Clay Minerals (2005) , 317±332

40

Origin of mixed-layered (R1)

muscovite-chlorite in an anchizonal slate
from Puncoviscana Formation
(Salta Province, Argentina)
M. DO CAMPO 1 , * AND F. NIETO 2
1
Instituto de GeocronologõÂa y GeologõÂa Isoto
Âpica and Facultad de Ciencias Exactas y Nautrales, U.B.A., Pabello
Ân
2
INGEIS, Ciudad Universitaria, 1428 Buenos Aires, Argentina and Departamento de MineralogõÂa y PetrologõÂa and
I.A.C.T., Universidad de Granada-CSIC, Avda. Fuentenueva s/n, 18002 Granada, Spain

( Received 1 December 2004; revised 13 April 2005 )

ABSTRACT: Mica-chlorite mixed-layering was identified by X-ray diffraction (XRD) as a major

or subordinate constituent in several slates of the Puncoviscana Formation from Sierra de Mojotoro
(Eastern Cordillera, NW Argentina). In order to determine the crystallochemical characteristics of
these mixed-layered sequences and interpret their petrological meaning, anchizonal slate P90 was
chosen for TEM observations. In this slate, dioctahedral mica and chlorite form interleaved
phyllosilicate grains (IPG) or stacks, up to 110 m long, preferentially oriented with (001) planes at a
m

high angle to the slaty cleavage but also oblique to S0.

In agreement with XRD results, the main phyllosilicates identified by transmission electron
microscopy (TEM) were dioctahedral mica and random mixed-layer muscovite-chlorite, with
chlorite in subordinate amounts and scarce smectite. In the lattice-fringe images of mixed-layer
packets, a sequence of irregular stacking that produced apparent 24 AÊ (10 + 14) layers was observed,
but it was frequently possible to distinguish the 10 AÊ layers from adjacent 14 AÊ layers. In nearly all
packets, 14 AÊ layers prevail, exhibiting 14 AÊ:10 AÊ ratios between 1:1 and 3:1. Some elongated
lenticular fissures which are probably a consequence of layer collapse caused by the TEM vacuum
were identified in these packets. The straight, continuous appearance of lattice fringes plus the scarce
evidence of collapsed layers identified suggest that these packets correspond principally to mixed-
layer muscovite-chlorite, which is confirmed by analytical electron microscopy analyses. However,
smectite-like layers are probably the third component of some of these mixed-layer sequences, which
may account for their high Si and low (Fe + Mg) contents, their low interlayer charge in relation to
theoretical interlayer muscovite-chlorite, and for the presence of Ca in the interlayer site.
Textural relationships between chlorite and muscovite packets in IPG along with the observed
transformations from 14 AÊ to 10 AÊ along the layer, is compatible with a prograde metamorphic
replacement of chlorite in stacks by dioctahedral mica layers, probably in the presence of an aqueous
fluid.
KEYWORDS: mixed-layering, anchizone, Central Andes, Puncoviscana Formation, Argentina.
In the realm of diagenesis and low-grade meta- represent major components of pelitic and semi-
morphism, illite/muscovite and chlorite commonly pelitic rocks and frequently constitute fine-scaled
intergrowths called stacks, or interleaved phyllosi-
licate grains (IPG from Francescheli ., 1991). et al

