Bodnar RJ (2003) Reequilibration of fluid inclusions. In I. Samson, A. Anderson, & D. Marshall, eds.
Fluid Inclusions: Analysis and Interpretation. Mineral. Assoc. Canada, Short Course 32, 213-230.
CHAPTER 8. REEQUILIBRATION OF FLUID INCLUSIONS
Robert J. Bodnar
The Bubble Factory
Virginia Tech
Blacksburg, VA 24061 USA
rjb@vt.edu
INTRODUCTION
A fluid inclusion provides microthermo -
metric data that can be used to infer trapping
conditions only if the inclusion satisfies several
criteria (Roedder 1984). First, the inclusion must
trap a single, homogeneous phase. Secondly, the
inclusion must remain a constant volume system
after trapping (excluding reversible elastic
volume changes) and, thirdly, nothing can be
added to, or removed from the inclusion follow-
ing trapping. These criteria are here referred to as
"Roedder's Rules", and must be met if one wishes
to use inclusions to reconstruct the thermobaric
history of the host rocks. If the inclusion volume
changes, or if anything is added to or lost from
the inclusion following trapping, the inclusion is
said to have reequilibrated. Reequilibration can
occur in nature during continued burial or uplift
of the rock to the surface, or reequilibration may
occur during sample preparation and/or data
collection in the laboratory. Less often considered
by inclusionists is the possibility that fluid
inclusions in samples collected from surface
outcrops may have experienced elevated temper-
atures during exposure to the sun or to forest fires,
or may have undergone freezing in colder
climates. Especially for low temperature
inclusions, these temperature fluctuations may
have been sufficient to cause reequilibration.
As a result of numerous studies of both
natural and synthetic fluid inclusions over the past
few decades, we now have a fairly comprehensive
understanding of the reequilibration process.
Before I discuss the physical and chemical factors
that affect the reequilibration process, it is first
necessary to introduce the various terms that are
used to describe fluid inclusion reequilibration. In
the fluid inclusion literature, reequilibration is a
general term that has been used to describe fluid
inclusions that have cha nged volume, or have lost
or gained components, or both. Stretching is a
term that is generally used to describe fluid
inclusions whose volume has changed with little
or no discernible loss of fluid from the inclusion
213
(Fig. 8-1). The term was first introduced by
Larson et al. (1973) to describe permanent,
nonelastic deformation of the walls of inclusions
in fluorite and sphalerite as a result of
overheating. Stretching usually results when an
inclusion reequilibrates in a low strain rate
environment in which the host phase deforms
plastically, and is more common in softer
minerals than in harder minerals. Any material
that is lost from the inclusion occurs as a result of
diffusion or leakage along dislocations (Wilkins
et al. 1981, Bodnar & Bethke 1984, Wilkins
1986, Bakker & Jansen 1991, 1994, Hall &
Sterner 1993, Vityk et al. 2000).
With increasing strain rate, fractures may
develop in the host adjacent to inclusions, with
partial loss of fluid by advection along the
microfractures. This type of reequilibra tion is
referred to as leakage or partial decrepitation.
Sometimes, the extent of fracturing is so intense
that all fluid is lost, leaving an empty, dark cavity
in the host phase. This is referred to as
decrepitation. Note that the resulting inclusions
are probably not sensu stricto empty but, rather,
likely contain a low-density version of the
original fluid (water vapor or CO2 gas, for
example). The inclusions are referred to as being
empty because no fluid phase is observed during
petrographic or microthermometric examination.
The term decrepitation was introduced
by researchers in the former Soviet Union to
describe the explosive release of inclusion
contents during heating. In the early days of fluid
inclusion research, before the development of
microscope heating/cooling stages and high-
quality long-working distance microscope
objectives, workers would heat mineral samples
in a furnace with a sensitive microphone attached.
The microphone records acoustic emissions (i.e.,
noise) associated with decrepitating fluid
inclusions, and the decrepitation temperatures
would be related to inclusion trapping
temperatures (incorrectly, in many cases!).
 Type of Deformation Deformation Fluid Loss Observational
Reequilibration Environment Mechanism Mechanism Result

