PROCEEDINGS, 6th ITB International Geothermal Workshop 2017
Institut Teknologi Bandung, Bandung, Indonesia, March 2223, 2017
STUDY OF ROCK MICROSTRUCTURE BASED ON SEM-EDX AND XRD
CHARACTERIZATION TO EVALUATE ARJUNO-WELIRANG GEOTHERMAL
POTENTIAL
Husnia Nur Annisa, Almira Mahsa, Silvia Veronica, Nuha Malihati, Karim Rahman Hartono
Geophysical Engineering, Institut Teknologi Sepuluh Nopember
Jl. Raya ITS, Keputih, Sukolilo, Keputih, Sukolilo, Kota SBY, East Java
e-mail: husnia.nia.annisa@gmail.com
ABSTRACT
The X-ray Diffractometer is used to qualitatively or
quantitatively identify individual minerals. While
SEM-EDX used for the surface analytical
techniques. Samples are selected from eleven
lithologic units around Arjuno-Welirang Volcanoes.
The purpose of this study is to determine how the
state morphology, crystal structure and the
percentage of the mineral content of the samples
using X- ray characterization Diffraction (XRD)
and Scanning Electron Microscope-Energy
Dispersive X-Ray Spectroscopy (SEM-EDX).
Arjuno-Welirang Geothermal prospect area is
situated in ring of fire Indonesia and located in
Kab. Mojokerto, Kab. Malang, Kab. Pasuruan and
Kota Batu, East Java. Geologically, the prospect
area is dominated by Quartenary volcanic rocks,
both lava and phyroclastic. The samples obtained
from Arjuno-Welirang Volcanoes by digging to a
depth of 1-1.5 m as many as eleven points. The
method used in this research is the method of
powder. Eleven samples were crushed and sifted in
the sieve of 200 mesh. Characterization of the
eleven samples were done with the technique of X-
Ray Diffraction (XRD) and Scanning Electron
Microscope- Energy Dispersive X-ray
Spectroscopy (SEM-EDX). Based on SEM-EDX
test, the morphology of the eleven samples is
generally shaped slab or blob defects and sizes.
While the result of XRD test, mineral contents in
the samples are dominated by Albite, Anorthite,
and Kyanite mineral that showed geothermal
potential.
Keywords: Geothermal, SEM-EDX, XRD
BACKGROUND
The Arjuno Welirang geothermal complex
is located in East Java, with stratovolcanoes Mt.
Arjuno (3,339 meters) and Mt. Welirang (3,156
meters) being the dominating landscape.
Coordinates-wise, it is located between latitudes
7037'56.00"-7049'51.00" and longitudes
112029'12.00" 112037'39.00". This geothermal
complex is indicated by the manifestations. The
manifestations are controlled by several factors,
especially geological structures and lithology.
Some examples of them are hot springs, fumarole,
and altered rocks which the mineralogy can explain
preceding hydrothermal processes. In this paper,
methods used geological observation, sampling,
and laboratory analysis. Geological features
observed morphology, lithology, geological
structures, and geothermal manifestation, hot
spring. Based on the observation, known outcrops
and hot springs will be mapped. After the
observation, the following method is rock
sampling. Sampled rocks are of those situated
around hot springs. These samples will be used for
laboratory analysis using SEM-EDX and X-Ray
Diffraction. The SEM-EDX method is utilized
particularly for fresh samples while X-Ray
Diffraction method is used only for weathered
samples.
The result of laboratory analysis will be used to
predict the reservoir temperature in the Arjuno
Welirang geothermal complex based on the
preceding alterations processes of sampled rocks.
The identification of hydrothermally altered rock-
forming minerals and rock mineralization from the
analysis can be used as information for
interpretations and further understanding of region-
related mineralization, especially its correlation
with formation temperature, fluids, cause of
alteration, and depositional environment of
minerals. Thus, the final result of this research can
be related with overall geothermal potential in
Arjuno-Welirang complex.
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 Figure 1: geology structure of MT. Arjuno Welirang (Tim Survei Geologi PSDG, 2010)
ARJUNO WELIRANG GEOLOGY
Arjuno Welirang is a mountain complex
comprising several mountains: Mt. Arjuno (3339
m), Mt Bakal (1960 m), Mt. Kembar (3156 m),
which are formed as a result of the southwest-west
movement of eruption point and controlled by a
fault which result in a formation of a gap that
permits magma flow onto the earths surface.
Besides, there are also several others, namely: Mt.
Ringgit (2477 m), Mt. Pundak (1544 m), and Mt.
Butak (1207 m), which are formed because of
lateral eruption. In addition, there are several faults
in Arjuno-Welirang complex. They are Padusan,
Claket, Bulak, Welirang, Kembar.
Atop Mt. Welirang, there are springs
which are parallel to Coban and Padusan Fault.
This indicates geothermal potential in vicinity.
According to conceptual model of Arjuno-Welirang
geothermal system, there are three point of fluid
outflow: Padusan, Cangar, and Coban (Daud et al,
2015). Fumarole is also visible on top of Mt.
Welirang. And then, altered rocks can be found at
Mt. Pundak (Bakrudin, 2016). Lava that produced
by Mt. Arjuno is made of olivine basalt and
pyroxene andesite, meanwhile, Mt. Welirang
produced hyperstein-augite andesite (Verbeek-
Fennema, 1896. Catalogue of the active volcanoes
of the World Including Solfatara Fields, Part 1).
Rocks that made up most of Arjuno-Welirang
complex are the results of three eruptions from Mt.
Arjuno Tua, Mt. Welirang Tua, dan Mt. Welirang in
the form of lava flow, pyroclastic flow. The
direction of the erupted products are mainly to the
north and west (Berita Berkala Vulkanologi, Edisi
Khusus, 1992, G. Arjuno -Welirang) (see fig. 1).
METHOD
Some factors which are responsible in the
formation of altered minerals are as follows:
Temperature, pressure, rock type, origin,
permeability, duration of hydrothermal exposure,
and composition of hydrothermal fluids (Browne
and Ellis, 1970).
A total of eleven samples are acquired from eleven
spots around Arjuno-Welirang as shown in figure 1.
These samples crushed into silt sized fractions.
Then, this fraction analyzed with Electron
Microscope energy Dispersive X-ray
Spectroscopy (SEM-EDX) to understand the
forming elements and morphology. After that, X-
ray Diffraction (XRD) applied to the crushed
samples to detect the minerals and hydrothermal
related altered minerals. SEM-EDX analysis was
done in Laboratorium Energi LPPM ITS,
2
meanwhile, the XRD analysis was done in minerals match those of XRD analysed samples.
Laboratorium Material dan Metalurgi ITS. The This matching procedure is done via Match!
result of SEM-EDX were used to determine which