* E-mail: docampo@ingeis.uba.ar Curiously however, illite-chlorite or muscovite-

DOI: 10.1180/0009855054030176 chlorite mixed-layering rarely appears at the
# 2005 The Mineralogical Society
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 318
atomic scale, based on the few reports of such
phases in the literature (Lee ., 1984; Lee &
et al
Peacor, 1985, Ahn & Peacor, 1986). Mixed-layering
of dioctahedral mica and trioctahedral chlorite is
less common than mixtures between biotite and
trioctahedral chlorite, described on multiple occa-
sions and considered to be the result of biotite
alteration (e.g. Veblen & Ferry, 1983; Eggleton &
Banfield, 1985). As Lee & Peacor (1985) noted,
ordered mixed layering of this type should not be
stable in large volumes, owing to the large
difference in and crystallographic dimensions
a b
between dioctahedral and trioctahedral layers. Such
a mismatch implies that considerable strain must
exist across the layer boundaries.
Different mechanisms of formation have been
invoked to explain mixed-layer dioctahedral mica-
trioctahedral chlorite. Lee & Peacor (1985) inter-
preted the random mixed layering between 10 AÊ
layers and 14 AÊ layers which they observed in a
transitional sample from mudstone to slate as an
intermediate stage in the development of slaty
cleavage that would begin with the dissolution of
illite and chlorite grains, and probably I-S, parallel
to bedding. These authors considered that dissolu-
tion and crystallization, rather than solid-state
reactions, were the primary mechanism of transfor-
mation. In turn, mixed-layer illite-chlorite occurring
in volcanogenic sediments was interpreted by Ahn
& Peacor (1988) as formed through crystallization
following dissolution of smectite. In contrast, Knipe
(1981), in his study of slaty cleavage development,
interpreted the irregular mixed layering of chlorite
layers inside mica packets as developed by solid-
state reordering of illite.
On the other hand, the origin of muscovite-
chlorite stacks was discussed extensively by Li
al . (1994), who carried out a TEM and AEM study
of their occurrence in Lower Palaeozoic mudstones
of the Welsh Basin. Those authors concluded that
these stacks were derived from a detrital precursor,
such as volcanogenic biotite, and other ferromagne-
sian minerals, which underwent considerable
textural change in response to diagenesis and very
low-grade metamorphism. According to Li .,
(1994), most intergrowths of chlorite and mica in
stacks formed by mica replacement of chlorite and
altered biotite along cleavage fissures. A coincident
model was proposed by Giorgetti . (1997) to et al
explain the origin of the widespread IPG occurring
in low-grade Verrucano metasediments of the
northern Apennines (Italy). However, evidence
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M. Do Campo and F. Nieto
exists for the original growth of chlorite-mica
stacks as crystals parallel to bedding in a diagenetic
foliation at very low to low-grade metamorphic
conditions, prior to deformation (Weber, 1981;
Greg, 1986).
In this study we examined mixed-layer musco-
vite-chlorite occurring in anchizonal slate from the
Puncoviscana Formation (Eastern Cordillera, NW
Argentina). This material was first detected by
XRD, as it represents a major component of the
clay fraction. In this slate, dioctahedral mica and
chlorite also form interleaved phyllosilicate grains
that can be recognized at the optical scale. The
purpose of this work is to study in detail mixed-
layer mica-chlorite by scanning electron microscopy
(SEM) and transmission electron microscopy
(TEM) with the aim of determining their crystal-
lochemical characteristics, and to interpret their
petrological meaning.
GEOLOGY AND SAMPLE
DESCRIPTION
Mixed-layer mica-chlorite was identified by XRD,
as described below, in several Puncoviscana slates
from Sierra de Mojotoro, in which they may
represent a major or a subordinate phase.
Anchizonal slate P90 (KI = 0.30) was chosen for
TEM observations because, according to X-ray
data, it contains abundant interstratified musco-
vite-chlorite; furthermore, it displays less evidence
of retrograde alteration of clay minerals than other
slates of the area (Do Campo, 1999b; Do Campo &
Nieto, 2003). This sample comes from an outcrop
of the Puncoviscana Formation (Turner, 1960)
located near Chamical church in Sierra de
et Mojotoro, Salta province, Argentina (Fig. 1). The
Puncoviscana Formation, which constitutes the
basement of the area, is mainly composed of a
pelite-greywacke turbidite sequence, with subordi-
nate sandstones and locally interbedded conglom-
erates, shelf limestones, and volcanic rocks
(Omarini, 1983; Omarini & Baldis, 1984; Jezek,
1990). The Neoproterozoic Puncoviscana Formation
et al was affected by polyphase deformation due to
superposed folding. Mon & Hongn (1991, 1996)
have identified two NS belts with different tectonic
styles (Fig. 1) in the basement of northwestern
Argentina. According to these authors, Sierra de
Mojotoro corresponds to the eastern Lules-
Puncoviscana belt, which is characterized by
asymmetric folds overturned to the west, with
 Mixed-layer muscovite-chlorite 319

FIG. 1. Geological sketch and location map.

concomitant development of axial plane cleavage.
A second superimposed deformation produced
crenulation cleavage and associated microfolding,
which affected bedding and the axial plane
cleavage. This unit is uncomformably overlain by
Cambrian sandstones of the Meson Group. Do
Campo . (1998), Do Campo (1999a,b), and Do
et al
Campo & Nieto (2003) studied the metamorphic
evolution of these rocks, determining the mineral
assemblages of slates, the KuÈbler index (KI), and
the parameter of white mica by powder XRD. The
b formed white mica grains, 10ÿ50 m long, show
white mica indicates intermediate-pressure condi-
tions for the metamorphism (Do Campo et al.,
1998; Do Campo, 1999a).
The slate studied is mainly composed of detrital
quartz and albite plus newly formed phyllosilicates,
and alternates between silt and clay-rich laminae
several mm thick. Clasts were reduced in size by
pressure solution, alteration and mechanical frag-
mentation, which produced elongated quartz and
plagioclase grains with preferred orientation. Newly
m

metamorphic grade established via KI indicated preferred alignment that causes a continuous slaty
medium anchizonal to epizonal grade meta- cleavage in clay-rich laminae and leads to
morphism for the Puncoviscana Formation in the disjunctive anastomosing cleavage in quartz-plagi-
Sierra de Mojotoro. In addition, the parameter ofb oclase-rich silt laminae. In thin section, tabular to

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 320 M. Do Campo and F. Nieto