STRETCHING LOW PLASTIC DIFFUSION UNDETECTABLE

STRAIN FLUID LOSS (±H2)
RATE

LEAKAGE

DETECTABLE
FLUID LOSS
PARTIAL
DECREPITATION

HIGH
STRAIN COMPLETE
DECREPITATION RATE BRITTLE ADVECTION FLUID LOSS

FIG. 8-1 Schematic representation of the relationship between different types of fluid inclusion
reequilibration (stretching, leakage, decrepitation) and the environment of deformation (strain rate), the
mechanisms of deformation (plastic vs. brittle) and fluid loss (diffusion vs. advection), and the amount of
fluid lost from the inclusion during deformation (undetectable to complete). According to these
relationships, stretching is associated with plastic deformation in a low strain environment, where
undetectable amounts of fluid may be lost from the inclusion by diffusion. Conversely, decrepitation is
associated with brittle deformation in a high strain environment, with partial to complete loss of fluid by
advection along fractures. (from Vityk et al. 2000).
Related to this, Hall & Bodnar (1989) showed during cooling, and were able to reverse this
that energy detected during acoustic emission process during laboratory heating. In this chapter,
studies of natural rocks and minerals is directly these somewhat specialized cases of
related to decrepitation of fluid inclusions in the reequilibration will not be considered further.
sample. The type of reequilibration that occurs is
An additional type of reequilibration a function of many factors, and in a given fluid
sometimes occurs when the fluid in the inclusion inclusion assemblage some inclusions may show
reacts with the host phase after trapping to evidence of significant reequilibration, while
generate a new mineral assemblage. For example, others may show no evidence of reequilibration.
Kleinefeld & Bakker (2002) report the presence Below I outline some of the many factors that
of calcite, paragonite and pyrophyllite crystals in affect the reequilibration process. Of particular
fluid inclusions in plagioclase, and relate their importance is the effect of time on the
origin to reaction of the CO2 -rich fluid with the reequilibration process, because this may affect
calcite host. Similarly, Heinrich & Gottschalk the applicability of laboratory-based studies to
(1995) observed inclusions containing calcite and reequilibration of fluid inclusions in nature. The
quartz crystals in wollastonite. These phases were intent of this chapter is to provide information
generated by the reaction of the wollastonite host that inclusionists might gain from petrographic
with the CO 2 -bearing fluid during retrogression. and microthermometric analyses of inclusions,
Kodera et al. (2003) reported the occurrence of and excludes detailed theoretical discussions of
ferropyrosmalite [(Fe,Mn)8Si6 O15 (OH,Cl)10 ] in the reequilibration process. Note, however, that
fluid inclusions in magmatic quartz. These the empirical observations presented below are
workers attribute the origin of this phase to generally consistent with theoretical models for
reaction of an original clinopyroxene daughter mineral deformation. For a more detailed
mineral with the saline solution in the inclusion discussion of the theoretical basis for mineral

214
deformation, the reader is referred to Poirier
(1985) and to Küster & Stöckhert (1997) for a
discussion of rock deformation theory applied to
fluid inclusion reequilibration.
WHAT DETERMINES HOW EASILY AN
INCLUSION WILL REEQUILIBRATE?
Mineralogy
The most important factor that
determines the ease with which fluid inclusions
reequilibrate is the structure and composition of
the host phase. As fluid inclusion reequilibration
involves the breaking or modification of bonds
within the host mineral, the ease with which a
mineral reequilibrates can be correlated with the
weakest bond in that mineral. While there are
many ways of characterizing bond strength, one
of the most basic is related to the hardness of the
mineral. Minerals with small atoms that are
tightly packed and involve covalent bonds are
harder than those containing larger atoms that are
held together by van der Waals or metallic bonds.
Among the first to recognize the rel-
ationship between mineral hardness and the ease
with which fluid inclusions reequilibrate were
Tugarinov & Naumov (1970), who noted a linear
relationship between Mohs hardness and the
pressure required to decrepitate fluid inclusions in
several minerals (Fig. 8-2). Thus, fluid inclusions
in soft minerals such as orpiment and stibnite
(Mohs hardness ˜ 2) will reequilibrate
(decrepitate) when the internal pressure reaches
only a few hundred bars, whereas about 800 bars
of internal pressure is required to initiate
reequilibration of inclusions in quartz (Mohs
hardness ˜ 7). Faiziev & Alidovov (1976) also
noted that inclusions in soft minerals with perfect
cleavage (e.g., fluorite, calcite, sphalerite, and
scheelite) show an increase in measured
homogenization temperature during repeated
measurements. These workers attributed reequil-
ibration to the presence of weak bonds between
cleavage layers, consistent with observations by
Tugarinov & Maumov (1970). The consistent

FIG. 8-2. Relationship between the internal pressure necessary to initiate reequilibration of fluid inclusions
and the Moh s hardness of the host mineral (modified from Tugarinov & Naumov, 1970). Ranges in
pressure for calcite, barite, sphalerite, fluorite and quartz represent the variation in pressure as a function of
inclusion size. Size data for quartz are from Bodnar et al. (1989); data for fluorite and sphalerite are from
Bodnar & Bethke (1984); data for barite are from Ulrich & Bodnar (1988); data for calcite are estimated
from Hall et al. (1993) and Prezbindowski & Larese (1987).

