Mineralogical Magazine, February 2017, Vol. 81(1), pp. 167–173

A multimethodic approach for the characterization ofmanganiceladonite, a new member of the celadonite family
from Cerchiara mine, Eastern Liguria, Italy
G. O. LEPORE1,*, L. BINDI1, F. DI BENEDETTO1, E. MUGNAIOLI2,3, C. VITI2, A. ZANETTI4, M. E. CIRIOTTI5 AND
P. BONAZZI1
1
2

3

4
5

Dipartimento di Scienze della Terra, Università degli Studi di Firenze, Via G. La Pira 4, I-50121, Firenze, Italy
Dipartimento di Scienze Fisiche, della Terra e dell’Ambiente, Università di Siena, Via Laterina 8, I-53100, Siena,
Italy
Center for Nanotechnology Innovation@NEST, Istituto Italiano di Tecnologia, Piazza San Silvestro 12, 56127, Pisa,
Italy
CNR, Istituto di Geoscienze e Georisorse, Università di Pavia, Via Ferrata 1, I-27100 Pavia, Italy
Associazione Micromineralogica Italiana, Via Gioconda 3, I-26100 Cremona, Italy[Received 1 December 2015; Accepted 31 January 2016; Associate Editor: Sergey Krivovichev]
ABSTR ACTIn the manganesiferous ores associated with the metacherts of the ophiolitic sequences at the Cerchiara mine,
Eastern Liguria (Italy), a new Mn-bearing mineral belonging to the mica group has been recently found andcharacterized. High resolution transmission electron microscopy and electron diffraction tomography studies
confirm that the mineral belongs to the mica group. Unit-cell parameters from the powder diffraction patternare: a = 5.149(1), b = 8.915(1), c = 10.304(1) Å, β = 102.03(1)°, space group C2 or C2/m. On the basis of theelectron paramagnetic resonance spectroscopic results, the Mn4+ content represents a very subordinate
fraction of the total Mn, the remaining occurring as Mn3+. The Raman spectrum clearly indicates the presenceof OH groups in the structure. Laser-ablation inductively-coupled-plasma mass-spectrometry measurements
assess the presence of considerable amounts of Li.
Assuming all Mn as Mn3+ and 22 negative charges, the empirical formula can be expressed as:3þ
(K0.83□0.17)(Mn3þ
1:14 Mg0.80Li0.20Fe0:02 )(Si3.89Al0.10)O10[(OH)1.92F0.08] with the sum of the octahedral
cations indicating a ‘transitional’ character between a di- and a tri-octahedral structure. This formula
corresponds ideally to the Mn3+ analogue of celadonite, thus expanding the range of solid solution in theceladonite family. The ideal end-member formula KMn3+MgSi4O10(OH)2 can be easily related to celadonite
by the homovalent substitution VIMn3+ → VIFe3+. The mineral and its name have been approved by theCommission on New Minerals, Nomenclature and Classification of the International Mineralogical
Association, (IMA 2015-052).
K E Y WO R D S : manganiceladonite, celadonite family, Cerchiara mine, Eastern Liguria, Italy.

Introduction
HIGH concentrations of Mn in the mica-groupminerals are quite rare, although several Mnbearing micas do actually exist. The Mn2+ → Fe2+

*E-mail: lepore@esrf.fr
https://doi.org/10.1180/minmag.2016.080.087© 2017 The Mineralogical Society

substitution relates shirozulite (Ishida et al., 2004)
to annite, as well as masutomilite (Harada et al.,1976) to ‘zinnwaldite’. Norrishite (Eggleton andAshley, 1989; Tyrna and Guggenheim, 1991) is atrioctahedral mica with the M2 site occupied
mainly by Mn3+ and M1 by Li. Hendricksite,
polylithionite and kinoshitalite have been reported
to bear significantly large amounts of Mn(Guggenheim et al., 1983; Boggs, 1992; Tracy

