Materials Characterization 58 (2007) 1095 – 1103

The use of the scanning electron microscope in the determination

of the mineral composition of Ballachulish slate
Joan A. Walsh ⁎
University of Paisley, Scotland, United Kingdom
Received 21 February 2007; accepted 13 April 2007

Abstract

Slate is a fine-grained, low-grade metamorphic rock derived from argillaceous sediments or occasionally volcanic ash.
Although most slates contain mainly quartz, chlorite and white mica, they vary considerably in their durability, some lasting
centuries while others fail after a few years of service. A detailed characterisation of their mineralogy is required for the assessment
of performance, and to establish the provenance of a used slate. A combination of methods was used to examine Ballachulish
slates; XRD analysis to determine the principal minerals present, XRF analysis to determine the total chemical composition, and
scanning electron microscopy to determine the chemical composition of individual minerals. It was found that the white mica in
Ballachulish slate is phengite and the chlorite is ripidolite. Feldspar is present as albite and carbonate as ferroan dolomite. Several
accessory minerals were also identified, including chloritoid, monzonite and zircon. There was considerable variation in the ratio of
the principal minerals, making it impossible to identify used slates by this criterion. Instead, chemical composition of the individual
minerals, and possibly key accessory minerals, should be used to determine the provenance of slates.
© 2007 Published by Elsevier Inc.

Keywords: Roofing slate; Provenance; BSE images; Elemental maps

1. Introduction contains a range of accessory minerals, the most important

Slate is a fine-grained low-grade metamorphic rock
derived from argillaceous sediments or occasionally
volcanic ash. The principal minerals are quartz and the
phyllosilicates, chlorite and white mica. The high
proportion of phyllosilicates, which become aligned during
metamorphism, imparts to the rock a schistosity enabling it
to be split into thin slabs. It is this property that makes it
suitable as a building material, in particular as a roofing
slate. In addition to the principal minerals, slate also
⁎ Tel./fax: +44 414 4276466.
E-mail address: ja_walsh@tiscali.co.uk.
1044-5803/$ - see front matter © 2007 Published by Elsevier Inc.
doi:10.1016/j.matchar.2007.04.013
of which are the iron oxides, iron sulphides and carbonates.
The properties of slate are largely dependent on its
mineral composition: the proportion of platy minerals
controls its splitting, quartz controls its hardness and
durability, while the presence of some minor minerals
adversely affects its durability. Therefore the chemical
composition and the relative proportions of the major
minerals present are important criteria in determining
the properties of a slate. However, due to the fine-
grained nature of the material, and the intergrowth of the
phyllosilicates, determination of mineral composition is
not straightforward. Previous researchers [1–4] have not
normally gone beyond identifying the broad proportions
1096 J.A. Walsh / Materials Characterization 58 (2007) 1095–1103

Table 1
Composition of slate according to different authors
Source Phyllosilicates Quartz
(%weight) (%weight)
Illite Chlorite
Le Corre [1] 70–87 13–30
No differentiation
Crockett [2] 38–40 6–18 31–45
Wagner et al. [3] 40 20 30
of the principal minerals contained in slate, i.e., quartz,
white mica (illite) and chlorite (Table 1). While in the
case of true argillaceous slate these make up over 95%
of the total, it is nevertheless important to identify the
chemical composition of the remaining fraction.
The above are very general characterisations which fail
to recognise the variation in the phyllosilicates. For
example illite is only one of a group of minerals referred to
in this research as white mica. They also overlook the
accessory minerals commonly found in slate, such as
feldspar, ore minerals, carbonates and graphite. Although
often present in only small amounts, some of these
minerals are easily weathered and their presence may
have a disproportionate effect on the durability of a slate.
Previous research associated with the present study [5,6]
has resulted in a general mineralogy of all slate from
Scottish sources, including Ballachulish. The present re-
search goes on to focus on Ballachulish slate, on the com-
position of the phyllosilicates present and of those minerals,
which are prone to weathering. It also seeks to identify
accessory minerals which may be used in the identification
of a used Ballachulish slate. Although a wide range of
slates, British and some foreign, have been tested, the list of
minerals which may serve as provenance indicators is not
exhaustive. However, the data are continually being revised
and extended as more slates are tested.
industry started in the 18th century and it was the main
producer until superseded by Ballachulish later in the 19th
century. Easdale slate also contains pyrite but it is paler in
colour than Ballachulish and often has a distinctive crinkly
surface, due to the presence of crenulation cleavage.
There are no pyrites in the last two groups. The High-
land Boundary Group is a series of quarries along the
Highland Boundary fault line. This slate comes in a
variety of colours, green, lilac and purple, and weathers to
a paler colour. Much of the production of these quarries
was for local consumption, but slate from Aberfoyle was
used extensively in Glasgow and surrounding areas.
Finally, the Macduff type was used extensively in the
northeast of Scotland. It is a grey slate with a slight purple
tint and characteristic “spotting” due to the presence of
porphyroblasts of biotite now retrogressed to chlorite.
After long exposure on a roof, slates are usually covered in
a thick patina of pollutants, making it difficult to
distinguish between the different types. It is hoped that
the detailed investigation of the mineralogy of the
different slates will provide information which will enable
them to be more easily and reliably identified.
2.1. Quartz
Quartz is always present in slate and is the most
durable of minerals, surviving transport prior to original