215
relationship between Mohs hardness and the
pressure required to cause reequilibration of fluid
inclusions makes it possible to estimate the
suitability of a given mineral for fluid inclusion
studies. Thus, one would expect that gypsum,
with a Mohs hardness of 2, might not be the best
host for fluid inclusion studies, whereas
corundum, with a Mohs hardness of 9, would be
an ideal mineral for fluid inclusion studies.
It should be recognized that Mohs
hardness is not a quantitative scale but, rather, a
qualitative scale that makes it convenient to
compare the relative hardness or tensile strength
of two minerals. The absolute hardness (or tensile
strength) of a mineral is not a linear function of
Mohs hardness. Thus, the difference in absolute
hardness between quartz (Mohs hardness = 7) and
topaz (Mohs hardness = 8) is about the same as
the difference in absolute hardness between talc
(Mohs hardness = 1) and quartz. As such, Figure
8-2 shows the relationship between pressure
required to initiate reequilibration and Mohs
hardness over the range of experimental
observations (Mohs hardness ˜ 1-7), but should
not be applied to minerals with a Mohs hardness
greater than that of quartz (=7). It is expected that
in the future additional empirical data will
become available for minerals with Mohs
hardness above that of quartz, allowing the trend
shown on Figure 8-2 to be extended to higher
values of Mohs hardness.
The type of reequilibration that occurs is
also somewhat related to mineral hardness. As
noted above, soft minerals tend to reequilibrate by
stretching to produce a gradual increase in
homogenization temperature as reequilibration
proceeds, whereas harder minerals such as quartz
tend to maintain their original homogenization
temperature until the inclusion decrepitates with
complete loss of fluid. It should be emphasized,
however, that many exceptions to this general
trend have been reported. For example, Ulrich
and Bodnar (1988) observed decrepitation of
inclusions in the soft mineral barite (Mohs
hardness ˜ 3), and Bodnar et al. (1989) noted that
some fluid inclusions in quartz reequilibrated by
stretching (followed by later decrepitation).
Additionally, minerals that reequilibrate by brittle
failure (decrepitation) in the laboratory may
reequilibrate by stretching or leakage under the
higher confining pressures and much lower strain
rates common in nature. Thus, Guilhaumou et al.
216
(1987, 1988) found that fluid inclusions in fluorite
decrepitated with complete loss of fluid when
overheated in the laboratory at one atmosphere
confining pressure, whereas inclusions from the
same sample that were overheated under 200 or
400 bars of confining pressure reequilibrated by
stretching.
Inclusion Size
Whereas the mineralogy of the inclusion
host appears to be the most important factor
controlling the pressure required to reequilibrate
fluid inclusions, the "average" pressure can vary
significantly depending on inclusion size.
Naumov et al. (1966) and Tugarinov & Naumov
(1970) determined that fluid inclusions larger than
about 35 µm in quartz decrepitate when the
internal pressure reaches about 850 bars. Leroy
(1979) reported that this pressure increases to 1.2
kbar for 12 -13 µm fluid inclusions, and that
inclusions smaller than 12 µm did not decrepitate
even when the internal pressure reached 2.7
kbars. Swanenburg (1980) reported that
approximately 1 µm inclusions were able to
maintain internal pressures of 5–7 kbars before
decrepitating.
Bodnar et al. (1989) conducted an
experimental study of the decrepitation behavior
of fluid inclusions in quartz and combined their
results with those of Leroy (1979) and
Swanenburg (1980) to produce the following
relationship between inclusion size and the
internal pressure required to initiate
reequilibration (Fig. 8-3):
Pressure (kbar) = 4.26 D-0.423 (1)
where D is the inclusion diameter in micrometers.
According to equation (1), the internal pressure
required to reequilibrate inclusions in quartz
varies from 0.8 kbar for a 50 µm inclusion, to 1.6
kbars for a 10 µm inclusion, to 4.3 kbars for a 1
µm inclusion (Fig.8- 3).
Bodnar and Bethke (1984) found a
similar relationship between inclusion size and
the minimum pressure required to initiate
stretching of fluid inclusions in fluorite.
According to these workers, the internal pressure
required to initiate stretching decreases with
inclusion size according to:
Pressure (bars) = 900 - 147 log10V (2)
FIG. 8-3. Relationship between inclusion size and the pressure required to reequilibrate fluid inclusions in
quartz under one atmosphere confining pressure. Inclusion volumes shown on the lower abscissa were
converted to inclusion diameter assuming a spherical geometry and are shown on the top abscissa (modified
from Bodnar et al. 1989).
where V is the inclusion volume in µm3 . concentration surrounding flaws (fluid inclusions)
Assuming a spherical geometry, this translates to in minerals.
about 635 bars for a 5 µm inclusion, and 200 bars Prezbindowski & Larese (1987)
for a 50 µm inclusion. Bodnar & Bethke (1984) conducted an experimental study of stretching of
also observed a clear relationship between fluid inclusions in calcite and found that larger
inclusion size and the internal pressure required to inclusions stretch more (i.e., the homogenization
stretch fluid inclusions in sphalerite, but were temperature increases by a larger amount) than
unable to accurately calculate the inclusion smaller inclusions subjected to the same P-T
volumes because the vapor bubbles were not history. Based on the results of Bodnar & Bethke
spherical at room temperature, precluding (1984), which indicate that the amount of
application of the technique described by Bodnar stretching (change in the homogenization
(1983). According to their data, the pressure temperature) for a group of inclusions that
necessary to stretch an inclusion smaller than initially had the same homogenization
about 5-10 µm in sphalerite is about 800 bars, temperature can be related to the temperature at
whereas an inclusion 50 µm in diameter requires which stretching begins, the results of
about 300-400 bars of internal pressure (Fig. 8-2). Prezbindowski & Larese (1987) would suggest
The relationship between inclusion size and the that the larger inclusions began to stretch before
pressure required to initiate stretching is less well the smaller inclusions. Goldstein (1986) observed
defined for inclusions in barite (Ulrich & Bodnar a similar size-pressure relationship for naturally
1988), although the trend indicates higher reequilibrated inclusions in low temperature
pressures for smaller inclusions, consistent with calcium carbonate cements. However, Hall et al.
other minerals studied. Prezbindowski & Tapp (1993) found no correlation between inclusion
(1991) showed that the size-pressure relationship size and ease of stretching during an experimental
observed in fluid inclusions is consistent with study of calcite, although they did notice that
theoretical models of crack propagation and stress inclusions closer to the mineral surface were more

