Mineralogical Magazine, August 2006, Vol. 70(4), pp.

347±355

Kamphaugite-(Y) from La Cabrera massif, Spain:

a low-temperature hydrothermal Y- REE carbonate

J. GONZAÂLEZ DEL TAÂNAGO1,*, A. LA IGLESIA1 AND A. DELGADO2

1 Departmentamento de PetrologõÂa y GeoquõÂmica and Instituto de GeologõÂa EconoÂmica CSIC, Facultad de Ciencias
Geolo
 gicas, Universidad Complutense, 28040 Madrid, Spain
2 Departmentamento de Ciencias de la Tierra y QuõÂmica Ambiental, EstacioÂn Experimental del ZaidõÂn, CSIC, 18008
Granada, Spain

ABS TR AC T

Kamphaugite-(Y) occurs as white to cream-coloured spherical to semi-spherical aggregates of radial

crystals in the La Cabrera granitic pluton (Spanish Central System). It mainly occurs on the free
surfaces of alkali feldspar, quartz, calcite, kainosite-(Y) and laumontite, and inside miarolitic cavities.
La Cabrera kamphaugite-(Y) has13 an average composition of Ca 0.94Y0.89 0.21(CO3)2
[F0.05(OH)0.95]´1.19H2O. Negative d CV-PDB values (ÿ14 to ÿ15%) indicate a meteoric carbon
REE

source. Textural relations between kamphaugite-(Y) and coexisting minerals, its relatively high d18OV-
SMOW values (+25 to +26%), and the occurrence of laumontite inclusions in kamphaugite-(Y), point to
a genesis at <50ëC during very low-temperature post-magmatic hydrothermal activity.

K EY WORDS : kamphaugite-(Y), stable isotopes, Spanish Central System.

of the above studies investigated the conditions of

Introduction

K AM PHA UG IT E -(Y), ideally Ca(Y, ) REE formation of this mineral.

(CO3)2(OH)´1.5H2O, is a rare mineral ®rst
described by Raade and Brastad (1993) and its
crystal structure by Rùmming . (1993) for a
et al
sample from Hùrtekollen, Norway. Raade et al.
(1993) report kamphaugite-(Y) occurrences in
two Norwegian granitic pegmatites, occurring
either as an alteration product of kuliokite-(Y)
or as crystallized rosettes along cracks in quartz
and feldspar. Raade and Brastad (1993) suggest
that the unknown mineral UN-21 of the Evans
Lou granitic pegmatite, Canada (Hogarth, 1972),
is kamphaugite-(Y). This mineral was later
reported by Orlandi (1997) and Gamboni and
Gamboni (1998) as associated with stilbite in the
Maddalena Island granite, Italy, by Petersen .
et al
(2001) in the RoÈssing uranium mine granite,
Namibia, by Wallwork et . (2002) on
al
Geological setting
Kamphaugite-(Y) is scarce at La Cabrera and
so far it has only been found in miarolitic cavities
of pegmatitic bodies. It occurs as spherical to
semi-spherical aggregates of radial crystals up to
1.5 mm in diameter, grown over free surfaces of
K-feldspar, quartz, pyrite, clinochlore, calcite,
kainosite-(Y) and laumontite. This zeolite,
laumontite, has also been found as inclusions in
the outer zone of the kamphaugite-(Y) aggregates.
The aim of this paper is to investigate the
conditions of kamphaugite-(Y) formation at La
Cabrera granitic pluton. Presented here are
compositional data, and for the ®rst time, stable
isotopic analyses of kamphaugite-(Y).

decrespignyite-(Y) in the Paratoo copper The La Cabrera massif is located in the NW of

