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Spectroscopic and X-ray diffraction studies on fluid deposited rhombohedral

graphite from the Eastern Ghats Mobile Belt, India

Article  in  Current Science · June 2006

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G. Parthasarathy Sreedhar Bojja

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Spectroscopic and X-ray diffraction to characterize this variety of graphite. However, there
are no previous reports on the occurrence of epigenetic or
studies on fluid deposited rhombohedral graphite (typical of fluid-deposited graphite)
rhombohedral graphite from the from India. Here we report, the detailed spectroscopic, X-
Eastern Ghats Mobile Belt, India ray diffraction (XRD) and differential thermal analysis
(DTA) data on the fluid-deposited graphite from the
Eastern Ghats Mobile Belt (EGB), Andhra Pradesh, India.
G. Parthasarathy1,*, B. Sreedhar2 and The EGB, a Precambrian high-grade granulite belt, occurs
T. R. K. Chetty1 along the east coast of India (Figure 1) and plays a crucial
1
National Geophysical Research Institute, Hyderabad 500 007, India role in the reconstruction of East Gondwana. The EGB
2
Indian Institute of Chemical Technology, Hyderabad 500 007, India consists of an intensely deformed and metamorphosed as-
semblage of both metasedimentry and metaigneous granulite
We report here the first experimental results on the facies rocks, which were subsequently intruded by Pro-
laser Raman spectroscopic, powder X-ray diffraction terozoic anorthosite and alkaline and granitoids rocks.
(XRD) and X-ray photoemission spectroscopic and
The metasedimentary rocks mainly include garnet-sillimanite
high-temperature differential thermal analysis studies
on graphite from the Burugubanda–Tapasikonda shear gneiss (khondalite), quartzites and calc-granulites, while
zone in the Proterozoic Eastern Ghats Mobile Belt the metaigneous rocks range from basic to felsic in compo-
(EGB) of Andhra Pradesh, India. Crystallinity, inter- sition and are essentially hypersthene-bearing (charnockites).
planar spacing and unit-cell parameters were deter- Geology, structure and geochemistry and Gondwanian
mined by powder XRD. Powder XRD studies on the correlations are extensively discussed in several recent
graphite samples from the shear zone show all the reviews4–8. The peak metamorphic pressure and temperature
strong XRD peaks corresponding to syngenetic (hex- conditions have been calculated9 based on the mineral as-
agonal) graphite and additional peaks at 0.208 and semblages in calc-silicate rocks from Vizianagaram area
0.197 nm corresponding to the presence of epigenetic of the EGB as P = 6.5 kbar and T = 730°C. However, no
(rhombohedral) polytype of graphite. On the basis of such geothermobarometric calculations are reported from
the intensity ratio of the (101) diffraction peaks for
the study area.
both syngenetic and epigenetic phases, the content of
epigenetic phases within this sample is estimated to be
up to 20–25%. The presence of epigenetic phase indi-
cates that the Burugubanda shear zone contains fluid-
deposited graphite, a solid carbon from natural carbon-
bearing fluids such as those containing CO2, CO and
CH4. The fluid-deposited nature of the graphite has
also been confirmed independently by X-ray photo-
electron spectroscopic studies. Laser Raman spectro-
scopic studies on all the samples show Raman bands
at 1581 to 1585 cm–1 (ordered peak), 1351 to 1355 cm–1
(disordered peak) and second order peak at 2724 cm–1.
The intensity ratio of ordered to disordered peaks
(0.09 to 0.10) indicates the peak metamorphic tem-
perature of the host rocks corresponding to sillimanite
zone. The values of interplanar spacing d002 (0.3346
nm), crystallite size (or stacking height; 54.83 nm) and
degree of graphitization (135.5) indicated the peak
metamorphic temperature of the host rock to be about
750 ± 30°°C, and hence the high temperature that pre-
vailed along the EGB shear zone.

Keywords: Eastern Ghats, graphite, precambrian, spec-

troscopic studies, shear zones.

GRAPHITE is common in a variety of rocks metamor-

phosed under a range of pressure–temperature conditions
and has proved to be a valuable indicator of fluid move-
ments1–3. Luque et al.3 have reviewed the world-wide occur-
rences of fluid-deposited graphite and various methodologies
Figure 1. Geological map of Burugubanda–Tapasikonda area on 1 :
*For correspondence. (e-mail: [email protected]) 50,000 scale.