217
prone to stretching compared to those deeper in
the sample.
Inclusion shape
A secondary factor that determines how
easily a fluid inclusion will reequilibrate is
inclusion shape. Bodnar et al. (1989) noted that
the average pressure required to reequilibrate
fluid inclusions in quartz increased by about 400
bars as the inclusion shape varied from very
irregular, with many reentrants or "tentacles", to
one that was spherical or negative-crystal shaped.
Goldstein (1986) noted a similar dependence on
inclusion shape for calcite, as did Bodnar &
Bethke (1984) for inclusions in fluorite and
sphalerite. The relationship between inclusion
shape and the amount of pressure required to
initiate reequilibration is generally consistent with
theoretical deformation models which indicate
that stress is concentrated at sharp corners, and
that the stress approaches infinity at crack tips
(ends of tentacles in irregularly-shaped
inclusions) or at the corners of angular inclusions
(Prezbindowski & Tapp, 1991). However, the fact
that most angular inclusions do not spontaneously
stretch or decrepitate during heating suggests that
while theoretical models of deformation provide
valuable insights into the reequilibration process,
they may be less useful than empirical models for
predicting the reequilibration behavior of fluid
inclusions.
Fluid Composition
Little information is available
concerning the role of fluid composition in the
reequilibration process. However, one would
expect that fluid inclusions containing water
might reequilibrate more easily than those that are
water-free, owing to the presumed higher
solubilities of host minerals in aqueous fluids
compared to, for instance, carbon dioxide. Hall &
Wheeler (1992) conducted a preliminary study of
the relationship between fluid composition and
inclusion decrepitation and found that 3 µm
diameter inclusions containing H2 O-NaCl
required a lower pressure (3.0 kbars), and
inclusions containing H2 O-CO2 a higher pressure
(4.2 kbar), compared to pure H2 O inclusions (3.4
kbars) of the same size. The role that fluid
composition plays in reequilibration is an area of
research that should be given high priority in
future studies.
218
HOW DO WE RECOGNIZE INCLUSIONS
THAT HAVE REEQUILIBRATED?
Often, one may be able to infer that
reequilibration has occurred based on
petrographic observations of fluid inclusions and
the surrounding host mineral. If the fluid
inclusions within a fluid inclusion assemblage
(FIA) satisfy "Roedder's Rules" described above
and have not reequilibrated, all of the inclusions
in the FIA will contain the same phases, and in
the same volume proportions, when observed at
room temperature. Thus, an FIA composed of
two-phase (liquid + vapor) inclusions in which
the liquid-to-vapor ratio is identical in all
inclusions might indicate that reequilibration has
not occurred. But, one must use care in
determining whether the inclusions have the same
liquid-to-vapor ratio. For example, consider an
FIA containing inclusions with a salinity of 5 wt.
% NaCl and which homogenize at 150°C. If some
of the inclusions reequilibrate by stretching such
that the new homogenization temperature is
175°C, the volumes of the reequilibrated
inclusions would have increased by 2.6 volume
percent (see Bodnar & Bethke 1984, p. 153). If a
spherical vapor bubble in one such inclusion had
a diameter of 6 µm before stretching, the vapor
bubble diameter after stretching would be about
6.6 µm! Inclusions with smaller bubbles would
show proportionately smaller increases in bubble
diameter after stretching. It is unlikely that one
would be able to distinguish between two
inclusions in the same FIA with vapor bubble
diameters that differ by only 0.6 µm or less. Thus,
an FIA could contain fluid inclusions, some of
which had stretched by 25°C and others of which
had not stretched (or stretched by a smaller
amount), and still appear to have consistent
liquid-to-vapor ratios. However, this difference
would become obvious during microthermometric
analysis of the inclusions, as described below.
Finally, it should be emphasized that, whereas
most reequilibration results in a "smearing" of
data to produce a wide range in homogenization
temperatures, in some environments the reequilib-
ration process may progress to the extent that the
inclusions completely equilibrate at some new P-
T condition, resulting in fluid inclusions with
consistent phase ratios and microthermo metric
results, even though these are not representative
of the original formation conditions (Vityk &
Bodnar 1995a, 1998).
 Just as an FIA with real or apparently
consistent phase ratios is possible even if
inclusions have reequilibrated, a range in liquid-
to-vapor ratios is not always indicative of
reequilibration. If the inclusions were trapped in a
boiling (or immiscible fluid) system, a bimodal
distribution of phase ratios will result, with a
complete range between the end-member ratios
from trapping mixtures of the two phases present.
Fortunately, the range of possible phase ratios is
not entirely random, and is controlled by the
PVTX properties of the two immiscible fluids,
and the possible phase ratios that might result
from trapping mixtures may be calculated using
PVTX data (see Bodnar et al. 1985, their Fig.
5.5).
Textural features in the host mineral
surrounding fluid inclusions perhaps provide the
most diagnostic evidence for reequilibration.
When inclusions reequilibrate, the host phase
surrounding the inclusions is deformed to produce
a variety of features that are visible using
conventional optical microscopy or more sophist-
icated techniques such as cathodoluminescence,
transmission electron microscopy (TEM), or X-
ray tomography. Moreover, the textures that result
may be diagnostic of the P-T path followed dur-
ing reequilibration. Most experimental studies, as
well as studies of naturally reequilibrated inclus-
ions have focused on the mineral quartz, and the
discussion of fluid inclusion textures below is
limited to this mineral. It is expected that petro-
graphic features observed for quartz may not
always apply to other minerals that have signific-
antly different crystallographic and rheological
properties or solubility in the inclusion fluid.
Before discussing the various textural
features associated with reequilibrated fluid
inclusions in quartz, it is first necessary to
consider the vario u s P-T histories under which
fluid inclusions may be reequilibrated, because
each produces slightly different and, in some
cases, diagnostic textural features. Following
trapping, fluid inclusions may follow a P-T path
that maintains an internal pressure in the inclusion
equal to the confining (or lithostatic) pressure, or
may follow paths such that the internal pressure is
greater than or less than the confining pressure
(Fig. 8-4). If the inclusion follows an isochoric
path such that the confining pressure and the
internal pressure are always equal, reequilibration
is unlikely to occur. This type of cooling path is a
219
FIG. 8-4. Relationship between the cooling/
unroofing path and the confining pressure and
internal pressure in a fluid inclusion trapped at
temperature and pressure Tf, Pf.
special case that occurs only rarely in nature. In
most natural systems the rocks do not follow a P-
T path that approximates the inclusion isochore.
Rather, the confining (geologic) pressure is either
greater than, or less than, the internal pressure in
the inclusions. In these cases the inclusion is not
in equilibrium with the surrounding rock and
reequilibration may occur (see Diamond 2003,
Fig. 3-5).
If the inclusion follows a P-T path that
results in internal overpressure, the first
modification that inclusions experience is a
change in shape, often without a measurable
change in volume. Specifically, the inclusions
become more regularly shaped, and elongated
inclusions become more rounded or equant (Fig.
8-5) (Gratier & Jenatton 1984, Pêcher & Boullier
1984, Bodnar et al. 1989, Bakker & Jansen 1991).
The evolution from less to more regular or
negative-crystal shape represents the normal
maturation process that all fluid inclusions
undergo as they try to minimize their surface area,
as discussed by Bodnar et al. (1985). Given
sufficient time, all inclusions should approach an
equant or negative-crystal shape. Thus, the
evolution from irregular to more-regular inclusion
shape that occurs under conditions of internal
overpressure is not diagnostic of this type of