3
 Table 1: Coordinate of Sample Location
No Rock Unit Sample Code Coordinate
Longitude Latitude

1 Produk Anjasmara QPA 11232'18.9" E 740'52.3" S

2 Lava Tua Arjuno Welirang LTAW 11238'59.71" E 742'31.09" S
3 Aliran Piroklastik Tua Arjuno Welirang QAPTAW 11234'47.8" E 740'12" S
QAPTAW+ 11237'44.5" E 740'24.3" S
4 Erupsi Samping QES 11234'7.7" E 740'48.5" S
5 Lava Welirang I QLWI 11232'55.3" E 741'4.3" S
6 Aliran Piroklastik Welirang I QAPWI 11234'30.7" E 740'26.6" S
7 Aliran Lava 1 G.Arjuno Al1 11239'36.15" E 746'24.4" S
8 Aliran Lava 2 G.Arjuno Al2 11240'7.5" E 747'19" S
9 Aliran Lava 3 G.Arjuno Al3 11241'55.5" E 745'3.6" S
10 Aliran Piroklastika 1 G.Arjuno Aap1 11239'44.7" E 749'18" S
11 Endapan Jatuhan Piroklastika 2 Ljp2 11240'21.3" E 748'47.9" S
G.Linting

Software. The result of matching process was identified with several other minerals which are indicators of
hydrothermal-alteration formation temperature.