deposit, Australia, and by FeheÂr . (2003) on
et al
®ssures in the SzarvaskoÄ granite, Hungary. None
* E-mail: tanago@geo.ucm.es
DOI: 10.1180/0026461067040338
# 2006 The Mineralogical Society
Madrid Province, Spain. It is a late-Variscan
granitic pluton forming part of the Spanish
Central System (Bellido, 1979; Villaseca ,
et al.
1993; Villaseca and Herreros, 2000).
Geochemically, the massif shows I-type char-
acteristics and an evolutionary trend from
 Â LEZ DEL TA
J. GONZA
marginal amphibole-bearing granodiorites
towards a dominant biotite monzogranite and
leucogranites. In the most evolved rocks, there are
occasional occurrences of garnet, cordierite and
muscovite (Bellido, 1979). Rare elements,
lithium-yttrium-¯uorine-type granitic pegmatites
(after the classi®cation of CÏernyÂ, 1991) with
gadolinite-(Y) occur in the most differentiated
granites (GonzaÂlez del TaÂnago et al., 1986;
GonzaÂlez del TaÂnago, 1997). Remarkable post-
magmatic hydrothermal activity is recorded
throughout the Eastern Spanish Central System,
with several main events (Caballero ., 1992;
et al
Tornos et al . 2000). The hydrothermal activity
(ascending hydrothermal solutions and downward
percolating groundwater) is recorded in the La
Cabrera granitic pluton by a medium-to-low
temperature overprint, that through a compact
microfault system as well as several major faults,
affects all of the pluton (GonzaÂlez Laguna , et al.
2000; Lozano, 2003). One of the most important
affects of this overprint is the Na/Ca ratio increase
of plagioclase which raised the calcium activity in
the hydrothermal ¯uids. As a consequence,
epidote, allanite-(Ce), ferro-axinite, prehnite and
a large range of secondary minerals formed.
These secondary minerals are mainly low-temp-
erature calcium silicates and carbonates such as
titanite, zeolites, ¯uorapophyllite, kainosite-(Y)
and bavenite. Many miarolitic cavities in
pegmatites, where the hydrothermal ¯uids were
concentrated, contain important secondary
minerals (GonzaÂlez del TaÂnago, 1997; GonzaÂlez
del TaÂnago and La Iglesia, 1998; Lozano, 2003).
The most abundant magmatic high-Y mineral
in the La Cabrera pluton is zircon. Crystal rims
may have up to 2.22 wt.% of Y2O3 and,
occasionally, some pegmatite zircons have up to
7.39 wt.% (Perez Soba . 2003), among the
et al
highest Y2O3 wt.% content reported (Hoskin and
Schaltegger, 2003). Xenotime-(Y), and monazite-
(Ce) up to 4.34 wt.% of Y2O3, are less abundant.
In the garnet-bearing rocks and pegmatite bodies,
the most abundant Y-bearing minerals are garnet,
which contains up to 2 wt.% Y 2O 3 , and
gadolinite-(Y) (GonzaÂlez del TaÂnago, 1997).
Methodology
X-ray powder diffraction (XRD) patterns were
obtained using a Philips X'PERT diffractometer.
Silicon powder was added to the analysis as a
standard. Due to the small amount of
kamphaugite-(Y) sample available (10 mg), a
 NAGO ET AL.
low-background oriented silicon crystal was
used as the sample holder. Unit-cell parameters
were re®ned by a least-squares method.
Differential thermal analysis (DTA) and gravi-
metric analysis (TG) were simultaneously carried
out with a Seiko Exstar 6000 instrument, using
~6 mg of sample, staticÿ1air atmosphere and a
heating rate of 10ëC min .
Semi-spherical aggregates of kamphaugite-(Y)
were mounted in epoxy and polished.
Wavelength-dispersive electron microprobe
(EPM analysis) data were collected using a
JEOL JXA-8900M instrument at the
Universidad Complutense, Madrid with the
following operating conditions: acceleration
voltage ÿ 20 kV, probe current ÿ 50 nA, and
peak counting times between 10 and 30 s and
background counting time of 5 to 15 s. The beam
diameter was 2ÿ5 mm to minimize sample
damage under the beam. The standards used
were albite, kaersutite, and REE -phosphates
described by Jarosewich et al . (1980) and
Jarosewich and Boatner (1991). For Th and U,
commercial glasses were used. An on-line ZAF
correction program was used for data correction
and reduction. Using the same standards, the
REE
overlaps were checked. To minimize the over-
estimation of Gd, Er and Lu (<5 wt.% as Gd2O3,
Er2O3 and Lu2O3) a peak and background overlap
JEOL correction program was used. Identi®cation
of mineral phases (¯uorapophyllite, tveitite-(Y),
bastnaÈsite-(Y), etc.), including kamphaugite-(Y)
was done by XRD and/or EMP analysis.
CO2 determination as well as isotopic analyses
were carried out at the Stable Isotope Laboratory
of EstacioÂn Experimental de El ZaidõÂn (CSIC),
Granada, Spain. CO2 was obtained from carbo-
nate using 100% phosphoric acid for 12 h in a
thermostatic bath at 25ëC (McCrea, 1950).
Isotopic ratios were measured in a Finnigan
MAT 251 mass spectrometer. The standard
reference materials NBS-18 and NBS-19 were
measured concurrently and yielded13 experimental
errors of <Ô0.1% (1s) for d C and d18O
determinations. In order to calculate the VSMOW
values, the acid fractionation factor used for
calcite and kamphaugite-(Y) was 1.01044 at 25ëC
(Kim and O'Neil, 1997).
Results
From the XRD patterns, and considering a
tetragonal symmetry, the following unit-cell
parameters have been calculated for the La
348
 KAMPHAUGITE-(Y) FROM SPAIN