lenticular interleaved phyllosilicate grains (IPG) up
to 110 m long, sometimes bent or folded, are
m sections were employed for optical observations and
abundant, especially in clay-rich laminae. The IPG
aspect ratio (length/width) ranges from 0.7 to 5.3,
with a mean of 2.8. Alternating chlorite-like and
mica-like packets are always subparallel and can be
easily distinguished when both kinds of layers make
up a similar volume of the IPG (Fig. 2a). In other
cases, chlorite packets clearly predominate, and
then the IPG resemble pure chlorite grains under
the optical microscope and even in backscattered
SEM images (Fig. 2b). Chlorite shows slight green
pleochroism and very weak birefringence. The IPG
are preferentially orientated with chlorite and
muscovite (00l) planes at high angle to the slaty
cleavage but also oblique to S0, which in turns
forms an angle of 70ë with the former.
ANALYTICAL TECHNIQUES
The clay mineralogy was studied by XRD using
oriented mounts, with Cu- radiation, employing a
Ka
Philips PW1050 diffractometer (INGEIS) operated
at 40 mA and 30 kV, and a Bruker D8 Advance
operated at 40 mA and 40 kV (Centro de
y = 1.15 ÿ 0.01 ( 2 = 0.989). Polished thin
x R
SEM study using back-scattered electron (BSE)
imaging and X-ray dispersive (EDS) analysis.
Analyses were carried out with a LINK QX2000
microanalyzer attached to a ZEISS DSM 950
scanning electron microscope. The following
compounds were used as calibration standards:
albite (Na), orthoclase (K), periclase (Mg), wollas-
tonite (Si), and synthetic oxides of Al2O3 (Al),
Fe2O3 (Fe) and MnTiO3 (Ti and Mn).
Representative areas for TEM observations were
chosen based on prior observations by optical
microscopy and SEM of thin sections. The sample
was prepared as a Canada-balsam-mounted thin
section oriented approximately normal to bedding.
It was further thinned using a Gatan 600 ion mill
and carbon-coated for TEM observation with a
Philips CM-20 scanning transmission electron
microscope (STEM) equipped with an ultra-thin
window EDX detector (Centro de InstrumentacioÂn
CientõÂfica, C.I.C., Granada University). Quantitative
analyses (AEM) were obtained only from thin
edges, using a 70 AÊ beam diameter and a
1000 200 AÊ scanning area, with the long axis
6

Instrumentacio n CientõÂfica, Universidad de oriented parallel to the phyllosilicate packets. The

Granada). The <2 m size fraction separated by
m sample was tilted by 20ë towards the detector,
centrifugation was scanned air-dried after saturation giving an X-ray take-off angle of 34ë. Standards
with ethylene glycol (EG) and heating at 500ëC. used to obtain the k-factors for the transformation
The KI was determined following the recommenda- of intensity ratios to concentration ratios, following
tions by Kisch (1991); our data were converted to the methods of Cliff & Lorimer (1975) and
the CIS scale (Warr & Rice, 1994) by the formula: Champness et (1981) were: albite, biotite,
al.

FIG. 2. BSE images of P90 slate: (a) IPG composed of alternating muscovite and chlorite packets; (b) IPG with a
predominance of chlorite packets, resembling a pure chlorite grain.

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 Mixed-layer muscovite-chlorite
spessartine, muscovite, olivine, titanite, CaSO4 and
MnSO 4 . Atomic concentration ratios were
converted into formulae according to stoichiometry
(number of oxygen atoms in theoretical formulae).
Structural formulae of mixed-layer clay minerals
were calculated on the basis of 25 oxygen atoms
(14 chlorite + 11 mica). Alkali loss is a significant
problem in the TEM analysis of clay minerals,
particularly for defect-rich minerals (Van der
Pluijm et ., 1988). Therefore, short counting
al
times were employed as a compromise for major
alkali analysis (Nieto ., 1996).
et al
X-ray diffraction data
In the pattern of the air-dried oriented mount, the
basal reflections of illite-muscovite appear along
with an irrational series of reflections (at 12.45,
7.99, 6.26, 4.84, 4.17 and 3.49 AÊ). Furthermore, on
the high-angle side of the 7.99 AÊ peak there is a
shoulder corresponding to 7.35 AÊ (Fig. 3a). The
XRD patterns of the EG-treated and heated
specimens were not included in the figure because
they register minimal changes. After EG treatment,
illite-muscovite basal reflections do not show
significant changes: the shoulder at 7.35 AÊ persists
and the irrational series of basal reflections remains
almost unchanged except for the reflection at
12.45 AÊ, which decreases in intensity. In the same
pattern, a weak reflection visible at 17.5 AÊ becomes
unobservable after heating, and must thus corre-
spond to smectite (<5%). After heating, the peak at
12.45 AÊ shifts towards 11.95 AÊ and increases in
intensity, resembling the behaviour of odd reflec-
tions of chlorite under this treatment. Taking into
account the optical observations of thin sections,
this irrational series of basal reflections was
interpreted as due to irregular muscovite-chlorite
mixed-layering.
The reflections attributed to the mixed-layer
phase are broad and asymmetrical, suggesting that
reflections from two or more phases may overlap.
In order to investigate this further, a decomposition
program ( ) was applied to the low-angle
MacDiff
region (3ÿ14ë2 ) of the air-dried XRD pattern
(results shown in Fig. 3b). The peak at 12.45 AÊ can
y
be decomposed into two peaks attributed to
smectite (1) and mixed-layer muscovite-chlorite (2),
in accordance with the changes observed in XRD
diagrams after EG and heat treatments. Meanwhile,
the peak at 7.99 AÊ can be resolved into three peaks
attributed to mixed-layer muscovite-chlorite (4),
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321
chlorite (6), and subordinate mixed-layer musco-
vite-chlorite very rich in chlorite layers (5).
In order to corroborate the interpretation of the
mixed-layer phase, several simulated patterns were
calculated with the program, varying the
MULCALC
relative proportions of muscovite and chlorite layers
in the mixed-layer sequence and the Reichweite
value. A good match with the experimental pattern
was obtained for a mixture of 60% chlorite layers
and 40% muscovite layers with R = 1 (Fig. 3c).
TEM results
In agreement with the XRD results, the main
phyllosilicates identified by TEM were dioctahedral
mica and mixed-layer muscovite-chlorite, with
chlorite in subordinate amounts and scarce smectite.
Muscovite occurs as coarse grains, interleaved with
chlorite packets in IPG grains, and it is the main
phyllosilicate in the matrix. Chlorite was identified
forming coarse grains 40ÿ125 m long and as a
m
subordinate phase in the matrix. Mixed-layer
muscovite-chlorite appears in IPG grains
20ÿ110 m long and interleaved in chlorite crystals.
m
The dominant polytype in dioctahedral micas is
2 , although 1 and three-layer sequences where
M Md
c* is perpendicular to * (or equivalent crystal-
b
lographic directions), therefore interpreted as 3 , T
were also recognized (Fig. 4a). Dioctahedral mica is
present in defect-free packets 15ÿ470 layers thick,
exhibiting straight and continuous 10 AÊ or 20 AÊ
lattice fringes. Up to four consecutive coherent
packets of muscovite have been observed, and, less
commonly, low-angle boundaries are also present.
Some isolated 14 AÊ layers interlayered inside thick
mica packets were seen in a few cases.
The SAED patterns obtained for the mixed-layer
muscovite-chlorite have the following reflections in
the 001 row (CV = coefficient of variation):
Fig. 4b: 12.0, 7.4, 5.9, 4.6, 3.7, 3.2, 2.8, 2.6, 2.3, 1.9,
1.8 AÊ. (CV = 2.6%).
Fig. 4c: 22.2, 12.0, 7.7, 6.1, 4.7, 3.9, 3.4, 2.9, 2.6, 2.3,
2.2, 2.0 AÊ (CV = 2.6%).
Fig. 4d: 12.2, 7.8, 6.2, 4.8, 3.5, 3.0, 2.7, 2.4, 2.0,
1.7 AÊ (CV = 1.6%).
The coincidence between the XRD and the
SAED data is quite good, although the shape and
position of the first peak in the XRD traces (002
reflection) seems to be affected by the presence of
smectite. In both cases, reflections appear at
7.3ÿ7.4 AÊ (underlined in the spacing list), possibly
 322 M. Do Campo and F. Nieto