FIG. 8-5. Evolution in the shape of fluid
inclusions in quartz during reequilibration at
conditions of Pinternal > Pconfining. The
length/width ratio of the inclusion indicated by
the arrow gradually decreases with time to
produce an equant negative-crystal-shaped fluid
inclusion after being held at a temperature of
370°C and an internal pressure of 400 bars for
5621 hours. The scale bar equals 50 µm.
(modified from Bodnar et al., 1989).
220
reequilibration, and the presence of equant or
negative-crystal shaped inclusions in a sample
does not necessarily indicate that the inclusions
have reequilibrated. With increasing departure of
the confining pressure from the inclusion
isochore, the largest inclusions begin to
reequilibrate as fractures are generated at sharp
corners of the inclusion and extend into the
surrounding host (Kotel'nikova 1994, Vityk et al.
1996) (Fig. 8-6). Some of the fluid that escapes
along these fractures may be trapped in the
surrounding quartz to produce a halo of very
small fluid inclusions adjacent to the fracture. As
the difference between the inclusion pressure and
the confining pressure increases further,
progressively smaller inclusions begin to
reequilibrate. Barker (1995) used the evolution in
shape of inclusions reequilibrated under
conditions of internal overpressure to identify
those inclusions that had experienced post-
entrapment modifications in the Caledonian Øse
Thrust, Norway. Detailed TEM studies by
Boullier et al. (1989), Bakker & Jansen (1994)
and Vityk et al. (2000) show an increased
dislocation density surrounding reequilibrated
inclusions in quartz (Fig. 8-7). This is associated
with diffusive loss of water into the quartz host,
which results in hydrolytic weakening of the
quartz and facilitates later fracturing and
additional water loss.
Fluid inclusions in quartz that
reequilibrate under conditions of internal
underpressure (confining pressure greater than the
internal pressure) show some distinct differences
compared to those reequilibrated under conditions
of internal overpressure. The first change
observed in these inclusions is that the inclusion
walls, which are initially smooth, become
corrugated and rough (Pêcher 1981, Sterner &
Bodnar 1989, Bakker & Jansen 1991) (Fig. 8-8).
Associated with this change is the development of
a halo of secondary inclusions surrounding the
original inclusion. Bakker & Jansen (1991, 1994)
and Vityk et al. (2000) suggested that fluid from
the original inclusion (before reequilibration)
migrated into the surrounding quartz along
dislocations and was later trapped to form the
secondary inclusion halo. Compared to conditions
of internal overpressure, in which the largest
inclusions begin to reequilibrate first (at the
lowest amount of overpressure), the smallest
inclusions reequilibrate most easily under
 FIG. 8-6. Relationship between the intensity of
reequilibration features and the size and pressure
differential (P internal - Pconfining) for methane
inclusions in quartz from the Ukrainian Carpathian
Mountains. At low pressure differential (top row)
none of the inclusions show reequilibration
textures. With increasing departure of the
confining pressure and internal pressure in the
inclusions, the largest inclusions begin to
reequilibrate, while the smaller inclusions show no
reequilibration textures. Progressively smaller
inclusions begin to reequilibrate as the pressure
differential increases. All inclusions in samples
with the largest pressure differential (bottom row)
show evidence of fracturing and development of
haloes of secondary inclusions surrounding the
original inclusion. (from Vityket al., 1996)