Cabrera kamphugite-(Y): = 7.449(4) AÊ, = most signi®cant compositional variations are in

21.793(4) AÊ3, RW factor 0.00151, and =
a c
1209.3(0) AÊ . These data are in excellent agree-
V REE
ment with the parameters of Raade and Brastad
(1993), Rùmming . (1993) and FeheÂr .
et al et al
(2003).
The differential thermal analysis (DTA) curve
for kamphaugite-(Y) shows three endothermic
effects at 342, 430 and 754ëC (Fig. 1). The ®rst, a
very small effect, is ascribed to dehydration and
the second and third one to dehydroxylation and
decomposition reactions. The thermogravimetric
(TG) curve shows four steps at temperature
intervals of 80ÿ380, 400ÿ450, 450ÿ600 and
600ÿ780ëC with weight losses of 4.0, 12.4, 10.8
and 12.6%, respectively. The ®rst step, with a
weight loss at a very low rate, may correspond to
the existence of interstitial water. The following
steps correspond to OH and CO2 loss through
reactions probably involving metastable forma-
tion of CaCO3 and ®nal decomposition to CaO at
750ëC in a process similar to the dolomite
decomposition (Wiedemann and Bayer, 1987).
Moreover, the TG cooling curve shows a weight
increase of 1.2% in the temperature interval of
450ÿ400ëC which may correspond to CO2
absorption and carbonation of CaO.
the , Ca and Y contents. Analyses in the
various zones show that Y and Yb have a positive
covariance. On the contrary, negative correlations
exist between these elements and the other REE
as well as Ca. Thus, it seems that the main
substitutions in kamphaugite-(Y) are: Yÿ1 1 REE
and Caÿ3 2 (as shown in Fig. 3) which would
REE
explain the Ca cation de®ciency in this mineral.
The Th and U contents are highly variable, though
always low. We suggest that the actinide elements
enter into the kamphaugite-(Y) structure by
means of substitutions such as: Caÿ2(U, Th)1.
The chondrite-normalized REE pattern for
kamphaugite-(Y) is shown in Fig. 4. For compar-
ison, three other analyses are shown for
kamphaugite-(Y) from other localities. The
patterns show enrichment in the heavy . REE
Kamphaugite-(Y) and calcite from the La
Cabrera granitic pluton have negative d13CV-PDB
values ranging from ÿ14.16 to ÿ15.26%18 and from
ÿ18.45 to ÿ11.40%, respectively. d OV-SMOW
values in kamphaugite-(Y) are +24.82 to +25.91%
and for calcite, +19.3 to +23.2% (Fig. 5).
Discussion

The La Cabrera kamphaugite-(Y) EPMA The scarcity of kamphaugite-(Y) occurrences is

results and cation proportions, calculated on the responsible for the scarcity of studies on its
basis of 2.5 oxygens, are given in Table 1. The formation conditions. None of the existing
structural formula was calculated using EPMA
data and values for CO2 (volumetric determina-
tion) and H2O (TG measurement). The following
structural formula was calculated on the basis of 7
o x yg e n s: C a 0 . 9 4 Y 0 . 8 9
REE 0.21(CO3)2
[F0.05(OH)0.95]´1.19H2O. The 1.19 H2O per
formula unit (p.f.u.) is in agreement with the
results of FeheÂr . (2003).
et al
The kamphaugite-(Y) spherical aggregates
display concentric banding (Fig. 2). The bound-
aries between zones are not always sharp and the

FIG. 2. BSE image of an equatorial radial section

aggregate of kamphaugite-(Y). The brighter zones are
FIG. 1. DTA and TG curves of the La Cabrera granitic richer in relative to Y. The width of the radial
section is 930 mm.
REE
pluton kamphaugite-(Y).
349
 Â LEZ DEL TA
J. GONZA Â NAGO ET AL.