Sampling
Eleven samples were taken from several parts of
Arjuno Welirang Complex (Table 1). These samples are considered to represent the condition of the whole
complex. Afterward undergo the coring process. Coring was done in order to get the fresh part of the samples
which is free from weathering, temperature, or pressure effects.

Sample Preparation SEM-EDX and XRD

Rock samples were taken from the Mt. Arjuno Welirang, we took a small portion of rock samples with
a size of approximately 5 x 5 x 5 cm for each one lithology. After that, we do grinding to minimize the size of
the samples. Grinding was done by pounding it with a hammer and become powder. Then, the powder of the
samples inserted into a plastic clip and labeled in accordance with the code of each rock sample . Each plastic
has mass approximately 50 grams of powdered rock.

SEM-EDX Laboratory Tests

The tools were used is SEM EVO MA 10. Prior to the test SEM-EDX, first coating process which
serves to coat the non-conductor material to be conductors so that X-Ray beam can be reflected. A magnification
used in this analysis is 500x, 750x, 1000x and 5000x. First, the sample placed in the sample chamber then turn
on the

vacuum pump so that no air can hinder the speed of electrons strikes the atoms in the sample. Then the
electronic control switched on. This process takes approximately 3 minutes, while the screen is turned on. The
results of the topography of the sample could be seen through the screen, trackball used to find parts of the
sample to be tested, and the magnification can be set.

X-Ray Diffraction (XRD) Laboratory Tests

The XRD test is done using XRD PANalytical X-Pert. The crushed rock samples are put into the tool. This tool
is connected to a computer in order to see the output of a graph. The graph shows diffraction peaks which
indicate certain profile of minerals in the rock samples. In order to understand the type of minerals, the XRD
data has to be further processed using additional software.

4
Creating Graphs using Software
Mineral analysis was done by using Match! Software. Match! works by picking peaks which
resemble the profile of rock forming minerals in each sample. The known minerals will be related to the
elements found from SEM-EDX. The processing result of XRD data is shown in attachments.

HYDROTHERMAL ALTERATION
Various rock properties and heat intensity show the uniqueness of geothermal systems. They are
different with another. Not only they differ in terms of surficial manifestations and reservoir characteristics, but
also the chemical properties of the water and the gas. Meteoric water which gets into the subsurface can be
altered chemically if it flows near a heat source, changing its composition. Same thing applies to rocks. The
minerals that form the rocks can be altered if they are exposed to a heat source.
Hydrothermal alteration is a process of reaction between rocks and deep chloride water. The reaction
results in the settling and exchanging of elements between the rocks and the fluids. It produces minerals like
chlorite, adularia, and epidote. Minerals inside shallow water environment are acid and are able to alter initial
rock minerals into clay minerals while in the same time, removing other minerals. Resulting minerals of the
process in shallow environment are kaolinite, alunite, residual sulfur, silica, and gypsum. In short, hydrothermal
alteration can be defined as the alteration of mineralogy and texture of rocks as a result of contact between
hydrothermal fluid and rocks.
Hydrothermal alteration affects the formation of altered minerals that are grouped based on formation
temperature and fluid pH (Guilbert and Park, 1986). In this process, mineral alteration is mainly controlled by
two factors, temperature and chemical properties of hydrothermal solution (Browne, 1991) (table 1). Based on
these factors, there are eight types of alteration. (Guilbert dan Park, 1986)(table 2).