FIG. 8-7. TEM photomicrographs showing microstructures produced during reequilibration at 625°C and 2
kbar. The inclusions were originally formed at 700°C and 5 kbar, resulting in an internal overpressure
(Pinternal - Pconfining) of about 2.1 kbar at the reequilibration conditions. Fluid inclusions in "A" and "B"
are surrounded by poorly healed fractures (arrow 1), a few dislocations connected to the inclusion walls
(arrows labeled 2), and a Dauphine twin (arrow #4 in "B"). Note the high density of water bubbles in the
healed fracture in "A". Also note that some dislocations are pinned with bubbles (arrows #3 in "A"). (from
Vityk et al., 2000).

221
 FIG. 8-8. Evolution of fluid
inclusions in quartz after
reequilibration at con-
ditions of Pinternal <
Pconfining. The inclusions
were originally formed at
800°C and 1.35 kbars, and
then reequilibrated at
700°C and 4 kbars,
producing a pressure
differential (Pconfining -
Pinternal) of about 2.75
kbars. Note the develop-
ment of corroded walls and
the formation of a halo of
secondary inclusions in the
surrounding quartz. The
scale bar in A, C and E
represents 25 µm. (from
Sterner et al. 1989).

conditions of internal underpressure (Fig. 8-9)
(Hurai & Horn 1992, Vityk et al. 1994). Careful
petrographic observations to determine whether
the smallest or the largest inclusions in a given
sample show the most intense reequilibration
features may provide a means of determining
whether the sample experienced an initially
isobaric cooling path, or an initially isothermal
unroofing path, following formation.
Microthermometric Evidence
As the inclusion volume or composition
changes, the microthermometric behavior of
inclusions will change in a somewhat predictable
manner. An increase in volume without fluid loss
results in a lower density and concomitant
increase in the homogenization temperature.
Based on numerous laboratory studies, when a
group of inclusions with initially uniform
homogenization temperatures is overheated by a
certain amount, the amount of stretching (percent
volume increase) of the inclusions in the FIA is
highly variable, resulting in a wide range of
homogenization temperatures. For example, Vityk
& Bodnar (1998) reported that 160 fluid
inclusions in quartz that were trapped at 700°C
and 5 kbars all homogenized within a three degree
range from 282-285°C. Another sample was
formed at the same conditions and then cooled to
625°C and 2 kbar and held at these conditions for
30 days, resulting in an initial internal
overpressure in the inclusions of about 2.1 kbars.
After 30 days the sample was quenched and the
homogenization temperatures of the inclusions
were measured. Not only had the temperatures
been shifted to higher values compared to the
original Th, but also the original three degree
Celsius range in Th (282-285°C) had expanded to
about 65 degrees Celsius (˜ 310-375°C).
The relationship between the range in Th
and extent of stretching observed in laboratory
studies may not be applicable to reequilibration in
nature, as noted in the introduction to this chapter.
While it is true that stretching results in a wide
range in Th during laboratory reequilibration
studies, if these same samples were held at the
reequilibration conditions for durations
approaching geologic time scales (102 - 106
years), it is likely that the homogenization
temperatures of all the inclusions would approach
some new "equilibrium" homogenization
temperature. Results presented by Vityk &

