particu-
lar case).
(2) Unlike the Skempton activity index (AC), the blue activ-
ity index (ACB) reflects the differences between the sam-
ples.11
(3) Based on Skempton’s classification, the soils analysed
can be rated as “normal,” since the Skempton activity
index (AC) ranges from 0.75 and 1.25. According to (approximately 800 landslides following the flood of No-
Lautrin’s (1989) classification, based on the blue activ- vember 1994), are triggered in Oligo-Miocene formations
ity index (ACB), the soils belong to the class of soils consisting of marl–sand sequences, on surfaces at a dip (of
containing an active clay fraction, since ACB is seen to between 8° and 15°) virtually coinciding with the inclination
range from 8 to 13 g/100 g. of the slopes. Sliding planes are often located inside marly
(4) In the materials tested, there is a good correlation be- layers (Forlati et al. 1998) corresponding to the sedimenta-
tween the blue value and swelling pressure. tion planes. Such planes include oxidized zones reflecting
the prolonged presence of water. Numerous studies on the
behaviour of marly materials have been initiated to gain an
Applications of the methylene blue test for understanding of these instability phenomena and how they
the identification of stratigraphic levels are triggered on gently sloping planes (Forlati et al. 1998;
containing greater proportions of active Coccolo et al. 1998). The investigations conducted so far
clay minerals have identified the marked swelling behaviour of these ma-
terials, with swelling pressures varying from 1 to 3 MPa.
Having verified the applicability of the methylene blue This behaviour is due to the presence of active clay miner-
stain test for the characterization of geomaterials, further als, and in particular to the presence of smectite contents of
tests were performed to investigate the effectiveness of the up to 50%. It has also been observed that the highest con-
test in identifying, within a stratigraphic sequence, the levels centrations of smectite are located within layers a few milli-
containing higher percentages of active clay minerals com- metres thick. To be able to readily identify such “critical
pared with the adjacent levels. levels,” the methylene blue technique was employed
In this case also, the tests were conducted according to the (Chiappone and Scavia 2000).
AFNOR procedure on materials taken from landslide sites in Figure 6 shows the variations in VB along three verticals
the Langhe region of Italy. at the site of a landslide at San Benedetto Belbo (CN),
The Langhe region is characterized by periodical landslide Località Borgaletto. The samples tested come from the land-
phenomena, mostly due, in terms of nature and spatial distri- slide scarp and two boreholes drilled at the foot of the scarp,
bution, to planar sliding instability. These phenomena, which and they include marly–silty and arenaceous–sandy materi-
have occurred following abundant rainfall (Govi et al. 1985) als. Table 5 lists the results obtained in terms of VB value on
7
According to the American Geological Institute (AGI), British Standard, and Massachusetts Institute of Technology (MIT).
8
Modified version of Udden’s classification (Wentworth 1922).
9
Silt–clay transition limit according to ASTM and American Association of State Highway and Transportation Officials (AASHTO) classifi-
cations.
10
Swelling pressures versus blue values (Fig. 4) were determined from tests (Simeoni 1998) performed on samples of marly material through
the determination of the pressure to be applied perpendicularly to the sedimentation planes to keep sample volume constant in the absence
of lateral confinement; initial sample saturation (approx. 90%) corresponded to natural in situ conditions.
11
It should be noted that the Skempton and blue activity indices refer to the fraction smaller than 2 µm, although it is often possible to ob-
serve, as in this particular case, the presence of (slightly) bigger particles of clay minerals.