CURRENT SCIENCE, VOL. 90, NO. 7, 10 APRIL 2006 995

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Three different batches of graphite samples of the present less than 5%. The DTA/TG apparatus was calibrated
study were collected from the tungsten bearing Buru- against alumina and melting temperature of In as standards.
gubanda–Tapasikonda shear zone, East Godavari district, Laser Raman spectroscopic studies were carried out at
Andhra Pradesh, south central part of EGB. Although, room temperature using 488 nm line of argon-ion laser
graphite is ubiquitous in khondalite rocks, the graphite with a low power of less than 10 mW in the sample (to
deposit at Burugubanda occurs at the sheared contact avoid any laser-induced heating effect, which could cause
zone between two major rock suites, i.e. khondalites and a shift in Raman peak)10. Triplicate runs were made in
charnockites. At Burugubanda there are two graphite-bearing static air atmosphere. Uncertainty in the observed value
bodies trending E–W, which are separated by 140 m. The of wavenumber is typically 2 cm–1 in the frequency range
eastern graphite body extends for about 250 m and its 2000–3000 cm–1.
14 m. The western body has a strike length of 320 m and Figure 2 shows the powder XRD pattern of graphite
ranges in width from 2 to 13 m. Graphite is associated samples from Burugubanda (EGB) as well as pure well-
with quartz-rich pegmatite veins that range in width from crystallized synthetic graphite. The well-crystallized graph-
10 to 60 cm. These quartz migmatitic veins are vertical ite exhibits four XRD peaks, all of which were indexed to
and sub-parallel to the foliation planes in the host graphite a hexagonal unit cell. The values of the d-spacing of the
gneiss. Tungsten is also commonly associated with peg- well-crystallized graphite are found to be in excellent
matite bodies. Foliations in migmatitic graphite gneisses agreement with the published XRD data on pure graphite
trend E–W and dip sub-vertical to vertical, but distinctly (ICPD card nos 13–148). However, samples from the Bu-
southwards. Field evidence within the graphite-bearing rugubanda shear zone show distinctly different XRD pat-
gneisses indicates that there have been movements result- tern with additional peaks, compared to highly ordered
ing in slickensides, and the rocks have been subjected to graphite. The additional peaks near 0.2075 and 0.1972 nm
intense shearing. are indexed to a rhombohedral phase of graphite, corre-
The graphite samples were characterized by powder X- sponding to (101) and (012) reflections. This phase is
ray diffraction (XRD), Laser Raman spectroscopic, dif- known to be the thermodynamically unstable allotropic
ferential thermal analysis (DTA) and thermogravimetric form of graphite with an ABCABC stacking sequence of
(TG) analyses. The diffraction patterns were obtained us- the layers. The exact crystallographic description of this
ing Philips Diffractometer and also Siemens D-5000 allotropic form is given by the space group D3d5-R3m,
Powder Diffractometer with HOPG graphite monochromator. (unit cell constants: a = 0.2566 nm and c = 1.0062 nm).
Cu-Kα radiation with a wavelength 0.15419 nm was used The structure of this phase can be considered as an ex-
in all the diffraction experiments. Differential thermal tended stacking fault in thermodynamically stable hex-
analysis and thermogravimetric studies were performed agonal graphite (IUPAC, 1997). It is well known that
on four different sets of powdered samples of about rhombohedral graphite cannot be isolated in pure form. It
15 mg using a Mettler Toledo Star System apparatus. The has been observed that this rhombohedral phase is also
analyses were performed in the temperature range be- produced by shear deformation of hexagonal graphite and
tween 300 and 900 K at a heating rate of 10 K/min. Ana- transforms progressively to the hexagonal ABABABB
lytical error in the measured values of temperatures is stacking sequence on heating above 1600 K (IUPAC

Figure 2. Powder X-ray diffraction pattern of syngenetic graphite (lower spectra) and fluid-deposited graphite from Burugu-
banda–Tapasikonda shear zone, Eastern Ghat Belt (EGB) (upper spectra). H, Hexagonal graphite and R, Rhombohedral phase.

996 CURRENT SCIENCE, VOL. 90, NO. 7, 10 APRIL 2006

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Figure 3. First-order laser Raman spectrum of fluid-deposited graphite from EGB. The ordered (O) peak is at 1582 cm–1 and the
disordered (D) peak at 1353 cm–1. The ratio of D/O is 0.10, indicating sillimanite zone of peak metamorphism (For details see text.)