222

FIG. 8-9. Relationship between the intensity of
reequilibration features and the size and pressure
differential (Pconfining - Pinternal) for aqueous
inclusions in quartz from the Bayanovoo granite
in central Mongolia. The inclusions were
reequilibrated at 500°C and pressures of 1 (A-C),
2 (D-F), 3 (G-I), 4 (J-L) and 5 (M-O) kbar for 7
days. At run conditions, all of the inclusions had
an internal pressure of about 500 bars. With
increasing pressure differential the smaller
inclusions begin to reequilibrate first, followed
by increasingly larger inclusions as the pressure
differential increased from about 500 bars (A-C)
to 4.5 kbar (M -O). (from Vityk et al. 1994).
Bodnar (1995a, 1998) are consistent with this
suggestion.
Goldstein (1986) examined fluid
inclusions from recent calcium carbonate cements
that had formed at the surface and were never
deeply buried. He compared these to inclusions in
223
similar cements that had formed at the surface but
were later buried to significant depths and
exposed to temperatures well above 100°C. The
recent samples that had never been buried
contained mostly all-liquid inclusions, in addition
to liquid + vapor inclusions that had trapped water
plus air. Deeply buried samples showed a wide
range in homogenization temperatures and
salinities, reflecting continued reequilibration
during burial and exposure to fluids of different
salinities as burial progressed. Goldstein (1986)
concluded that the deeply buried cements were
unlikely to provide any useful information
concerning original formation conditions, but
could prove useful for interpreting burial pore
fluid history. Barker & Goldstein (1990) used the
fact that inclusions in calcite reequilibrate
relatively easily to suggest that inclusions in
calcite from sedimentary basins and geothermal
fields might be used to estimate the maximum
burial conditions.
One misconception that many workers
have concerns the reproducibility of
microthermometric data as a means of testing
whether or not reequilibration has occurred.
Workers often report that homogenization
temperatures of inclusions are reproducible when
measured multiple times. These workers then
interpret this to indicate that the inclusions have
not reequilibrated. However, a reproducible Th is
necessary but not sufficient to prove that an
inclusion has not reequilibrated. As noted by
Bodnar & Bethke (1984), stretched fluid
inclusions in fluorite gave reproducible (±0.2°C)
homogenization temperatures, even though these
temperatures were ˜40°C higher than the Th
before the inclusions were stretched by laboratory
heating. Larson et al. (1973) also noted that some
inclusions in fluorite gave reproducible Th after
four heating runs, even though some of these
temperatures were as much as 70 degrees Celsius
too high (i.e., the inclusions had been stretched by
70 degrees Celsius). Thus, reproducibility of
homogenization temperatures is a necessary
criterion to confirm that inclusions have not
reequilibrated, but is not in itself sufficient to
prove that reequilibration has not occurred.
Compositional Reequilibration
Compared to volumetric reequilibration,
compositional reequilibration is less well
understood and more difficult to recognize. Most
compositional reequilibration involves the loss (or
gain) of hydrogen or water (OH-) from the
inclusion (Hall & Sterner, 1995). In melt
inclusion studies, other components, including
sodium and some trace elements, can be lost from
inclusions during heating. Melt inclusion
reequilibration is not considered here.
Pure carbon dioxide (or carbon dioxide-
rich) inclusions are common in medium- to high-
grade metamorphic environments. Based on
thermodynamic considerations, water-free (or
water-poor) fluids often are not in equilibrium
with the mineral assemblage in the rocks, and this
has led many workers to invoke post-trapping
reequilibration of the inclusions to explain the
high CO2 contents. Hollister (1990) has
suggested that CO2 inclusions in metamorphic
rocks are produced when water leaks out of
originally water-rich inclusions during plastic
deformation, to produce pure CO2 , or CO2 -rich,
inclusions. Bakker & Jansen (1991) were able to
reproduce this process experimentally. Water was
lost from H2 O-CO2 inclusions during
reequilibration, resulting in inclusions more CO 2 -
rich than the original inclusions. Alternatively,
Lamb et al. (1987) and Lamb (1990) suggested
that the "primary appearing" CO2 inclusions in
granulites were actually trapped during
retrogression and are not associated with peak
granulite grade conditions.
Owing to the small size of the hydrogen
ion, hydrogen is able to diffuse through most
mineral structures very easily. Mavrogenes &
Bodnar (1994) showed experimentally that fluid
inclusions several tens of micrometers beneath the
surface of a quartz crystal will reequilibrate to the
external hydrogen fugacity in only a few hundred
hours at 600-800°C, or in only a few tens of
thousands of hours (several years) at temperatures
of 400°C. As part of this work, these workers
were able to confirm that the common failure of
sulfide daughter minerals to dissolve during
heating is the result of post-entrapment hydrogen
loss from the inclusions. These workers were able
to reverse this process experimentally and
dissolve chalcopyrite daughter minerals - these
phases did not dissolve before hydrogen was
experimentally diffused into the inclusion at high
temperature and pressure. Hall et al. (1991)
attributed the presence of methane in fluid
inclusions from the Ducktown, Tennessee, USA,
massive sulfide deposits to hydrogen diffusion
224
into the inclusions during uplift and cooling. The
extremely negative hydrogen isotopic (D/H)
composition of the fluid inclusions was consistent
with enrichment in the hydrogen isotope, as the
larger deuterium diffuses through quartz at a
much slower rate. Hall & Bodnar (1990)
suggested that the small amount of methane often
reported in fluid inclusions from granulites is the
result of hydrogen diffusion into the inclusions
following trapping, consistent with
thermodynamic properties in the C-O-H system.
Hall & Sterner (1993) conducted
experimental studies of water loss from aqueous
fluid inclusions. As a result of water loss, the
salinity of the inclusions increased by 22 %.
Vityk et al. (2000) conducted similar experiments
and were able to increase the salinity by a few
tenths of a weight percent NaCl as a result of
water loss. Audétat & Günter (1999) noted
characteristic reequilibration textures associated
with fluid inclusions in quartz from the Mole
Granite, Australia, and attributed variable and
high salinities in the inclusions to loss of water to
produce "sweat haloes" around deformed
inclusions. It is likely that ranges in salinities of
apparently coeval inclusions in some magmatic
hydrothermal ore deposits, such as the porphyry
copper deposits, are due at least in part to water
loss from the inclusions following entrapment.
One could interpret the discussion above
to indicate that inclusions reequilibrate by an
increase in volume with no fluid loss (stretching)
or by loss of fluid through leakage or
decrepitation. In practice, these various
mechanisms of reequilibration likely operate
together, with perhaps one or the other
dominating, depending on the environment in
which reequilibration is occurring. Thus, Vityk et
al. (2000) note that stretching of fluid inclusions
in quartz requires the diffusive loss of fluid from
the inclusion into the surrounding quartz host to
initiate the stretching process. However, normal
petrographic observations would not reveal the
presence of water-bearing dislocations, and one
might assume that the change in homogenization
temperature was due solely to volume change.
Based on our experience and observations, we
believe that in all, or certainly most, examples of
reequilibration, both volume change and fluid loss
(or gain) occur. Possible exceptions might
include, for example, the reequilibration of "pure"
CO2 inclusions. Wanamaker & Evans (1989)
noted that following heating to generate high
internal pressures, the density of CO2 inclusions
in olivine had decreased. Assuming that CO2
cannot diffuse through olivine at these conditions,
these workers attributed the density decrease to
stretching (volume increase), in agreement with
their measurements of inclusion diameters before
and after heating.