G. O. LEPORE ET AL.

and Beard, 2003, respectively). Montdorite (Robertand Maury, 1979) is an uncommon Mn-bearing,tetrasilicic transitional mica with Mn content up to∼0.7 atoms per formula unit (apfu). However, it israre for these minerals to reach the ideal endmember composition (Tischendorf et al., 2007).
Preliminary chemical analyses obtained by energydispersive spectrometry (EDS) of a micaceous
mineral found at the Cerchiara mine, Eastern
Liguria (Italy) (Fig. 1), showed a composition
suggesting a new Mn-rich member of the micagroup. The analyses indicated a very high Si, Mn
and Mg content, with rather high F and low Al andFe concentrations. Therefore, the mineral underinvestigation was considered interesting enough toproceed with additional examinations.
This paper describes the results of a chemical,
structural and spectroscopic study to define anddescribe this new mica, named manganiceladonite
from ‘celadonite’ and ‘mangani’, in allusion to thedominant Mn3+ trivalent octahedral cation instead of
Fe3+. The mineral and its name have been approvedby the Commission on New Minerals, Nomenclature
and Classification of the International Mineralogical
Association (IMA 2015-052). The holotype material
is deposited in the mineralogical collections of theMuseo di Storia Naturale, Università di Firenze(Italy), under catalogue number 3164/I.

(Cabella et al., 1993), caoxite (Basso et al., 1997),
cerchiaraite-(Mn) (Basso et al., 2000), cerchiaraite(Fe) (Kampf et al., 2013) and balestraite (Lepore
et al., 2015). According to Cabella et al. (1998), theore body of the Cerchiara mine consists of braunitewith minor quartz layers interbedded with hematiteand quartz bands originated at low-temperature
metamorphic conditions. The ore was produced by
precipitation from submarine hydrothermal vents andreworkedbyturbiditic
resedimentation.
Manganiceladonite is orange-brown in colour witha micaceous appearance and forms thin and extremely
elongated lamellae in radial aggregates associatedwith calcite, hematite and braunite. The lamellae areso elongated to resemble, at a glance, acicular crystals.
The mineral is transparent with silky lustre and perfect{001} cleavage. It is moderately pleochroic, fromorange to greenish yellow. Calculated density is
3.042 g/cm3 on the basis of the empirical formula andunit-cell dimensions determined from powder X-ray
diffraction data (see below).

Experimental details
Powder X-ray diffraction
Numerous attempts to perform single-crystal X-ray
analysis were unsuccessful. Therefore, several minutefragments were handpicked from the rock sample andcrushed under acetone. Given the paucity of material,
it was possible to retrieve only a small amount of
powder, which was not enough to allow for a sample
preparation suitable for preventing preferred orientation. The spectrum was measured over the range 8 <2θ <70° using a Bruker D8-Advance diffractometer

Occurrence and physical properties
Manganiceladonite was found in the metacherts of
the ophiolitic sequences at Cerchiara mine, Val di
Vara, Eastern Liguria, Italy (∼44°11′58″N;
9°42′1″E). Since then, studies of the Cerchiara ores
have led to the description of many new minerals:
mozartite (Basso et al., 1993), brewsterite-(Ba)TABLE 1. Observed and calculated d spacings.

FIG. 1. Manganiceladonite associated with calcite andbraunite (L. Ceccantini photo); field of view is 2 mm.

hkld(obs)d(calc)

I/I0

001
002
020
021
003
022
112
023
004
2 2 3044
1 5 4

10.06
5.03
4.482
4.091
3.359
3.328
3.034
2.686
2.517
2.015
1.679
1.439

10.078
5.039
4.458
4.077
3.359
3.339
3.045
2.683
2.519
2.011
1.669
1.445

100
8
6
4
60
49
19
6
6
15
5
6

168

MANGANICELADONITE, A NEW MEMBER OF THE CELADONITE FAMILY

with ‘Da Vinci’ design equipped with CuKα
radiation, θ-θ goniometer and a multichannel fast
detector. Background was removed by using standard
polynomials through the software Rex.Cell (Bortolotti
and Lonardelli, 2013). Determination of peak positions was carried out initially in Rex.Cell by means ofan automated filtering/second-derivative approachbased on the Savitzky–Golay method (Savitzky and
Golay, 1964) and then carefully checked for incorrectly added peaks. Resulting d spacings are shown in
Table 1.
Transmission electron microscopy