Compendium of Chemical Technology, 1997, 2nd edn, pp. 1000}] × 100. This relation has been successfully applied
67, 504). The content of the rhombohedral phase within in determining the structural parameters of natural graph-
the Burugubanda sample has been estimated as 20 to 25% ite from different geological settings throughout the
(Figure 2), using the intensity ratios of the (101) diffrac- world15–23. The values of d(002) and β(002) obtained for
tion peaks for both hexagonal and rhombohedral phase. the EGB graphite are 0.3346 (4) and 0.0145 (5) nm res-
Kwiecinska11 has proposed that the relative amount of the pectively. The value of the interplanar crystallite size esti-
rhombohedral phase can also be evaluated by the intensity mated using the above relations is 54.83 ± 5.0 nm, and
ratio between the (101) and (012) peaks of rhombohedral GD is found to be 135.5 ± 5.0. Wada et al.15 have analysed
phase and the intensity of the (002) and (004) reflections several samples of carbonaceous matter extracted from
of the hexagonal phase. Luque et al.3 have observed that limestone and pelitic rocks of Ryoke metamorphic terrain,
the content of the rhombohedral phase decreases as the tem- and derived a simple linear correlation between GD and
perature (metamorphic grade) increases. Typically, about peak metamorphic temperature. The relation is T (in °C) =
20–30% of rhombohedral phase is observed in many 3.2 × GD (in Å) + 280. Substituting the values of GD =
fluid-deposited graphite mineralizations of Borrowdale, 135.5 for the Burugubanda graphite, we obtain the peak
and Huelma in the Betic Cordillera3,11. In the Buru- metamorphic temperature as 713.6°C. The values of crys-
gubanda samples, the content of the fluid-deposited tallite size and GD of Burugubanda graphite in combina-
graphite has been found to be about 20 to 25%, which is tion with the graphite formation curve as a function of the
found to be in good agreement with the values obtained metamorphic facies, yield a peak metamorphic tempera-
for the fluid-deposited graphite in Betic Cordillera, southern ture of 700 ± 20°C for the Burugubanda–Tapasikonda
Spain12 and graphite in KTB (German Continental Deep graphite and tungsten mineralization shear zone, indicat-
Drilling) core samples13. The amount of rhombohedral ing the high temperature of the shear zone.
graphite from fluid-deposited graphite in the Sri Lankan The Raman spectrum of carbonaceous matter is generally
granulite facies metasedimentry rocks is found to vary3 composed of first-order (1100–1800 cm–1) and second-
from as low as 3% to 21%. The value of interplanar spacing order (2500–3100 cm–1) regions. Figure 3 shows the first-
d(002) for the EGB syngenetic graphite is found to be order Raman spectrum of graphite from EGB at room
0.3346 ± 0.0003 nm. The crystallite size and degree of temperature. The strong peak at 1582 cm–1, the Raman
graphitization have been calculated by measuring the full (O) peak corresponds to the E2g vibration mode of a crystal
width half maximum of the (002) peak. The size of the with D6h4 symmetry, i.e. to in-plane vibration of aromatic
crystallites LC (002) has been calculated using Scherrer’s carbons in the graphitic structure. The Raman band at
equation, LC = Kλ/β(002) cos θ, where the constant K is 1353 cm–1 is less intense and wide, which corresponds to
usually assumed14 to be 0.9; β(002) is the value of full the vibrations of disordered carbons (called D peak). Dur-
width of Bragg (002) peak at half height in radians; λ is ing the graphitization process, its relative area decreases
the wavelength in angstrom (10 angstrom = 1 nm) and θ with the stiffening of aromatic planes. Consequently, this
is the angle of diffraction in radians. The graphitization band is attributed to in-plane defects like heteroatoms (O,
degree (GD) has been calculated using the relation sug- H, N for instance). Figure 4 shows the Raman spectra of
gested by Wada et al.15: GD = [{d(002)–3.7}/log {LC/ fluid-deposited graphite from EGB and pure graphite
CURRENT SCIENCE, VOL. 90, NO. 7, 10 APRIL 2006 997
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Figure 4. Laser Raman spectra of fluid-deposited graphite (EGB) (upper spectrum), and pure inorganic graphite (lower spec-
trum), including wavenumber regions of second-order Raman spectra.