2. Mineralogy of slate from Scottish sources

There are four main types of Scottish slate; Ballachul-

ish, Easdale, Highland Boundary and Macduff. The most
famous of these is Ballachulish (Fig. 1). These slates are
dark blue grey with a rough texture and have characteristic
pyrite cubes. Peak production coincided with rapid
industrial and commercial growth in the second half of
the 19th century, and it is found on traditional buildings
throughout Scotland.
Ballachulish slate probably the type of slate most
commonly referred to as Scottish. However it was not
always so; historically slate from Easdale and its
neighbouring islands just south of Oban was synonymous
with Scottish slate. It was here that the Scottish slate Fig. 1. Location of the main slate quarries in Scotland.
 J.A. Walsh / Materials Characterization 58 (2007) 1095–1103
Table 2
Classification of white micas according to the chemical composition
after Deer et al. [7]
Mineral Cation Yoctahedral site Ztetrahedral
Muscovite K1 Al2 Si3Al
Illite K1–x Al2 Si3+xAl1–x
Phengite K1 Al2–x(MgFe)x Si3+xAl1–x
sedimentation and the increased temperature and pressure
of low-grade metamorphism. With the development of
slaty cleavage during metamorphism, detrital grains of
primary quartz become more elongated and are orientated
with their long axis parallel to the cleavage. At the same
time secondary quartz grows in a number of ways. It may
grow around pre-existing quartz grains or as clusters of
new crystals in the pressure shadows of larger grains of
any mineral. It may also grow independently in veins,
filling the fissures caused by joints and faults. These veins
can range in size from those visible to the naked eye,
which can distort cleavage on a large scale, to minor
clusters only detected at microscopic level, but which can
destroy the homogeneity necessary to produce a regular
slate surface.
2.2. White micas
White micas are dioctahedral phyllosilicates with an
inter-atomic spacing of 1 nm (10 Å) as seen in X-ray
diffraction patterns. The naming of white micas in the
literature is not consistent and the terminology used by
Deer et al. [7] is used in this research.
Sericite (fine-grained muscovite) and illite are the two
general terms used to describe white micas found in slate.
Using the terminology of Deer et al. as shown in Table 2,
the type of mica is defined according to the cation present
in the various locations. This research has found that
instead of the end member muscovite KAl2(AlSi3O10)
(OH)2, the most common type of white mica present in
Scottish slate is phengite and to a lesser extent illite. In
addition to the potassium-rich micas, the sodium-rich
equivalents are also found. These micas are described
relative to the end member paragonite NaAl2(AlSi3O10)
(OH)2, analogous to the system outlined in Table 2.
The illite group of white micas differs from
muscovite in having a higher Si4+:Al3+ ratio in the
tetrahedral sheet and hence fewer interlayer cations
holding the structure together, i.e., illites are white micas
which are deficient in potassium. The sodium equivalent
is brammallite, but this term is only rarely used.
Phengite is a member of the illite group in which
excess silica in the tetrahedral sheet is compensated by
replacement of trivalent Al by bivalent Mg and Fe in the
1097
octahedral sheet, and the sum of the interlayer cations is
approximately equal to that of muscovite.
With increasing metamorphic grade, the composition
site of the white mica changes from illite to phengite and
then to white muscovite. It is assumed that durability
increases with metamorphic grade, i.e., the closer the
composition approaches muscovite the more durable is
the white mica. This research has found that sodium-rich
white micas are more prone to weathering than their
potassium-rich equivalents.
2.3. Chlorite
Chlorite is the general term for phyllosilicates with
basal spacing of approximately 1.4 nm (14 Å). This is
the method used to identify chlorites using XRD
analysis. Chlorite is a primary mineral found in low-
grade metamorphic rocks growing at the expense of clay
in argillaceous rocks. The colour of chlorite gives
greenschists their name. The general formula is (Mg, Fe,
Al)6(Al, Si)4O10(OH)8, with considerable chemical
variation due to isomorphous substitution. Foster [8]
using these isomorphous replacements classified chlor-
ites according to: (1) the number of silicon atoms per
formula unit, and (2) the proportion of the divalent
cations which are iron. However, the system is arbitrary
and carries no generic significance. The actual compo-
sition reflects the original composition of the rock and
does not change in a systematic way with increasing
temperature and pressure [9].
It is surprising, given the potential variation, that the
types of chlorite found in the Scottish slates tested have
very similar chemical composition. Using the Foster
method of classification, the chlorite in the slates tested
has the chemical composition of ripidolite, i.e., has