FIG. 3. XRD patterns: (a) of the <2 m air-dried oriented mount of slate P90; (b) decomposition of the low-angle
m

region of the air-dried pattern (obtained using ); (c) simulated pattern for a mixture of 60% chlorite
MacDiff
layers and 40% muscovite layers with R=1 (obtained using ). MULCALC

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 Mixed-layer muscovite-chlorite
attributable to chlorite. The CV values obtained for
these patterns are greater than the value of 0.75%
established by the Association Internationale pour
l'Etude des Argiles (AIPEA) for rational XRD
patterns (Bailey, 1982); therefore, the patterns
FIG. 4. SAED patterns. (a) 100 pattern of 3
muscovite; (b), (c) and (d): 100 or equivalent image FIG. 5. Lattice-fringe image of irregular mixed-layer
of mixed-layer muscovite-chlorite.
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323
obtained must be considered to be of random
mixed layering. In addition, non-00 reflections are
l
ill-defined, non-periodic and markedly diffuse
parallel to . The parameter is equal to 9.1 AÊ.
c* b
A sequence of irregular stacking produced fringes
with 24 AÊ periodicity, but frequently it is possible
to distinguish the 10 AÊ layers from the adjacent
14 AÊ layers. In nearly all packets, 14 AÊ layers
prevail, exhibiting 14 AÊ/10 AÊ ratios between 1:1
and 3:1 (Figs 5 and 6). In one case, five consecutive
14 AÊ fringes were observed inside a mixed-layer
muscovite-chlorite packet. The 10ÿ14 AÊ pair is
repeated up to seven times; this order is broken by
stacking faults (10-14-14-10), excess 14 AÊ layers,
or, less frequently, 10 AÊ layers. A few lenticular
voids as consistent with layer collapse caused by
the TEM vacuum were identified.
Other examples of 10ÿ14 AÊ mixed layering can
be seen in Fig. 7, displaying a fine-scale interleaved
phyllosilicate grain composed of eight subparallel
packets of random mixed-layer muscovite-chlorite
(A and B), chlorite and muscovite. The mixed-layer
packet A (Fig. 7b) shows the same characteristics
as those described above. Packet B is similar to A,
but less disordered, comprising >50% of 14 AÊ
layers. The straight, continuous appearance of
lattice fringes in all the mixed-layer packets
imaged in this sample, plus the scarce evidence of
collapsed layers identified (Fig. 7a,b), suggests that
they correspond principally to mixed-layer musco-
vite-chlorite. However, scarce smectite layers could
be present. The AEM analyses carried out for these
packets (Table 1) reveal highly variable composi-
T
muscovite-chlorite.
 324 M. Do Campo and F. Nieto