(lower spectrum in Figure 4). The studied graphite shows deposited graphite. Broadening of the graphite Raman (O)
a strong disordered peak at 1353 cm–1, which is absent in band (~30 cm–1 in Burugubanda compared to 15 cm–1 for
pure graphite. The ratio of the intensity of the D peak a synthetic graphite) is due to the probable bending of the
with respect to O peak (D/O) is measured as 0.10 ± 0.01, graphite sheets in fluid-deposited graphite (Figure 4). Our
yielding the crystallite size along the intraplanar graphite observation of fluid-deposited graphite with high-
structure (La) as 34.0 ± 0.5 nm. The ratio of D/O is found temperature grade is in accordance with the reported presence
to vary from 0.09 to 0.14 for typical sillimanite grade of high-density CO2-fluids in spinel bearing high Mg–Al
metapelites1,19,22,23. The data in combination with the cor- granulites in the Vizianagaram area of the EGB and the
relation between the (D/O) and La show that the peak ultra high-temperature metamorphism of the EGB26.
metamorphic grade of the host rock is in the sillimanite X-ray photoelectron spectroscopic studies on Buru-
zone and the samples are well-crystallized graphite. The gubanda graphite samples show several peaks corres-
value of the ratio of the second-order Raman peak to the first- ponding to C–O (at 286.9 eV) and O=C–O bonding (at
order peak (S/O) is determined as 0.33 ± 0.02 for fluid- 289.0 eV), in addition to the C–C (285.2 eV) bonding
deposited graphite. The studied graphite shows some ad- present in syngenetic graphite (284.2 eV; Figure 5),
ditional weak peaks at 2457, 2946 and 3241 cm–1. In the thereby supporting the nature of fluid-deposited graphite
second-order region, graphite shows a peak at about in the shear zone. Our observations are supported by a re-
2700 cm–1, which splits into two components at 2686 and cent report by Panigrahi et al.27, who have carried out mi-
2725 cm–1 during the final stage of the graphitization cro-Raman studies on migmatites of the EGB around
process. This splitting has been interpreted as a result of Angul and confirmed the presence of carbonic inclusions
the transition between the two-dimensional structures towards with densities as high as 1.172, and presence of high
the three-dimensional one25. The second-order Raman amounts of methane as fluid inclusions. It is possible that
spectrum of the fluid-deposited graphite includes peaks fluid-deposited graphite is formed by precipitation from
near 2450 cm–1 (S1 peak), 2735 cm–1 (S2 peak), 2950 cm–1 C–H–O fluids trapped in the shear zone, under conditions
(S3 peak) and 3248 cm–1 (S4 peak), which can all be as- near those of peak metamorphism at the host rock through
signed to overtone scattering or combination scattering. the reaction CO2 + CH4 → 2C + 2H2O. The XPS spectrum
The Raman peak at 2946 cm–1 observed for the fluid de- of the metamorphic graphite from East Antarctica, whose
posited graphite from Burugubanda shear zone (Figure 4) peak metamorphic temperature is 700°C is also shown in
may be attributed either to the C–H stretching vibration Figure 5 for comparison. Metamorphic graphite does not
in impure carbonaceous matter or to the theoretically pre- show any peak corresponding to C–O or O=C–O bonds,
dicted disorder-induced band at 2950 cm–1. However, it is clearly demonstrating the presence of fluid-deposited
observed that the peak at 2940 cm–1 becomes more intense graphite in the Burugubanda shear zone of EGB.
with decrease in crystallite size. Therefore, observation of the Figure 6 shows representative DTA and TG traces for
2946 cm–1 peak in the EGB graphite represents the pres- the Burugubanda graphite samples. The sample exhibits a
ence of C–H vibration and hence the nature of the fluid- strong exothermic peak at around 973 K and a weak exo-