TABLE 1. Electron microprobe data for kamphaugite-(Y) from the La Cabrera granitic pluton and other
localities.
La Cabrera Hùrtekollen RoÈssing SzarvaskoÄ
wt.% 1s (51) wt.% 1s (5) wt.% wt.%
SiO2 0.04 0.02 n.a. n.a. n.a.
P 2O 5 0.12 0.11 n.a. n.a. n.a.
CaO 17.80 1.06 18.40 0.2 15.11 20.07
Y 2O 3 33.80 2.61 30.50 0.3 27.12 29.72
La2O3 0.05 0.02 n.a. n.a. 0.10
Ce2O3 0.24 0.10 n.a. n.a. 0.93
Pr2O3 0.10 0.07 n.a. n.a. 0.33
Nd2O3 0.51 0.10 1.40 0.3 1.47 2.13
Sm2O3 0.55 0.24 0.80 0.3 2.03 1.55
Eu2O3 0.14 0.11 n.a. n.a. 0.53
Gd2O3 1.98 0.48 n.a. 3.57 3.26
Tb2O3 0.76 0.29 1.60 0.3 0.81 0.63
Dy2O3 3.91 0.93 n.a. 5.58 4.91
Ho2O3 0.64 0.19 2.20 0.4 1.27 0.99
Er2O3 2.24 0.55 1.20 0.1 2.59 2.74
Tm2O3 0.17 0.09 n.a. 0.37 0.50
Yb2O3 1.07 0.24 1.10 0.3 1.07 1.65
Lu2O3 0.70 0.17 n.a. n.a. 0.43
ThO2 0.14 0.10 n.a. n.a. n.a.
UO2 0.15 0.09 n.a. n.a. n.a.
F 0.29 0.10 n.a. 0.81 n.a.
Total 65.41 57.10 61.91 70.47
Total F:O 65.28 61.57
Si 0.01
Ca 0.90
P <0.01
Y 0.84
La <0.01
Ce <0.01
Pr <0.01
Nd 0.01
Sm 0.01
Eu <0.01
Gd 0.03
Tb 0.01
Dy 0.06
Ho 0.01
Er 0.03
Tm <0.01
Yb 0.02
Lu 0.01
Th <0.01
U <0.01
F 0.04
La Cabrera kamphugite-(Y) cation proportions calculated on the basis of 2.5 oxygens giving at total of 1.99 cations
(S = 0.20; and Y/S(Y+ ) = 0.81). Hùrtekollen: Raade and Brastad (1993); RoÈssing: Petersen . (2001);
REE et al
SzarvaskoÄ: FeheÂr (2003). Number of analyses for each calculated standard deviation is given in brackets.
REE

et al.
n.a. = not analysed.