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1176
Table 5. Blue values (VB) obtained from methylene blue stain tests on samples taken from
two landslide sites in the Piedmont region, Italy.
Sample location
Top of sliding surface
Within sliding surface
Bottom of sliding surface
Fig. 6. Variations in blue value (VB) along the landslide scarp
and two boreholes at San Benedetto Belbo (CN), Località
Borgaletto (lithostratigraphic scheme from Simeoni 1998).
samples taken from the interior of the same marly level at
and adjacent to the sliding surfaces of two different land-
slide sites, namely San Benedetto Belbo (CN), Località
Borgaletto (see also Table 4), and Somano (CN), Località
Pedrotti.
The results show that, in addition to large-scale litho-
stratigraphic variations (Fig. 6), the blue value also reflects
the presence of more active levels (Table 4; Fig. 6) within
the sliding surfaces (VB = 2.7–2.9 g/100 g). Such levels can-
not be distinguished through a simple visual examination,
but can be identified through other tests, such as grain size
and hydrometer analyses, XRD, and tests for the determina-
tion of the specific particle surface,12 all of which are more
expensive and more time-consuming than the methylene
blue test.
To decide whether tectonic discontinuities should be rated
as probable triggering points of landslide phenomena, addi-
12
For instance, the classical method of the Brunauer–Elmet–Teller (BET) tests.
13
The graphs reproduced in Figs. 7 and 8 refer to the analyses of tests performed after the treatment with ethylene glycol for the identification
of swelling minerals.
Can. Geotech. J. Vol. 41, 2004
VB (g/100 g)
San Benedetto Belbo, Somano,
Località Borgaletto Località Pedrotti
1.6 2.0
2.7 2.9
2.2 2.6
tional materials taken from a site displaying postsedimentary
tectonic deformations (Murisengo, Alessandria, Italy) were
subjected to the AFNOR testing procedures; the methylene
blue stain method was used to identify possible mineralogi-
cal peculiarities of the warped levels within the tectonic
zone compared with the adjacent levels. Samples were taken
from four different levels: sample 1 from the badly de-
formed marl level within the shear zone; sample 2 from a
loosely bonded sandy–arenaceous level; sample 3 from the
same marly level as sample 1 but from the upper part of the
shear zone (scarcely deformed marl level); and sample 4
from a nondeformed marl level located below the level of
sample 2.
The results of the methylene blue stain tests performed on
these samples are summarized in Table 6. Samples 1 and 3
were also subjected to grain-size analysis, hydrometer analy-
sis (Table 7), and XRD (Table 8; Fig. 7). XRD results are
shown in Table 8 and Figs. 7 and 8.13
From grain size and mineralogical analyses it can be seen
that sample grain size and mineralogical composition are
similar: sample 1 displays a smectite content (35%) slightly
higher than that of sample 3 (31%). This difference is de-
tected by the methylene blue stain test, which yielded blue
values (VB) of 3.67 and 3.22 g/100 g for samples 1 and 3,
respectively. The methylene blue stain tests also supplied
markedly higher VB values for the materials sampled from
Murisengo (Alessandria, Italy) compared with those ob-
tained on materials that were similar in every respect but had
a much higher smectite content. This result seems to contra-
dict the criteria described so far. The XRD pattern shown in
Fig. 7, however, reveals the presence of a broad smectite
peak (as also observed in sample 3): as a first approxima-
tion, this may be taken to imply a relatively low crystallo-
graphic structural order for the material in question. The
discrepancy in the results can be accounted for by assuming
a low crystallinity index for smectite: the degree of disorder
of the crystalline structure of a mineral, in fact, reflects the
presence of an imbalance in electric charges due to isomor-
phic substitutions, and the VB values obtained can be corre-
lated with this characteristic. The anomalous behaviour
observed for the level being considered might be ascribed to
postsedimentary tectonic phenomena associated with pres-
sure and temperature increases resulting in a more or less
extensive recrystallization of the minerals involved.
These findings suggest the possibility of identifying a re-
lationship between the crystallinity index of a mineral and
© 2004 NRC Canada
Chiappone et al. 1177

Table 6. Blue values (VB) determined on samples taken from four different marl levels in
Murisengo, Alessandria, Italy.
Sample No. VB (g/100 g) Zone of sampling
1 3.67 Shear zone marl level very “deformed”
2 1.00 Sandy–arenaceous level not very cementate
3 3.22 Marl level not very “deformed”
4 2.72 Marl level not “deformed”

Table 7. Grain size and hydrometer analysis on samples 1 and 3 collected from the out-
crop at Murisengo, Alessandria, Italy.
Sample No. Pebble (%) Gravel (%) Sand (%) Silt (%) Clay (%, <2 mm)
1 — — 8.0 72.5 19.5
3 — — 11.0 70.0 19.0