fewer than 2.76 silicons per formula unit and 25% to
75% of the divalent cations are iron.
2.4. Feldspar
Feldspar as found in slate is of limited variability.
The most common form is albite NaAlSi3O8. Some
orthoclase (KAlSi3O8) is found in some slates and its
presence is used as a provenance indicator.
Table 3
Types of carbonate found in Scottish slates
Mineral Formula Solubility products [11]
Magnesite MgCO3·3H2O 2.0 × 10− 5
Calcite Ca CO3 4.5 × 10− 9
Siderite Fe CO3 3.0 × 10− 11
Dolomite CaMg(CO3)2 10− 17–10− 19
1098 J.A. Walsh / Materials Characterization 58 (2007) 1095–1103
2.5. Carbonates
The types of carbonate found in Scottish slates are
listed in Table 3. Calcite is the most frequent, but other
types are fairly common. Carbonates, although only
slightly soluble in water, are susceptible to attack by
acid and in the presence of a strong acid react rapidly
giving off carbon dioxide gas. Where the acid is
sulphurous or sulphuric acid, hydrated calcium sulphate,
i.e., gypsum, is produced.
CaCO3 þ H2 SO4 →CaSO4 þ H2 O þ CO2 ↑ ð1Þ
The European standard prEN12326 specifies that the
thickness of a roofing slate should be increased depending
on the concentration of carbonate present [10]. However,
it makes no distinction between the different types,
treating all carbonates as being equivalent. Although all
carbonates react to acid, they vary widely in their suscep-
tibility. Assuming that the solubility product (shown in
Table 3) is indicative of vulnerability to weathering, it can
be seen that the minerals range from magnesite, the most
vulnerable, to dolomite, more durable by many orders of
magnitude [11].
2.6. Iron ore minerals
The most common ore minerals found in slate are the
oxides and sulphides of iron, the type depending on the
environment of deposition of the original muds. Iron
oxide, haematite, is found in slates which were laid down
in an oxidising environment such as turbidity currents.
Haematite is the iron ore mineral found in Highland
Boundary and Macduff slate. In contrast, the iron ore
mineral found in slate such as Ballachulish, which was laid
down in a stagnant reducing environment, is a sulphide.
The type of sulphide also varies; pyrite and pyrrhotite
being the typical minerals found in Ballachulish slate.
Pyrite occurs either as large euhedral crystals or
disseminated throughout the rock. The large cubic crystals
are usually resistant to weathering, but when pyrite does
break down it weathers to a mixture of hydroxides and
oxides of iron such as limonite. Marcasite is usually
associated with pyrite and weathers more easily to
limonite. Pyrrhotite (FeS1 + x nonstoichiometric) is a less
stable iron sulphide than pyrite and is easily decomposed
by hydrochloric acid, while pyrite is not. Pyrrhotite is
found in slate in contact metamorphic deposits as
pseudomorphs of pyrite.
A considerable amount of research has concentrated
on the weathering of iron ore minerals in the presence of
calcite or aragonite. This is discussed in greater detail by
Shayan and Lancuck [12] and Kessler and Sligh [13]
among others. Pyrite/Pyrrhotite reactions in Ballachul-
ish slate are described in depth by Hall et al. [14–16].
Other ore minerals not susceptible to weathering but
used in the identification of provenance are rutile,
together with its low temperature polymorph anatase
(TiO2), and ilmenite (FeTiO3).
3. Samples of Ballachulish slate
Several samples of Ballachulish slate were collected
from the main quarry at East Laroch and from Khartoum
quarry. The former were collected from the quarry floor
and had been exposed at least since the closure of the
quarry in the 1950s. The Khartoum slates were extracted
from the quarry face in 2002.
4. Methodology
A combination of methods was used to determine the
mineralogy of Ballachulish slate. The principal minerals
were first identified using X-ray diffraction (XRD)
analysis. Then both the optical and the scanning electron
microscope (SEM) were used to identify some of the
accessory minerals not present in sufficient concentra-
tion to be identified by XRD. The total chemical
composition of the slate was determined using X-ray
fluorescence (XRF) analysis. In addition, the amounts of
carbon dioxide, sulphide and water were also deter-
mined, but little reference is made to these in this paper.
The SEM images described in this paper were acquired
using a Hitachi S 4100 cold field emission SEM, fitted
with an Oxford Instrument Gem energy-dispersive X-ray
(EDX) detector and ISIS software. Conditions used in
acquiring the BSE images and the elemental maps were
20 keV accelerating voltage, a working distance of
15 mm, and a high count rate of N15,000 counts/s. Spot
analyses were also carried out to determine the chemical
composition of some of the minerals present, using a
lower count rate of 1000–1500 counts/s in order to
maximise the resolution of the peaks.
5. Results
5.1. Hand specimen
The slate was found to be heterogeneous with very