Nevertheless, AEM analyses clearly indicate that

these packets correspond to interstratifications of
chlorite-like and dioctahedral mica-like layers. The
main cation in the interlayer site is K, sometimes
accompanied by Ca. In some cases, the interlayer
charge is lower than expected for muscovitic 10 AÊ
layers, which could be a consequence of the
existence of illitic substitution in mica-like layers.
However, the comparison with EDS analyses
indicates that problems of alkali loss could have
affected some AEM analyses. In addition, several
analyses exhibiting low (Fe+Mg)/Si contents
(P90-8, P90-3 in Table 1) or Ca in interlayer sites
(P90-12 in Table 1) may correspond to complex
muscovite-chlorite-smectite mixed-layering.
In this sample, diffraction patterns characteristic
of semi-random chlorite were obtained occasionally
(Fig. 8, inset). Furthermore, in almost all the lattice-
fringe images, 10 AÊ layers were observed inter-
layered among predominant 14 AÊ layers, in ratios
from 1:4 to 1:10. Some elongated lenticular
fissures, which are probably a consequence of
layer collapse caused by the TEM vacuum, were
FIG. 6. Lattice-fringe image of irregular mixed-layer identified in these packets. Figure 8, for example,
muscovite-chlorite packets. This image is bidimen- shows a packet with 25 successive 14 AÊ layers and
sional; the cross fringes correspond to or 110. an area that has no more than 3 to 7 consecutive
14 AÊ layers and 10 AÊ layers in between. The 10 AÊ-
b*
These cross fringes show continuity along 5 to 10
successive 14 AÊ or 10 AÊ layers as well, denoting the 14 AÊ pair is repeated no more than three times. In
existence of crystallographic continuity along (or this same image, lateral transformation from 14 AÊ
layers to 10 AÊ is evident. These data further
b
equivalent directions such as <110>) for both kinds of
layers. validate the results obtained by decomposition of
the XRD trace (Fig. 3b), as the peak at 7.99 AÊ was
tions, in part due to the variable proportions of resolved in a mean peak at 7.97 AÊ attributed to the
14 AÊ to 10 AÊ layers from one packet to another. mixed-layer muscovite-chlorite, and two less
TABLE 1. AEM analyses of mixed-layer muscovite-chlorite.
Element P90-3 P90-4 P90-8 P90-12 P90-1b P90-5b P90-7b P90-8b
SiIV 6.14 5.58 6.24 5.69 5.62 5.60 5.14 5.67
Al 1.86 2.42 1.76 2.31 2.38 2.40 2.86 2.33
VIAl 2.14 2.00 2.74 1.74 1.88 1.86 1.67 1.67
Mg 3.18 3.53 2.24 3.50 3.47 3.47 3.73 3.72
Fe 3.12 3.45 3.29 3.83 3.56 3.55 4.09 3.76
Ti 0.05 0.02 0.00 0.00 0.00 0.00 0.00 0.00
Mn 0.06 0.04 0.00 0.00 0.07 0.07 0.00 0.00
S oct. 8.55 9.05 8.27 9.07 8.98 8.95 9.48 9.15
K 0.43 0.19 0.48 0.14 0.42 0.51 0.23 0.36
Na 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
Ca 0.00 0.00 0.00 0.14 0.00 0.00 0.00 0.00
S int 0.43 0.19 0.48 0.28 0.42 0.51 0.23 0.36

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 Mixed-layer muscovite-chlorite 325

FIG. 7. (a) Lattice-fringe image of a fine-scale IPG made up of packets of random mixed-layer muscovite-chlorite
(A and B), chlorite and muscovite. (b) Detail of chlorite and mixed-layer packet A; black arrows indicate
elongate lenticular fissures which are probably a consequence of layer collapse caused by the TEM vacuum.

intense peaks at 7.54 AÊ and 7.19 AÊ, interpreted as
mixed-layer muscovite-chlorite very rich in chlorite
layers and a chlorite (002) reflection, respectively.
The lattice-fringe images shown in Figs 6 and 8
are bidimensional, meaning that, in addition to the
basal fringes, they show cross-fringes corresponding
to imaging (0 0) or (110) rows of reflections. These
k and muscovite. The mixed-layer packet shows 24,
cross-fringes show continuity along 5 to 10
successive 14 AÊ layers or 10 AÊ layers. This
feature indicates the existence of crystallographic
continuity along (or equivalent directions such as
b observed. Only four packets of chlorite without
<110>) for both kinds of layers, which means that
this mixed-layer sequence has crystallographic
coherence. In other words, it is a crystal and not
merely a fortuitous stacking of layers (Dong &
Peacor, 1996).
The unique diffraction pattern of ordered chlorite
obtained in this sample (Fig. 9, inset) corresponds
to a one-layer polytype (1L). In addition, this
pattern shows spots corresponding to 10 AÊ periodi-
city superimposed in the (001) row that could be
correlated with mica. Figure 9 depicts a fine-scale,
IPG composed of three subparallel packets of
chlorite, a random mixed-layer muscovite-chlorite,
28 and 20 AÊ fringes with a 24 AÊ:14 AÊ ratio of 3:10;
moreover, some lenticular voids, as consistent with
layer collapse caused by the TEM vacuum, were
interleaved 10 AÊ layers were identified (packets
labelled Chl in Figs 7b and 9).
The AEM analysis of this IPG (P90-8) indicates a
mixture of dioctahedral mica and trioctahedral
chlorite with a predominance of chlorite layers, in
agreement with evidence from the lattice-fringe
image. However, the interlayer charge (K = 0.48) is