source, ultra-high resolution (UHR) pole pieces andan Oxford ISIS energy dispersive X-ray (EDX)
detector. Images (Fig. 2) and diffraction patterns
were recorded with an Olympus Tengra camera (14bit, 2048 × 2048 pixels) and analysed by ‘iTEM’software. The powdered sample was dispersed on a
Cu mesh. Electron diffraction tomographic (EDT)
data were acquired in a tilt range of ±25° using a
JEOL double tilt holder, with a SAED aperture of
20 μm (equivalent to an illuminated sample area of∼200 nm). Data analysis was performed using
ADT3D software (Kolb et al., 2011).
Chemical analyses

Transmission electron microscopy (TEM) was
performed with a JEOL 2010 microscope, working
at 200 kV and equipped with a LaB6 electron

FIG. 2. (a) Low magnification bright field TEM image ofmanganiceladonite forming nanosized thin lamellae; (b)high-resolution TEM image of a manganiceladonite
bundle viewed orthogonal to c*; (c) TEM image of thecrystal selected for the collection of tomographic electron
diffraction data. Reconstructed three-dimensional electron
diffraction volume viewed along a* (d ), b* (e) and c* ( f );in (d ) and ( f ) the projections of c* and a* on (100) and(001), respectively, are shown.

A crystal aggregate of about 200 μm × 80 μm × 80 μm
was embedded in epoxy and polished for electron
microprobe analysis. Electron microprobe analyses
were performed using a JEOL JXA-8600 instrument
in wavelength dispersion mode at 15 kV, 10 nA beam
current and 5 μm beam size. The following standards
were used: albite (SiKα), plagioclase (AlKα), bustamite (MnKα), olivine (MgKα), ilmenite (FeKα),
sanidine (KKα), fluorite (FKα).
Determination of Li content was carried out
on the same aggregate using laser-ablationinductively-coupled-plasma
mass-spectrometry(LA-ICP-MS). The laser probe consists of a
Q-switched Nd:YAG laser, model Quantel(Brilliant), whose fundamental emission in thenear-IR region (1064 nm) was converted into
266 nm wavelength using two harmonic generators. The spot diameter was in the range of 40–50
μm. The ablated material was analysed by using an
Elan DRC-e quadrupole mass spectrometer.
Helium was used as carrier gas and mixed with
Ar downstream of the ablation cell. Data reduction
was carried out using Glitter software (http://www.
glitter-gemoc.com). NIST SRM 610 was analysed
as an external standard, while the SiO2 was used as
an internal standard. Precision and accuracy wereassessed from repeated analyses of the BCR-2 g,
NIST SRM 612 and 610 standards and resulted inbetter than 3%. Full analytical details are reported
in Tiepolo et al. (2005) and Miller et al. (2007).
Chemical analyses of major elements are reported
in Table 2 (means and ranges in wt.% of oxides).
Electron paramagnetic resonance (EPR)
spectroscopy

169

Conventional continuous-wave (cw) EPR spectroscopy measurements were performed on loose sample
crystals, put into amorphous silica tubes. Data wereG. O. LEPORE ET AL.

TABLE 2. Chemical analyses (means and ranges, wt.% oxides).
Constituent

Mean

Range

SD

Probe standard

SiO2
Al2O3
Mn2O3
MgO
Fe2O3
K2O
Li2O*
F
Total
O≡F
Total
H2O†
Total

55.90
1.20
21.50
7.75
0.47
9.37
0.71
0.35
97.25
0.15
97.10
4.14
101.2454.34–56.84
0.37–2.66
17.77–26.46
5.56–9.10
0.24–0.72
8.48–9.85
0.61–0.78
0.25–0.52

0.40
0.05
0.06
0.20
0.06
0.10
0.25
0.04

albite (SiKα)
plagioclase (AlKα)bustamite (MnKα)olivine (MgKα)ilmenite (FeKα)sanidine (KKα)
NIST SRM 610
fluorite (FKα)