fine-grained peletic material interspersed with siltier
layers. The cleavage surface varies from smooth with a
slight sheen when fine-grained, to rough and irregular
when coarser-grained siltier layers are present. Most
samples have a well-developed grain, defined by
 J.A. Walsh / Materials Characterization 58 (2007) 1095–1103
Fig. 2. Photomicrograph of Ballachulish slate showing the alignment
of the quartz grains. The phyllosilicates are concentrated in the
cleavage domains which anatomise gently around the quartz grains
(PPL).
alignment of acicular minerals. In many cases more than
one fabric is visible. Porphyroblasts, identified using
both the optical and the scanning electron microscope as
ferroan dolomite, are concentrated in the siltier layers.
Bedding is complex, but the overall orientation is almost
parallel to cleavage. Pyrite cuboids vary in size from
1 mm to 9 mm. In addition, clusters of pyrite crystals,
some of which have been altered to pyrrhotite, were also
observed.
5.2. XRD analysis
This showed that the samples of Ballachulish slate
have a typical argillaceous slate composition, i.e.,
quartz, white mica and chlorite, but with the addition
Fig. 3. SEM-BSE image of slate showing the intergrowth of the
different minerals; the dark grey minerals are quartz (Q) and possibly
feldspar, intermediate grey minerals (not easily identified using this
method alone) are white micas, the pale grey minerals consist of
dolomite (D) and chlorite (Cl). The brightest areas are ore minerals
such as anatase.
1099
Fig. 4. Elemental map of titanium showing the location of anatase.
of feldspar. Carbonate, initially identified as dolomite,
was found on examination using the SEM to be ferroan
dolomite. Titanium is present as anatase. Although
pyrite was easy to identify in the hand specimen, none
was identified using XRD analysis. It is assumed that
the overall pyrite concentration in the sample is less than
the detection limit of the analysis.
5.3. Thin section using an optical microscope
Examination of a thin section showed well developed
slaty cleavage interspersed by zones rich in quartz and
feldspar. Although quartz, white mica and chlorite can
be identified, due to intergrowth of the phyllosilicates it
is only possible to get a rough estimate of the pro-
portions of the individual minerals (Fig. 2). Large
porphyroblasts, visible in hand specimen, were identi-
fied as a dolomite. The mineral chloritoid, which is not
commonly found in slate, was also identified using this
method. This mineral will be used as an indicator of
provenance for used Ballachulish slates.
Fig. 5. Elemental map of calcium showing the location of dolomite.
1100 J.A. Walsh / Materials Characterization 58 (2007) 1095–1103
Fig. 6. Elemental map of potassium showing the location of white
mica.
5.4. Scanning electron microscope BSE images
Using polished sections, back scatter electron (BSE)
images show the distribution of the different minerals of
varying density, the brighter the image the denser the
mineral. Elemental maps were then used to locate
identifying elements in each mineral after which spot
analyses were carried out.
An example of one such image is shown in Fig. 3.
Minerals of the lowest density, quartz and feldspar, are
shown by the zones of the darkest shade of grey. Minerals
of intermediate density are white mica and dolomite
followed by chlorite. These are shown by progressively
brighter zones. The brightest zones indicate metallic ore
minerals of high density such as ilmenite or anatase.
However due to the similarity in the density of some of the
minerals such as dolomite and chlorite it is not possible to
distinguish between the different minerals using the BSE
image alone. This was achieved by the use of elemental
maps as described below.
Fig. 7. Elemental map of sodium showing the location of albite.
Fig. 8. Elemental map of iron; the brightest areas are chlorite.
5.5. Elemental maps
To enable the identification of individual minerals in
the BSE images, a series of elemental maps were
prepared, some of which are shown in Figs. 4–11. All
the images show the same location and were carried out
simultaneously and compared with the BSE image shown
in Fig. 3. In the case of the elemental maps, brightness of
image corresponds to higher concentration of the element.
Starting with the simplest phase, the type of mineral
associated with each of the elements shown is described
below.
Ti: The brightest location in the BSE image is iden-
tified as being due to the presence of titanium. The most
significant titanium compound present has already been
identified by the XRD analysis as anatase TiO2 (Fig. 4).
Ca: Calcium is located in anhedral minerals with a
globular habit. It can be seen from the BSE image that
these minerals have an intermediate density, greater than
that of quartz and feldspar and similar to that of chlorite
Fig. 9. Elemental map of magnesium; the brightest areas are chlorite.
 J.A. Walsh / Materials Characterization 58 (2007) 1095–1103 1101