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 326
FIG. 8. SAED pattern along 100 (inset) and lattice-
fringe image of semi-random chlorite showing 10 AÊ
layers interlayered among predominant 14 AÊ layers.
Black arrow indicates an along-layer transformation
from 14 AÊ to 10 AÊ.
less than expected for such a mixture of a
muscovite, chlorite and mixed-layer muscovite-
chlorite. This fact, linked to the existence of
lenticular voids compatible with layer collapse
under the TEM vacuum, indicates that some of
the 10 AÊ layers in the mixed-layer packet are
probably smectitic.
Smectite occurs in packets clearly discordant
with other phyllosilicates, suggesting later forma-
tion. The AEM analyses of these packets reveal
dioctahedral smectite:
Si3.66 Al0.34(Al1.39Mg.0.33Fe0.39)K0.34O10(OH)2.
SEM-EDS composition of phyllosilicates
Representative chemical analyses of mixed-layer
muscovite-chlorite, dioctahedral mica, and chlorite
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M. Do Campo and F. Nieto
are presented in Tables 1, 2 and 3. Although the
AEM analyses of mixed-layer grains were discussed
briefly in the previous section, here they are
considered together with EDS analyses of chlorite
with evidence of mixed-layering and compared with
muscovite and chlorite compositions obtained by
EDS.
Dioctahedral micas . The matrix, as well as the
coarse grains and IPG illite-muscovite, displays a
wide range of variation in Si and in (Fe+Mg)
contents. In the Si-(Fe+Mg) diagram (Fig. 10a),
almost all analyses plot above the line for ideal
Tschermak substitution, indicating that a ferri-
muscovitic component is present in addition to
phengitic substitution. The Si/Al-interlayer charge
diagram (Fig. 10b) suggests that dioctahedral micas
from both the matrix and the IPG have low illitic
substitution. As can be seen in Table 2 and Fig. 10,
the Si content of the matrix mica is slightly higher
than that of the IPG, implying a greater phengitic
component in the former.
Chlorite. Only five chlorite analyses with <0.1
alkali cations (Na+K+Ca) p.f.u. were obtained at
the SEM scale (Table 3a). These analyses were
performed on coarse chlorite grains 40ÿ125 m m
long and also on chlorite packets in the IPG. Most
of the analyses, although carried out on grains
appearing to be homogeneous chlorite crystals
under BSE images, display a sum of octahedral
cations <6, variable amounts of alkali cations and in
some cases a high Si content (Table 3b). A similar
result was obtained at the TEM scale when crystals
identified as chlorite by SAED were analysed (P90-
8 and P90-12 in Table 1). In these cases, lattice-
fringe images reveal the existence of 10 AÊ layers
interleaved between dominant chlorite packets. The
less contaminated SEM analyses exhibit a structural
formula corresponding to magnesian chamosite
(Fe/(Fe+Mg) = 0.53):
(Si2.76Al1.24)(Al1.28Mg2.16Fe2.47Mn0.04)O10(OH)8.
Mixed-layer . The diagram
muscovite-chlorite
chosen for representing the compositions of mixed-
layer packets was (Fe+Mg)/Si ÿ Interlayer sum/Si,
because it is not affected by the normalization
criterion employed, and clearly discriminates among
muscovite, biotite-chlorite and chlorite-smectite
mixed-layering (Fig. 11). Moreover, this diagram
enables the identification of more complex mixed-
layer sequences composed of three different kinds of
layers. The EDS analyses of chlorite and muscovite
obtained for slate P90, along with the analyses of
 Mixed-layer muscovite-chlorite 327

FIG. 9. SAED pattern along 100 of ordered chlorite one layer polytype (inset) and corresponding lattice-fringe
image showing a fine-scale interleaved phyllosilicate grain composed of three sub-parallel packets of chlorite,
random mixed-layer muscovite-chlorite and muscovite.
mixed-layer grains obtained by EDS and AEM, are all of the analyses plot to the left of the upper line
also plotted in Fig. 11. Representative analyses of that connects the muscovite and chlorite composi-
biotite and smectite, plus 0.5/0.5 mixtures of tions. Second, the low (Fe+Mg)/Si and
muscovite-chlorite, chlorite-smectite, and biotite- (K+Na+Ca)/Si ratios exhibited by some AEM, as
chlorite, are also included in Fig. 11 for reference. well as EDS analyses of mixed-layer muscovite-
Two main conclusions are inferred by this figure. chlorite is apparent, which can be attributed to some
First, the dioctahedral character of 10 AÊ layers in the extent to the illitic component of muscovite-like
mixed-layer sequence is clearly implied, as almost layers. However, smectite-like layers are probably

FIG. 10. Diagrams showing composition relations for dioctahedral micas from IPG and mx.