Cr, V, Ti and Cl were sought but were found to be below the detection limit (<0.01 wt.%).
*Measured by LA-ICP-MS. † Estimated H2O content.

collected at room temperature, by using a Bruker ER
200D-SRC spectrometer operating at X-Band(∼9.5 GHz) interfaced with DS/EPR software to a
PC for data acquisition and handling. Given theextremely small amount of material available for the
spectroscopic measurement, EPR spectra werecollected in the range 1000–6000 G integrating 30
repeated scans registered at a scan speed of 0.1953s
per gauss, for a total integrated counting time of
3.5 h. The EPR spectrum is shown in Fig. 3.

equipped with a motorized x-y stage and an
Olympus microscope. The back-scattered Raman
signal was collected with 50x objective and theRaman spectrum was obtained from a non-oriented
crystal (8 μm × 30 μm × 100 μm, approximately).
The 632.8 nm line of a He-Ne laser was used as
excitation; laser power was controlled with a seriesof density filters. The minimum lateral and depth
resolution were ∼2 and 5 μm, respectively. The
system was calibrated using the 520.6 cm–1 Raman
band of silicon before the experimental session.
Spectra were collected with multiple acquisitions (2to 6) with single counting times ranging between 20
and 180 s. The spectrum was recorded using the
LabSpec 5 program (HORIBA, Jobin Yvon,
France) from 150 to 4000 cm–1.

Raman spectroscopy
The Raman spectrum (Fig. 4) was obtained using a
micro/macro Jobin Yvon LabRam HRVIS,

Results and discussion

FIG. 3. Electron paramagnetic resonance spectrum of
manganiceladonite.

170

The powder X-ray diffraction pattern closely
resembles that of a mica (e.g. Odom, 1984). Low
magnification TEM images show that manganiceladonite preferentially crystallizes with an elongated platelet habit (Fig. 2a). High-resolution TEM(HRTEM) images reveal that crystals tend to fray inbended lamellae that can be as thin as 20 nm(Fig. 2b). This morphology explains the difficulties
in finding suitable crystals for single-crystal X-ray
analysis. Data from EDT were collected from thecrystal shown in Fig. 2c. The reconstructed threedimensional electron diffraction volume (Figs 2d–f )shows indeed a C lattice compatible with a mica

MANGANICELADONITE, A NEW MEMBER OF THE CELADONITE FAMILY

FIG. 4. Raman spectrum of manganiceladonite.

(cell parameters: a = 5.4(1) Å, b = 9.1(2) Å, c =9.8(2) Å, β = 101.5(10)°, V = 472 Å3). The patternis characterized by a strong diffuse scattering along
c*, indicating strong stacking disorder along thisdirection.
The choice of a criterion for formula calculation,
which in micas involves an arduous task requiring a
direct determination of the hydrogen content, is, inthis case, even more complicated due to thepresence of an elevated content of Mn, which
could be present at different valence states (+2, +3,+4). Manganese in micas is indeed reported
commonly as Mn2+ although it rarely occurs at
the trivalent state, such as in norrishite; in the caseof manganiceladonite, given the strongly oxidizing
conditions assessed at the Cerchiara mine (Lepore
et al., 2015 and references therein), even thepresence of Mn4+ has to be taken into account.
The analysis of the EPR spectrum excludes thepresence of Mn2+, which would produce acharacteristic six-fold feature due to hyperfine
splitting. The weak paramagnetic signal observed(Fig. 3) is then attributed to the presence of Mn4+. In
order to obtain an evaluation of the Mn4+
concentration, a sample of birnessite containing
62.67 Mn (wt.%) of which 62% is considered as
Mn4+ (Di Leo et al., 2012; 2013) was used as theexternal standard. The spectrum was acquired under
the same conditions (1000–6000 G range, 0.1953s
per gauss) in a single scan. Taking into account thatthe intensity of the peak relative to Mn4+, corrected
for the differences in acquisition time and sample
mass, is ∼34 times higher than the peak observed
for manganiceladonite, it was possible to obtain arough estimate of Mn4+ content (1.1 wt.%) in thislatter phase, which corresponds to ∼1.8 MnO2 (wt.%).
This value can be considered as upper estimated.
171