350
 KAMPHAUGITE-(Y) FROM SPAIN

Yttrium2ÿ is mobilized in the ¯uids, possibly as

(CO3) and F complexes (MoÈller, 1989). The
occurrence of secondary ¯uorite, ¯uorapatite,
¯uorapophyllite and calcite, as well as with
tveitite-(Y) and bastnaÈsite-(Y) inclusions in
garnet, indicates elemental mobility during
hydrothermal activity. Other secondary Y-rich
minerals formed during the hydrothermal over-
print: kainosite-(Y), xenotime-(Y) and
thalenite-(Y). The former is the most common,
sometimes as a by-product of gadolinite-(Y)
alteration by carbonatation and Feÿ1Ca inter-
change. Thalenite-(Y) is rare. Nevertheless we
have shown that most of the yttrium is
incorporated into other medium- to low-temp-
erature minerals such as titanite (occasionally up
FIG. 3. Y3+ and Ca2+ 3+ substitutions for to 6.15 wt.% as Y2O3), allanite-(Ce) (occasionally
vs. REE
kamphaugite-(Y) from the La Cabrera granitic pluton. up to 11.36 wt.% Y2O3), epidote, and rare
The3+ 1.2312+ regression coef®cient from the straight line vigezzite. At lower temperatures, corresponding
(Y +Ca ) = 1.231( 3+) ®ts the value (Y3++Ca2+)/ with the cessation of zeolite cystallization,
( 3+) = 1.20 obtained
REE
considering a 2(Y3++Ca2+) = agardite-(Y) appears, forming as a result of
REE
5/3( 3+) coupled substitution. arsenopyrite oxidation (GonzaÂlez del TaÂnago
REE
and GonzaÂlez del TaÂnago, 2002).
Most of the Y entering kamphaugite-(Y) is
studies, other than that by Raade and Brastad possibly sourced from the alteration of
(1993), considered the source of the Y. gadolinite-(Y). Sometimes, bavenite is observed
Nevertheless, its occurrence and association to occur in association with kamphaugite-(Y).
suggests a low-temperature hydrothermal origin This indicates that gadolinite-(Y) was the Y and
(Raade and Brastad, 1993; Gamboni and Be source for both minerals, although so far we
Gamboni, 1998; Petersen . 2001; Wallwork
et al have found no direct textural evidence to support
et al. 2002). this inference.
In the La Cabrera granitic pluton, Y has been The textural relationship of kamphaugite-(Y)
removed from primary magmatic and pegmatitic with calcite, laumontite and other secondary
minerals by post-magamtic hydrothermal ¯uids. minerals, and the fact that it post-dates

FIG. 4. Chondrite-normalized REE patterns for kampahugite-(Y). Chondrite values from Taylor and McLennan
(1985).
351
 Â LEZ DEL TA
J. GONZA Â NAGO ET AL.

kainosite-(Y), suggests it is the last Y mineral to

FIG. 5. Isotopic composition of calcite and kamphaugi-
te-(Y) from the La Cabrera granitic pluton. Note that the
isotopic values plot close to the present (calculated)
Meteoric Calcite Line (MCL). The d18OV-SMOW value
(+24%) of the MCL was calculated using the equation
of Kim and O'Neil (1997) for the system 18calcite-water,
an average temperature of 9.5ëC and d OV-SMOW =
ÿ7.6% for groundwater of the Iberian Central System
(Plata, 1994; PeÂrez del Villar ., 1997).
et al
crystallize, after zeolite formation, and perhaps
contemporaneously with agardite-(Y).
Kamphaugite-(Y) displays very negative
d13CV-PDB values (ÿ14.16 and ÿ15.26%) close
to the calcite values (ÿ18.45 to ÿ11.40% V-
PDB; Fig. 5). For this reason, sources for this C
such as sea water, dissolution of primary
precipitated marine limestone, atmospheric CO2
and magmatic CO2 can be disregarded (Kyser,
1986). On the contrary, these values are typical of
carbonates precipitated from meteoric waters, in
which the main source of carbon is edaphic
(Talma and 13Netterberg, 1983; Cerling, 1991).
Although d CV-PDB values as negative as
ÿ18.45% are not common in this type of
carbonate (Cerling, 1991), they can be explained
considering that in slightly acidic soil-water,
typical of granitic rocks, the isotopic composition
of the dissolved inorganic carbon (DIC) has a
lower isotopic fractionation (4 or 5%) with
respect to edaphic CO2, whereas at pH >7.5 the
DIC is enriched at ~10% (Romaneck et al.,
1992). Additionally, in oxidizing environments,
subsurface biological activity associated with
sulphide decomposition by T. Ferrooxidans