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 328 M. Do Campo and F. Nieto

TABLE 2. SEM analyses of dioctahedral micas from matrix (mx), coarse grains (CG) and interleaved phyllosilicate
grains (IPG).
mx CG CG mx IPG mx
Element P90/2/3 P90/3/2 P90/5/3 90/6/2 P90/8/1 P90/8/3
SiIV 3.35 3.31 3.30 3.40 3.33 3.37
Al 0.65 0.69 0.70 0.60 0.67 0.63
VIAl 1.54 1.57 1.50 1.52 1.50 1.52
Mg 0.24 0.26 0.26 0.23 0.21 0.25
Fe 0.23 0.19 0.28 0.23 0.31 0.25
Ti 0.01 0.02 0.02 0.02 0.02 0.01
Mn 0.00 0.00 0.01 0.00 0.00 0.00
S oct. 2.03 2.04 2.06 2.00 2.04 2.04
K 0.81 0.87 0.83 0.86 0.80 0.79
Na 0.04 0.00 0.00 0.02 0.03 0.03
Ca 0.01 0.00 0.01 0.00 0.00 0.01
S int 0.85 0.87 0.84 0.88 0.83 0.82
mx CG mx mx IPG IPG
Element P90/13/3 P90/14/2 P90/14/3 P90/15/1 P90/16/2 P90/17/2
SiIV 3.32 3.22 3.32 3.53 3.27 3.23
Al 0.68 0.78 0.68 0.47 0.73 0.77
VIAl 1.58 1.57 1.65 1.51 1.61 1.65
Mg 0.18 0.17 0.13 0.24 0.22 0.22
Fe 0.23 0.25 0.21 0.21 0.18 0.14
Ti 0.01 0.03 0.02 0.02 0.03 0.02
Mn 0.00 0.00 0.01 0.00 0.00 0.00
S oct. 2.00 2.02 2.01 1.98 2.03 2.04
K 0.88 0.90 0.74 0.79 0.85 0.83
Na 0.05 0.04 0.08 0.01 0.02 0.04
Ca 0.00 0.00 0.01 0.01 0.00 0.01
S int 0.92 0.94 0.82 0.80 0.86 0.88

the third component of some of these mixed-layer
sequences, which may account for their high Si and
low (Fe+Mg) contents, their low interlayer charge in
relation to theoretical interlayered muscovite-
chlorite, and for the presence of Ca in interlayer site.
DISCUSSION
The disordered mixed-layer muscovite-chlorites
described in this study are analogous to those
described by Lee . (1984) and Lee & Peacor
et al
(1985) for a sample that is transitional between
mudstone and slate from Lehigh Gap in
Pennsylvania. Those authors pointed out that, even
though the mudstone contained abundant phyllosi-
licate grains with orientations parallel to bedding,
mixed-layer illite-chlorite occurred only parallel to
the slaty cleavage of the adjacent slates. Based on
their observations at TEM scale, they considered
that random and ordered mixed-layer illite-chlorite
developed by dissolution of illite and chlorite
detrital grains, and probably I-S, parallel to
bedding, followed by crystallization of the new
phyllosilicate parallel to the slaty cleavage. Lee &
Peacor (1985) remarked that these complex mixed-
layer sequences are clearly indicative of a
metastable state, because equivalent samples that
had been transformed into slate displayed no local
illite-chlorite mixed-layering.
The sample under consideration is clearly an
anchizonal slate (KI = 0.30 with a predominance of
2 muscovite) in which muscovite and chlorite
M
appear interleaved from the lattice to the millimetre
scale. Mixed-layer packets appear in the IPG, which
are oblique to S0, or associated with chlorite in the
matrix. Few chlorite packets without interleaved

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 Mixed-layer muscovite-chlorite 329
TABLE 3. SEM analyses of chlorite: (a) pure chlorite, (b) chlorite with evidence of mixed layering.
(a)
Element P90/1/1 P90/4/1 P90/9/2 P90/11/2 P90/16/1
SiIV 2.85 2.83 2.89 2.75 2.76
Al 1.15 1.17 1.11 1.25 1.24
VIAl 1.34 1.28 1.36 1.36 1.28
Mg 2.08 2.18 2.05 2.04 2.16
Fe 2.36 2.41 2.33 2.45 2.47
Ti 0.01 0.00 0.01 0.00 0.00
Mn 0.02 0.03 0.03 0.03 0.04
S oct. 5.81 5.90 5.78 5.88 5.94
K 0.04 0.00 0.00 0.00 0.00
Na 0.03 0.01 0.02 0.04 0.00
Ca 0.03 0.01 0.04 0.01 0.00
S Na+K+Ca 0.09 0.02 0.07 0.05 0.00
(b)
Element P90/3/1 P90/4/2 P90/5/1 P90/5/2 P90/13/1
SiIV 3.35 3.27 3.23 3.00 3.12
Al 0.65 0.73 0.77 1.00 0.88
VIAl 1.44 1.52 1.54 1.64 1.45
Mg 2.11 2.01 2.02 1.81 2.02
Fe 1.83 1.99 1.97 2.08 2.14
Ti 0.00 0.02 0.00 0.00 0.00
Mn 0.02 0.02 0.03 0.03 0.02
S oct. 5.40 5.55 5.57 5.56 5.63
Na 0.00 0.00 0.00 0.00 0.04
K 0.03 0.03 0.03 0.08 0.02
Ca 0.17 0.00 0.00 0.04 0.03
S Na+Ca+K 0.20 0.03 0.03 0.12 0.09