Table 8. Mineralogical composition (%) of samples 1 and 3 collected from the outcrop at
Murisengo, Alessandria, Italy.
Sample No. Cc Qz K-F Pl Am Ch Ka Mi Sm
1 6 7 5 4 6 16 13 8 35
3 11 9 5 5 6 13 11 9 31
Note: Cc, calcite; Qz, quartz; K-F, K-feldspar; Pl, plagioclase; Am, amphibole; Ch, chlorite; Ka,
kaolinite; Mi, mica; Sm, smectite.

Fig. 7. X-ray pattern for sample 1, collected from the outcrop at Fig. 8. X-ray pattern for sample 3, collected from the outcrop at
Murisengo, Alessandria, Italy. Murisengo, Alessandria, Italy.

VB. Accordingly, the testing program will be carried on
through a series of methylene blue stain tests on samples
characterized by the presence of smectite with known crys-
tallinity index to gain a better understanding of the efficacy
of this testing method for the identification of alterations to
the crystalline structure of clay minerals.
Conclusions
This study describes the results of an investigation of the
use of the methylene blue stain test to identify the presence
of relatively high activity clay minerals. This method makes
it possible to characterize geomaterials in terms of the quan-
tities and types of clay minerals present (and hence of their
activity) through an index that can supply semiquantitative
indications.
After a brief delineation of the properties and behaviour
of clay minerals in the presence of water, the testing method
is described together with the underlying physical–chemical
principles. The results obtained from methylene blue tests
performed according to the AFNOR and ASTM procedures
are compared, and it is pointed out that the former procedure
is more suitable for use on materials with heterogeneous
grain size or whole samples (i.e., samples tested without
having to separate the fine fraction), and the latter procedure
is more suitable when only information on the clay fraction
is needed (i.e., when dealing with fine-grained, homoge-
neous materials).
The validity of this testing technique is assessed by com-
paring the results obtained with the values supplied by other
testing methods commonly used in the characterization of
geomaterials (grain size and hydrometer analyses, determi-

© 2004 NRC Canada

1178
nation of Atterberg’s limits, X-ray diffractometry, tests for
the determination of swelling pressures). To this purpose,
methylene blue stain tests were performed on samples of
marly material taken from marly–arenaceous formations lo-
cated in the southeast Piedmont region of Italy; in view of
the heterogeneity of the materials analysed, the tests were
conducted according to the AFNOR standards. The indica-
tions provided by methylene blue stain tests were in good
agreement with the results of other characterization methods
that are used widely but are costlier and much more time-
consuming.
Having ascertained the applicability of this testing me-
thod, a series of tests was performed on marly–arenaceous
stratigraphic sequences to identify the levels displaying a
higher proportion of active clay minerals (i.e., the levels
with a higher propensity to swell in the presence of water).
The samples tested were taken from two areas of the
Piedmont region: the Langhe region, which is periodically
affected by major planar sliding phenomena triggered by
abundant rainfall; and Monferrato, where structural–geologi-
cal studies have found evidence of postsedimentary tectonic
deformation phenomena. The tests performed through the
methylene blue stain technique clearly revealed that both the
sliding planes of the Langhe region and the postsedimentary
tectonic deformation zones of Monferrato contained active
clay minerals in quantities significantly higher than those of
the adjacent levels. In particular, the test results suggest the
possibility of establishing correlations between the quantity
of methylene blue adsorbed (“blue value”) and the swelling
behaviour of materials, and between the blue value and the
crystallinity index of minerals, a function of the more or less
extensive recrystallization brought about by postsedimentary
tectonic events.
On the basis of the results obtained so far, this experimen-
tal investigation will be carried on to learn more about the
swelling behaviour of marly materials contained in slopes
that have undergone planar sliding phenomena and to ex-
plore further the possible correlation between the onset of
instability phenomena and the presence of tectonic deforma-
tion levels.
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© 2004 NRC Canada