FIG. 6. Temperature and d18OV-SMOW values of mineralizing waters. The curves represent the theoretical temperature
of formation of calcite and kamphaugite-(Y) in equilibrium with meteoric waters 18of different isotopic values.
Considering sur®cial temperatures (10ÿ20ëC) and the isotopic range of calcite (d O = +19.1 to +23.2% vs.
V-SMOW) it is possible to obtain the isotopic range for the equilibrium water. For comparison, the oxygen isotopic
range of present meteoric water (rainwater and groundwater) is given. The Kim and O'Neil (1997) and O'Neil . et al
(1969) equations were used to relate temperature with isotopic fractionation in the systems calcite-water and
strontianite (kamphaugite-Y)-water respectively. The dotted line represents the values of kamphaugite-(Y).
352
 KAMPHAUGITE-(Y) FROM SPAIN

generate d13C values of DIC close to those of editor, P.W.O. Hoskin, and referee, E.B.
organic mater (Melchiorre and Williams, 2001; Melchiorre, made interesting and helpful sugges-
Melchiorre and Enders, 2003; Boni , 2003).
et al. tions for the ®nal version.
Consequently, both pH and CO2 production by
soil microbes associated with weathering of
disseminated sulphides may have produced an References

isotopically light DIC responsible for the Bellido, F. (1979) Âgico y geoquõÂmico del
Estudio petrolo

precipitation of these minerals. Values similar to Ân de La Cabrera

Pluto . PhD thesis, Universidad de
those from the La Cabrera granitic pluton have Complutense, Madrid.
been reported by Reyes (1998) in fracture- Boni, M., Gilg, H.A. Aversa, G. and Balassone, G.
(2003) The `Calamine' of southwest Sardinia:
et al.
®lling carbonates in the El Berrocal granitic geology, mineralogy and stable isotope geochem-
pluton (also in the Spanish Central System), istry. , , 731ÿ748.
where the DIC of the present underground waters Economic Geology 98
Caballero, J.M., Casquet, C., Galindo, C., GonzaÂlez
have values between ÿ20.7 and ÿ17.4%. The Casado, J.M., Snelling, N. and Tornos, F. (1992)
present-day d13C values of DIC in La Cabrera Dating of hydrothermal events in the Sierra de
range between ÿ9.9% and ÿ21% (Lozano, Guadarrama, Iberian Hercynian Belt, Spain.
2003). Consequently isotopic values of associated , , 18ÿ22.
calcites and water corroborate this super®cial Geogaceta 11
Cerling, T.E. (1991) Carbon dioxide in the atmosphere:
origin for the carbon in kamphaugite-(Y). evidence from Cenozoic and Mesozoic paleosoils.
In order to estimate the formation temperature , , 377ÿ400.
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CÏernyÂ, P. (1991) Rare-element granitic pegmatites. Part
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equations for kamphaugite-(Y), the use of other
Geoscience Canada 18(2)
Fehe r, B., Skaka ll, S. and Nagy, G. (2003)
equations, such as those for calcite, strontianite, Kamphaugite-(Y), a rare hydrous Ca-Y-carbonate
malachite, azurite and smithsonite (O'Neil ., et al mineral from SzarvaskoÄ, BuÈkk Mountains, Hungary.
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1
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12
calcite and kamphaugite-(Y) isotopic values near 27ÿ28.
the calculated Meteoric Calcite Line (MCL) in GonzaÂlez del TaÂnago, J. (1997) Allanita-(Nd) y
Fig. 5, supports the inference of a low-temp- minerales de elementos raros en las pegmatitas de
erature origin. The slightly more positive d18O of La Cabrera, Madrid (Sistema Iberico Central).
kamphaugite-(Y) values can be related to an Âgica de Espan
Revista Sociedad Geolo Äa 10 , , 83ÿ105.
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las pegmatitas granõÂticas del plutoÂn de La Cabrera
Consequently, calcite and kamphaugite-(Y) (Sistema Central EspanÄol). , ,
formed at similar low-temperature conditions, 181ÿ190.
Âgicos 54
Estudios Geolo

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Acknowledgements

Electron microprobe analyses and BSE images electroÂnico de barrido (SEM + EDS).
were performed with the help of A. FernaÂndez
Boletin
Äola de MineralogõÂa 23 , , 135ÿ151.
Larios; J. FernaÂndez Suarez and C. InÄigo helped
Sociedad Espan
GonzaÂlez del TaÂnago, J. and GonzaÂlez del TaÂnago
with the English in the manuscript. Our thanks to Chanrai, J. (2002) Minerales y Minas de Madrid .
these people and to G. Raade for comments on an Comunidad de Madrid and Mundiprensa, Madrid,
early draft of the manuscript. Finally, associate Spain, 271 pp.
353
 Â LEZ DEL TA
J. GONZA Â NAGO ET AL.

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