Nevertheless, given the impossibility to obtainan accurate quantification of the Mn3+/Mn4+ ratio,
for further calculations Mn was assumed to occur in
its trivalent state, which is undoubtedly theprevalent one. In addition, the Raman spectrum(Fig. 4), although subjected to high noise level,
exhibits a distinct peak in the OH stretching region(3738 cm–1), indicating the presence of OH groups
in the structure. In consideration of the fact that it isvery common for Li-rich micas to show a partial
occupancy of the M1 trans site, it would be
unfeasible to normalize the formula on the basis of
a fixed number of cations. Chemical data were thus
tentatively normalized assuming 22 and 23 negative charges to take into account for a fully andpartially hydrogenated O4 site, respectively. As thenormalization based on 23 negative charges leads
to an unsatisfactory excess of tetrahedral cations(Si = 4.07; Al = 0.10 apfu), we assumed thefollowing empirical formula, based on 22 negative
charges, as the most appropriate:3þðK0:83 A0:17 ÞðMn3þ
1:14 Mg0:80 Li0:20 Fe0:02 ÞS¼2:16
ðSi3:89 Al0:10 ÞS¼3:99 O10 ½ðOHÞ1:92 F0:08 :

Tetrahedral sites in manganiceladonite are almost
fully occupied by Si and octahedra are filled by
Mn3+ and Mg, with a sum close to the typical valueof a dioctahedral mica; Li has been attributed tothe octahedral sites, as it is reported commonly inthe literature (e.g. Brigatti et al., 2002). The
corresponding ideal end-member formula is thenKMn3+MgSi4O10(OH)2 which is related to celadonite by the homovalent substitution VIMn3+ → VIFe3+.
In accordance with this conclusion, d values
calculated from fitted peak positions in the X-ray
spectrum (Table 1) were used to refine the unit-cell

G. O. LEPORE ET AL.

parameters using the software UnitCell (Holland andRedfern, 1997), basing the assignment of hkl
reflection positions on the data from Zhukhlistov(2005) for celadonite-1M. The resulting monoclinic
cell is: a = 5.149(1), b = 8.915(1), c = 10.304(1) Å, β= 102.03(1)°. Measured and calculated d values arecompared in Table 1. In analogy with the ideal
crystal structure of mica and, specifically, with that ofceladonite, we can assume that the most likely spacegroups are C2 or C2/m, and the polytype 1M. The
small b value is consistent with that of a dioctahedral
mica, in agreement with chemical data.
The ‘transitional’ character of manganiceladonite is a common feature, especially for Libearing micas (e.g. Levinson, 1953; Černý et al.,
1995; Roda-Robles et al., 2006; Van Lichtervelde
et al. 2008; Martins et al., 2012). The experimental
work of Monier and Robert (1986) also showed
how the gap between dioctahedral and trioctahedral
micas reduces with a progressive increase in Li. Du
Bray (1994) and Foord et al. (1995) also suggested
that the intermediate occupancy of the octahedral
sheet could be indicative of a mixed-layer form,
involving both dioctahedral and trioctahedral
structures, and could be a sign of disequilibrium
crystallization. The sum of interlayer cations<0.90 apfu constitutes an unusual feature in the
mica-group chemistry; nonetheless, micas frommetamorphic environments commonly show interlayer sites not fully occupied (e.g. Brigatti et al.,2011); moreover the presence of a minor amount of
Li in the interlayer cavity can also be hypothesized(Robert et al., 1983; Mesto et al., 2006), but cannot
be verified in the absence of a structure refinement.
Acknowledgements
The manuscript benefited from the revisions of two
anonymous reviewers and the editorial handling ofSergey V. Krivovichev. The authors also thank
Massimo Batoni for providing the sample and Luca
Ceccantini for the photo of manganiceladonite. The
X-ray diffraction spectrum was measured at CRIST,
Centro di Cristallografia Strutturale, University of
Florence, Italy. EDT measurements were supported by
FIR2013-Exploring the Nanoworld. This work was
funded by “Progetto d’Ateneo 2013” to P. Bonazzi and
F. Di Benedetto.

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