Table 4
Total oxides present in two Ballachulish slates (determined using XRF
analysis)
Khartoum East Laroch
SiO2 69.23 57.60
TiO2 0.87 0.58
Al2O3 14.59 16.28
Fe2O3 5.85 6.42
MnO 0.04 0.09
MgO 2.19 5.26
CaO 0.10 2.07
Na2O 1.03 0.80
K2O 2.65 2.56
P2O5 0.06 0.07
SO3 0.05 0.08
Fig. 10. Elemental map of aluminium; the brightest areas are white LOI 3.20 8.27
mica. Total a 99.86 100.08
a
Totals may not precisely equal 100% due to rounding.
(Fig. 5). By comparing the elemental maps at the same
location it can be seen that the mineral containing cal-
cium also contains magnesium and iron. Spot analyses spot analyses showed that the chemical composition of
were carried out at five locations. It was found that the the white micas is that of phengite of similar composition
chemical composition was constant, e.g., the coefficient to the white mica from the East Laroch quarry previously
of variations was less than 2%. The average chemical analysed [6]. The chemical composition of the white
composition is Ca1.16Mg0.57Fe0.23Mn0.03(CO3)2 (i.e., mica is Na0.13K0.81Al1.81Mg0.15Fe0.08(Al0.87Si3.13O10)
the mineral previously identified as dolomite by XRD (OH)2. The methods used in determining the chemical
analysis is actually ferroan dolomite due to the presence composition of the phyllosilicates of Ballachulish slate
of a small amount of iron). are described in detail in previous work [6].
K: It is not easy to identify the white mica in the BSE Na: The small amount of sodium which appears on
image because it occurs in narrow bands which are not the elemental map is due to the presence of albite (Fig. 7).
significantly different in colour from the surrounding Fe and Mg: The pale grey mineral forming over 60%
minerals (Fig. 6). However examination of the elemental of the BSE image contains larger than average amounts
map for potassium shows clearly the location of the white of iron and magnesium and lower proportions of silicon
mica since none of the other minerals known to exist in and aluminium (Figs. 8 and 9). This mineral is chlorite.
Ballachulish slate contains potassium. In addition the The chemical composition is similar to that of the East
other elements present in white mica, e.g., aluminium, Laroch sample and has a chemical composition of
magnesium, silicon and iron, are also found in the same Al1.47Fe1.85Mg2.58Mn0.01(Al1.34Si2.66O10) (OH)8 [6].
locations on the elemental maps. The results of several Al: Aluminium is present in most of the minerals, the
greatest concentration being in white mica and a
somewhat lower concentration in chlorite (Fig. 10).
Si: The element silicon is present in all the minerals
except the dolomite, in concentrations decreasing from
45% by weight in quartz to progressively lower concen-
trations in white mica and chlorite (Fig. 11).
Comparing the two examples shown in Table 4, it can
be seen that the chemical composition (total oxide
content as determined using XRF analysis) of Balla-
chulish slate is highly variable. For example the higher
silicon oxide content in the Khartoum sample is
indicative of a higher quartz content than in the East
Laroch sample. It was found possible to estimate the
mineral composition of different samples using the total
oxide, as determined by XRF analysis and the chemical
Fig. 11. Elemental map of silicon; the bright test areas are quartz. composition of the individual minerals.
1102 J.A. Walsh / Materials Characterization 58 (2007) 1095–1103
Table 5
Mineral composition of slate Ballachulish slate based on the total oxide