Table 2: Mineral alteration based on its mineral content (Guilbert dan Park, 1986)
Type Key Minerals Accessories Notes
Minerals
Propolitic Chlorite Albite Temperature 2000-3000C, salinity varied, pH
Epidote Quartz close to neutral, areas with low permeability
Carbonic Calcite
Pyrite
Clay Wrap
Iron Oxide
Argilic Smectite Pyrite Temperature 1000-3000C, low salinity, pH acid-
Montmorillonit Chlorite neutral
e Calsite
Illite-smectite Quartz
Kaolinite
Advanced Argilic Kaolinite Kelsidon Temperature 1800 C, pH acid
(low temperature) Alunite Cristobalite
Quartz
Pyrite
Advanced Argilic Pirofilit Quartz Temperature 2500-3500C, pH acid
(high temperature) Diaspora Tourmaline
Andalusit Enargit
Lunozit
Potassic Adularia Chlorite Temperature>3000C, near intrusion area
Biotite Epidote
quartz Pyrite
Illit-Serisit
Phyllic Quartz Anhidrit Temperature 2300-4000C, salinity varied, pH
Serisit Pyrite acid-neutral, permeable zone at the boundary of
Pyrite Calcite uric
Rutile
Serisitik Serisit (illit) Pyrite -
Quartz Illit-serisit
Muskovite
Silicification Quartz Pyrite -
Illit-serisit
5
Adularia
Table 3: The result of SEM-EDX Analysis of Arjuno Welirang rock samples
Sample Unsure Name
Code C O Na Mg Al
Atom. C [at.%]
AAP1 16.64 52.41 0.72 0.14 1.86
AL1 1.79 76.48 1.20 1.35 5.36
AL2 37.62 50.91 0.71 0.29 3.45
AL3 34.65 55.60 0.53 0.16 3.14
LJP2 20.08 64.93 0.94 0.28 4.62
QAPTW 1.16 75.24 1.43 0.21 8.08
QAPW 20.59 63.67 1.14 0.34 4.51
QES 20.59 63.67 1.14 0.34 4.51
QLTAW 22.61 62.81 0.81 1.09 3.55
QLWI 24.78 60.32 1.03 0.31 4.29
QPA 29.98 55.60 1.00 0.73 3.56