998 CURRENT SCIENCE, VOL. 90, NO. 7, 10 APRIL 2006

 RESEARCH COMMUNICATIONS

thermic peak at about 1073 K. The former peak is attributed TG data also show the presence of two weight losses at
to the combustion of carbonaceous matter under atmos- 970 and 1075 K, which are characteristics of typical car-
pheric condition. The latter peak is either due to the com- bonaceous matter precipitated from fluids such as CH4,
bustion of rhombohedral graphite present in the sample or CO2, etc. The DTA peak temperature 700–800°C also indi-
to the detrital fully crystalline graphite, which was admixed cates the range of peak metamorphic temperature. In the
with natural carbonaceous fluids during sedimentation15. case of metamorphic graphite, the DTA peak increases
linearly with decrease in d(002) values. However, fluid-
deposited graphite samples show lower DTA tempera-
tures than those of metamorphic graphite samples, for the
given d(002) value. Moreover, for natural fluid-deposited
graphite, the DTA maximum temperature is found to be
invariant with the change in d(002) spacings3. Hence we
did not attempt to plot our data in Kwiecinska’s plot11.
About eighteen occurrences of fluid-deposited graphite
have been reported so far throughout the world3,12,13.
However, the presence of rhombohedral graphite has been re-
ported only from three places, viz. Sri Lanka (up to 21%),
Spain (up to 25%) and Borrowdale, England (up to 31.9%)3.
Barrenechea et al.12 have proposed the cooling of C–O–H
fluid as the likely mechanism for precipitation of fluid-
deposited graphite, although hydration reactions might
have played a role in the volcanic rock-hosted graphite
mineralization. Kwiecinska11 has reported the coexistence
of highly crystalline hexagonal graphite and significant
proportion of rhombohedral graphite (31.9%) in the vol-
canic rock-hosted graphite deposit at Borrowdale. The
present study reports the occurrence of rhombohedral
graphite (up to 25%) from India. Pasteris and Chou13
have reported the presence of fluid-deposited graphite in-
Figure 5. XPS spectra of fluid-deposited graphite from EGB and clusions in quartz collected from 3341 m depth of KTB
syngenetic graphite, East Antarctica (Graphite). Note the presence of borehole. Raman studies on the sample show D/O peak
fluid components like C–O, O=C–O bonds only in EGB graphite.
ratio as 0.21 yielding, La = 10 nm. They also suggested
that higher temperatures are required to produce ordered
graphite by fluid deposition than by metamorphism of organic
matter. Hence the peak metamorphic temperature estimated
by graphite geothermometer is underestimated while
dealing with the fluid-deposited graphite. It should be
noted here that no calculations have been made so far to
estimate the energy required to nucleate the ordered and
disordered graphite from a given C–O–H fluid28.
The study by Pasteris and Chou13 also showed that the
degree of crystallinity of fluid-deposited graphite is a
more complex function of temperature than that of the
metamorphic graphite, suggesting that the metamorphic
temperature derived from the crystallinity data on the
fluid-deposited graphite possibly gives the lower limit of
the peak metamorphic temperature. Hence the peak meta-
morphic temperature of the Burugubanda–Tapasikonda
sector of EGB should be more than 750°C, indicating a
high-temperature shear zone.
In summary, our experimental studies on the graphite
Figure 6. Differential thermal analysis (DTA) and thermogravimetric
(TG) traces for fluid-deposited graphite from the Burugubanda– sample from the Burugubanda–Tapasikonda shear zone
Tapasikonda shear zone, EGB. The strong exothermic peak at 973 K is of the EGB, India, reveal the presence of rhombohedral
due to graphite combustion indicating high degree of order, comparable graphite in the EGB, which is a characteristic of fluid-
to that observed in graphite from sillimanite zone terranes of East Ant-
arctica. The weak exothermic peak at 1073 K corresponds to combus- deposited graphite. The peak metamorphic temperature of
tion of detrital graphite. the host rock was estimated as 750 ± 30°C, which has
CURRENT SCIENCE, VOL. 90, NO. 7, 10 APRIL 2006 999
RESEARCH COMMUNICATIONS

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Prace Mineral., 1980, 67, 5–79. ACKNOWLEDGEMENTS. This paper is dedicated to Dr T. M. Ma-
12. Barrenechea, J. F., Luque, F. J., Rodas, M. and Pasteris, J. D., hadevan, Former Director, Atomic Mineral Division, Hyderabad on his
Vein-type graphite in Jurassic volcanic rocks of the external zone 80th birthday. We are grateful to Dr T. M. Mahadevan, Prof. Jill Pas-
of the Betic cordillera, South Spain. Can. Mineral., 1997, 35, teris, Washington University in St. Louis and Prof. Steven Haggerty,
1379–1390. Florida International University, USA for useful discussions to improve
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sions in quartz: Comparison between KTB (German Continental Chemical Technology, Hyderabad for providing analytical facilities to
Deep-Drilling) core samples and artificially reequilibrated natural characterize the samples. We also thank Dr V. P. Dimri, Director,
inclusions. Geochim. Cosmochim. Acta, 1998, 62, 109–122. NGRI, Hyderabad, for support and permission to publish this paper.
14. Tagiri, M. and Tsuboi, S., Mixed carbonaceous material in Meso- This work is partly funded by ISRO, Department of Space, Government
zoic shales and sandstones from the Yamizo mountain system, Ja- of India, under the PLANEX programme.
pan. J. Jpn. Assoc. Mineral. Petrol. Econ. Geol., 1979, 74, 47–56.
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phism with references to carbonate and pelitic rocks of contact and Received 10 November 2005; revised accepted 21 January 2006
regional metamorphisms, Japan. Contrib. Mineral. Petrol., 1994,
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