composition as determined by XRF analysis (wt.% a)
Source Quartz Phyllosilicates Feldspar Iron ore Dolomite
(albite) mineral
White Chlorite
(pyrite)
mica
Khartoum 47.3 34.3 13.8 5.5 1.4 0 between minerals of similar density. This, followed by
East 34.6 26.3 21.1 4.5 2.7 6.5
Laroch
a
Totals may not precisely equal 100% due to rounding.
5.6. Algorithm used in the determination of the
percentage weight of each mineral
The chemical composition of the different minerals
was used, in combination with the total oxides present as
determined by XRF analysis, to calculate the weight of
each mineral present. One key element in each mineral
was used to determine the number of moles present. For
example the amount of apatite present was calculated
based on the moles of phosphorus and the corresponding
amount of calcium, then determined stoichiometrically
and subtracted from the total. The remaining calcium was
then attributed to ferroan dolomite according to the
average chemical composition determined using SEM
spot analysis. Other minerals were calculated in a similar
way and the final results were checked by comparing the
theoretical and actual volatiles. Total oxide analysis for
two samples of Ballachulish slate is shown in Table 5.
When compared with slates from different parts of the
quarry, and from other quarries in the area, there was a
wide variation in the relative proportions of the different
minerals. For example, the quartz content varies from
20% to 50%. This makes it impossible to identify a
Ballachulish slate based on the mineral content alone.
Of greater value in the identification of Ballachulish
slate is the actual chemical composition of the individual
minerals.
6. Conclusions
In arriving at the best understanding of the
characteristics and performance in service of slate as a
roofing material, a full analysis of its mineralogy is of
great value. This is not only because mineralogy is the
most significant factor directly influencing character-
istics and performance, but also because it enables
accurate identification of the provenance of used slates.
Slate has in the past been characterised in mineral-
ogical terms solely according to the proportions of its
phyllosilicates and quartz. This paper has shown that
this inadequately describes its mineralogy. With the
exception of quartz, all the minerals present vary in their
composition, so that to define completely the slate it is
necessary to determine the type of each mineral. This
paper demonstrates the use of SEM elemental maps in
identifying the minerals present, thereby distinguishing
spot analysis, enables the identification of accessory
minerals such as monzonite and the chemical compo-
sition of others such as ferroan dolomite. Having
analysed the chemical composition of the individual
minerals, the mineralogy can be calculated using the
bulk chemistry. The complete mineral characterisation
of the slate is used to confirm the provenance of the used
slates monitored.
Results are presented based on a fairly limited set of
samples from the quarries in the Ballachulish group in
Scotland. The techniques described are, however, appli-
cable to slates from any source.
Acknowledgements
I would like to acknowledge the help received in
preparation of the SEM images from John Hughes and
Margaret Corrigan. I would also like to acknowledge the
funding received for this research from Historic Scot-
land, the Scottish Stone Liaison Group and the Depart-
ment of Trade and Industry.
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