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 Table 4: X-Ray Diffractometry data analysis using Match! of Arjuno Welirang rock samples
Sample Code Minerals
AAP1 Maghemite, ALBITE High, Merrihueite, Clinopyroxene, Rutile, Calcite
AL1 Hawaiite, Quartz, Yeelimite, Anorthite, Yeelimite, Cassiterite
AL2 Anorthite, Bronzite, ALBITE, Sanidine, Agrelite, Hollandite, Diopside, Chalopyrite,
Apuanite
AL3 Enstatile, Chromite, Leucite, Slawsonite, Pyroxomangite, Monticillite, ALBITE High
LJP2 Anorthite, Jadaide, ALBITE Low, Labradorite, Kyanite, Cementite, Pyroxmangite
QAPTW Sapphirine, Labradorite, Kyanite, ALBITE Low, Pyroxmangite, Hedenbergdite, Jadeite,
Hollandite
QAPW Anorthite, Kyanite, Jadeite, Hedenbergite
QES ALBITE, Cristobalite low, Enstatite, Anorthite, Delafossite, Freudenbergite, Magnetite,
Hedenbergite, Jadeite, Olivine, Clinoferrosilite
QLTAW ALBITE, Cristobalite low, Enstatite, Anorthite, Delafossite, Freudenbergite, Magnetite,
Hedenbergite, Jadeite, Olivine, Clinoferrosilite
QLWI ALBITE, Cancrinite, Cristobalite, Ramsdellite, Baratovite, Yeelimite
QPA Hedengergite, Microcline Maximum, Bytownite, Cristobalite, Enstatite
Anorthite (Ca Al2 Si2 O8) is a mineral of
RESULTS AND DISCUSSION feldspar group which is formed the earliest at high
Quarter aged volcanic products are the dominating temperatures.
rock in nearly all of Arjuno-Welirang area. These Cristobalite (SiO2) is the other form of
volcanic products can be classified based on their silicate which is formed at 180C and is acidic.
eruption point. Lithology of the complex itself is Kyanite (Al2 (Si O4) O) is a silicate that is
mainly consisted of andesite-basalt which is further classified as neosilicates. It is a form of altered
be classified as volcanic products: Anjasmoro, minerals. The metamorphism process that results to
Arjuno, Welirang, Penanggungan, Kembar, and its formation is usually involving high pressure
Bulak. Sampling can be grouped into eleven rock with low temperature.
units, namely Produk Anjasmara (QPA), Lava Tua Calcite (CaCO3) is a mineral that is
Arjuno Welirang (LTAW), Aliran Piroklastik Tua considered as carbonate and is the most stable
Arjuno Welirang (QAPTW), Erupsi Samping polymorph calcium carbonate. It is formed between
(QES), Lava Welirang I (QLWI), Aliran Piroklastik 2300-4000C in various salinity. pH level ranging
Welirang I (QAPWI), Aliran Lava 1 G.Arjuno from acid to neutral.
(AL1), Aliran Lava 2 G.Arjuno (AL2), Aliran Lava Quartz is formed between 250-350C.
3 G.Arjuno (AL3), Aliran Piroklastika 1 G.Arjuno and tend to be acidic (table 2). Quartz is the most
(AAP1), and Endapan Jatuhan Piroklastika 2 stable form of silicate in a hydrothermal system
G.Linting (LJP2). All of the samples were analyzed that whenever a fluid is exposed to lower
in a laboratory using SEM-EDX and XRD. Based temperatures, silicate is readily in the form of
on these analyses on the samples, quartz. Meanwhile, anorthite is an indication of
minerals observed are as follow (see table 3 and lava (Keer P.D., 1959).
4). Laharic breccia and basaltic lava are
The XRD analysis of all eleven samples usually already exposed to strong alterations
indicates an appearance of altered minerals which mainly those located near hotsprings or fumaroles.
Formed altered minerals are albite, anorthite,
are albite (in samples AAP1, AL2, AL3, LJP2, cristobalite, kyanite, calcite, and quartz. All of
QAPTW, QES, QLTAW, and QLWI), anorthite (in these minerals are formed as a result of
samples AL1, AL2, LJP2, QAPW, QES, and hydrothermal alterations. Anorthite (table 1), is
QLTAW), cristobalite (in samples QES, QLTAW, interpreted as an indication of lava composition
QLWI and QPA), kyanite (in samples LJP2, (Keer P.D., 1959). Some parts of the lava is eroded
QAPTW, dan QAPW), clinopyroxene (in sample by lahar from eruptions. The eroded fragments are
AAP1), calcite (in sample AAP1), and quartz (in furthermore being transported along with the lahar,
sample AL1). being a part of the lahar. The parent rocks of altered
Albite (Al2 Si O5), is a mineral from rocks are andesite and basaltic lava.
feldspar group with silicate clast and tectosilicate In general, in the process of drilling,
sub clast and is formed by hydrothermal process geologists predict temperatures of particular
and alteration of plagioclase. Its formation involves minerals. Some minerals are good indicators of
temperature ranging between 100-200C (based on high temperature in the subsurface. These minerals
table 5) in various salinity. PH levels is usually are epidote, actinolite, and biotite. Epidote
nearing neutral. And it is formed in zones with low indicates temperature of 220C, actinolite indictaes
permeability.

7
300C, and biotite indicates 325C (Hoagland and According to Tim Survey Terpadu, 2010,
Elders, 1978). prospective area of Arjuno-Welirang geothermal
complex is limited to the area inside several
manifestations, namely the Welirang fumarole,
Cangar hotspring, Coban hotspring, and Padusan
hotspring. This prospective area is further can be
limited by several other factors. For example, it is
further limited to area with anomalous value of Hg
(>200 ppb), CO2 (>4.5%). Another factor including
resistivity contrasts in the northern and the southern
boundary of the predicted area, plus geological
structures on the west and eastern boundary. The
total area is approximately 20 km 2 and is classified
as predicted reserve. This calculated area excludes
forested area. Volumetric method (Lump
parameter) utilized to estimate the geothermal
potential. The estimation assumes reservoir
thickness to be 1.5 km, with a recovery factor of
50% and conversion factor of 10%, plus, a lifetime
prediction of 30 years. Based on this estimation,
the geothermal potential in the complex is
approximately 278 MWe and classified as predicted
reserve.
In this research, reservoir temperature can
be predicted by correlating the XRD analysis result
with altered mineral standards by Izawa 1993 (table
5). Based on the XRD analysis, found altered
minerals are albite, cristobalite, and quartz. Albite
is formed at temperatures less than 200C.
Cristobalite is formed at temperatures less than
100C with acidic ph level. Quartz is formed at
temperatures more than 250C. The appearance of
quartz indicates that the reservoir is predicted to
have a temperature of more than 250C and
therefore, classified as high enthalpy geothermal
system (Hochestein, 1990). Based on alteration
type standards (table 2), the dominating altered
minerals in the XRD analysis result indicates that
the involved alteration is propylitic to advanced
argillic.