mica-layers were identified by SEM and TEM in
the IPG, forming coarse grains, or in the matrix.
The studied mixed-layer sequences do not have a
distinct composition, as opposed to the sum of
muscovite- plus chlorite-like layers. Therefore, they
do not represent an independent mineral phase, as,
for example, corrensite in relation to chlorite plus
smectite (Shau ., 1990). As regards their
et al
composition, the interstratified sequences of slate
P90 differ from the mixed-layer mica-chlorite
described by RuõÂz Cruz (2001), which display
intermediate composition between muscovite-
chlorite and biotite-chlorite.
Textural relationships between chlorite and
muscovite packets in IPG along with the observed
transformations from 14 AÊ to 10 AÊ along the layer
are compatible with a prograde metamorphic
replacement of chlorite in stacks by dioctahedral
mica layers, probably in the presence of an aqueous
fluid. Such a mechanism has been described by
Giorgetti . (1997) to account for 10 AÊ layers
et al
interleaved in predominant chlorite packets of the
IPG in Verrucano metasediments, in which mixed-
layer mica-chlorite represent a minor component.
As Giorgetti . (1997) pointed out; the proposed
et al
reaction involves significant chemical 2+changes
requiring a loss of divalent cations +(Mg , Fe2+4+)
and of H2O, and a gain of K and Si .
Furthermore, this reaction can be considered a
topotactic transformation as the newly formed mica
layers retain the crystallographic orientation of the
previous chlorite. Thus, the proposed transformation
mechanism seems to imply that 14 AÊ and 10 AÊ
layers that form the mixed-layer sequence are not

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 330
FIG. 11. Chemical variations of muscovite, chlorite
(both minerals analysed by EDS) and mixed-layer
muscovite-chlorite (AEM and EDS analyses) on the
Na + K + Ca/Si Fe + Mg/Si diagram. Representa-
vs.
tive analyses of biotite and smectite, plus 0.5/0.5
mixtures of muscovite-chlorite, chlorite-smectite and
biotite-chlorite were included in order to use them as a
reference.
co-genetic, but the result of a replacement of one by
another. However, the evidence is not strong
enough to enable us to discard alternative inter-
pretations such as those of Lee & Peacor (1985)
and RuõÂz Cruz (2001), who postulated that the
mica- and chlorite-like layers that make up
interstratified illite-chlorite formed at the same
time.
The transformation reaction did not achieve
completion, probably due to kinetic factors, the
existence of irregular mixed layering at the
angstrom scale is unambiguously inconsistent with
the phase rule and therefore with attainment of
stable equilibrium (Essene & Peacor, 1995).
Another indication of a lack of thermodynamic
equilibrium in this sample is the different mica
compositions between the matrix and the IPG sites.
The difference in and lattice dimensions
a b
between muscovite and trioctahedral chlorite layers
in the IPG is smaller than for ideal end-member
compositions as a result of the phengitic substitu-
tion recorded in muscovite. The and parameters
a b
of the IPG mica, calculated from its average Si
content with the equation given by Guidotti .
(1989) are 5.208 AÊ and 9.034 AÊ, respectively. On
the other hand, the parameter of chlorite
b
calculated from its average (Fe + Mn) content
with the equation given by Nieto (1997) is 9.295 AÊ.
Although lower, the mismatch between the and
lattice parameters of both kinds of layers persists
and probably prevents the progression of ordering,
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M. Do Campo and F. Nieto
which is only present at the local scale. As Lee &
Peacor (1985) noted, such a mismatch always
implies that considerable strain must exist across
the layer boundaries, and therefore ordered mixed-
layering of this type should not be stable over large
volumes.
The existence of smectite in this slate as well as
the occurrence of smectitic layers in mixed-layer
packets are incompatible with a prograde meta-
morphic episode and are inferred to result from
retrograde diagenetic reactions (Nieto ., 2005).
et al
Considerable evidence of retrograde reactions was
found in Puncoviscana Formation slates from Sierra
de Mojotoro, including retrograde alteration of
chlorite by vermiculite and muscovite replacement
by smectite (Do Campo, 1999b; Do Campo &
Nieto, 2003). Retrograde alteration of chlorite to
smectite at the regional scale was first described by
Nieto . (1994) for slates of sub-greenschist
et al
facies in the Sierra EspunÄa (Betic Cordillera,
Spain). In those rocks, smectite occurs intercalated
with trioctahedral chlorite as thin packets of layers,
and as individual layers that commonly change to
chlorite along the layers. These authors considered
that the replacement of chlorite by smectite took
place under oxidizing conditions due to the
introduction of groundwater after the uplift of the
Betic Cordillera (Nieto ., 1994). In agreement
et al
with those authors, the origin of the retrograde
phases identified in slates from the Sierra de
Mojotoro was interpreted by Do Campo & Nieto
(2003) as the result of the interaction between rocks
and groundwater, under oxidizing conditions, after
the uplift of the Puncoviscana Formation in the
Lower Ordovician.
ACKNOWLEDGMENTS
The help of M.M. Abad-Ortega (Centro de
InstrumentacioÂn CientõÂfica, Universidad de Granada)
with the TEM and AEM, I. Guerra Tschuschke with the
SEM and EDX, J.D. Montes Rueda with the ion mill
and A. Molina Illescas in the photographic laboratory
was essential for the present work. C. Laurin helped
with the English in the manuscript. Financial support
et al
was supplied by Research Project BTE 2003-07867-
C02-01 from the Ministerio EspanÄol de Ciencia y
TecnologõÂa and the Research Group RNM-0179 of the
Junta de AndalucõÂa. The stay of M. Do Campo at the
a b University of Granada was supported by a UNESCO
fellowship awarded in 2000. The authors also thank
D.R. Peacor for his constructive review of the paper.
 Mixed-layer muscovite-chlorite 331
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