pH 100oC 200oC 300oC

Table 5:
Relationship -----------Alunit-------------
Acid betweenCristoballite ---------------Quartz------------------------------------
temperature,Haloisit
pH Kaolinit Dikit Pirofilit (Diaspor)
level, andMonmorilonit Ilit/SmektitIlit
Weak Acid-Neutral (Smektit/
altered minerals Biotite
Fe-saponit)
(Izawa, 1993). (Khlorit/Smektit) Khlorit (Aktinolit)
Epidote
---------K-felspar---------------------------------------------------
(Stilbit) Prehnit
Alkalin (Heulandit) (Yugarawait)
Mordenit Laumontit Wairakit (Plagioclas)
(Analsit) (Albite)

CONCLUSION

8
 Mineralization in Arjuno-Welirang
complex is mainly formed by propylitic to
advanced argillic alteration. It is consisted of
altered minerals: Albite, anortite, cristobalite,
kyanite, clinopyroxene, calcite, and quartz. Based
on this finding, it can be interpreted that there are
alterations in the complex. Mineralization is
formed around 230C which can be classified as
high enthalpy geothermal system with
hydrothermal fluid pH nearing acid to neutral.
Furthermore, the predicted prospective area is
around 20 km2 and reservoir thickness for about 1.5
kilometers. Thus, Arjuno-Welirang complex is
predicted to have a geothermal potential
approximately 278 MWe with 30 years lifetime.
BIBLIOGRAPHY
Corbett G and Leach T 1997. Hydrothermal
Alteration in Active Geothermal Fields.
Annual Review Earth and Planetary
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Kementrian Energi dan Sumber Daya
Mineral Panas Bumi Indonesia Baru
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bberita/panas-bumi/56-panas-bumi-
indonesia-baru-termanfaatkan-14-000-
mw.html. Accessed on 8th January 2017
Guilbert, G.M & Park, C.F. 1986. The Geology of
Ore Deposits. W.H Freeman and Company,
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Hedenqist, J.W and White N.C 1997. Epithermal
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Exploration. Kursus singkat, The University
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dan sekitarnya, kecamatan tirtomoyo,
kabupaten wonogiri, propinsi jawa tengah.
Proceeding TPT XVI PERHAPI.
Indarto, Sri, ETC. 2006. Studi Batuan Volkanik dan
Batuan Ubahan Pada Lapangan Panas
Bumi Gedongsongo Kompleks Gunung Api
Ungaran Jawa Tengah. RISET Geologi
dan Pertambangan Jilid 16 N0.1 Tahun
2006, Hal. 30-43
Izawa, E. 1993. Hydrothermal Alteration In
Geothermal System. Departement of Mining
Kyusu University.
Keer P.D., 1959, Optical Mineralogy, Mc. Graw
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Saptadji, Nenny Miryani. 2009. Karakterisasi
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APPENDIX

SEM-EDX Results

figure 2: Graph Elements of AAPI Rock Sample

figure 3: Graph elements of AL1 rock sample

figure 4: Graph Elements of AL2 rock sample

figure 5: Graph Elements of AL3 rock sample

Figure 6: Graph elements of LJP2 rock sample

Figure 7: Graph elements of QAPT rock sample

Figure 8: Graph elements of QES rock sample

Figure 9: Graph elements of QLTA rock sample

Figure 10: Graph elements of QLW rock sample

Figure 11: Graph elements of QPA rock sample

Figure 12: Graph elements of QPAW rock sample