Necking Down
Most fluid inclusions that we observe
today do not have the same shape as when the
fluid was originally trapped in the mineral.
Following entrapment in the host phase, most
inclusions change shape through a process
referred to as "necking down" that involves
dissolution and re-precipitation of the host phase
to reduce the surface area and produce many
smaller inclusions from the original larger
inclusion. For example, when a mineral fractures
during or after growth, some fluid may enter the
fracture as shown in Figure 8-10a. As necking
down proceeds, the fluid in the fracture becomes
isolated into progressively more and smaller fluid
inclusions. During this process, the inclusion
shape tends to become more regular. This process
is often referred to as maturation in the fluid
inclusion literature (cf. Bodnar et al., 1985). If
this process goes to completion, the former
fracture plane will be decorated by numerous
spherical or negative-crystal shaped fluid
inclusions, often showing a decrease in inclusion
size towards the original fracture tip (Fig. 8-10d).
If necking down occurs at the
temperature and pressure of trapping of the Fig. 8-10. Schematic representation of the
original fluid, the resulting inclusions will all formation of secondary fluid inclusions in a
show similar phase relations as well as fracture by necking down. Fluid enters the open
microthermometric behavior that is consistent fracture (a) and begins to dissolve material from
with the PTX trapping conditions. Indeed, the the walls and re -precipitate new mineral matter
process described above and illustrated in Figure to heal the fracture, isolating small pockets of
8-10 is identical to that used to trap synthetic fluid fluid in the process (b). With continued healing
inclusions according to the technique of Sterner & the originally irregularly shaped fluid inclusions
Bodnar (1984). Accordingly, fractured quartz (c) become more regular in shape and evolve
cores are placed into high temperature autoclaves through maturation to produce a plane decorated
along with a fluid of known composition. During by numerous negative-crystal shaped fluid
the constant-temperature experiment, fluid enters inclusions (d). (Modified from Roedder, 1962).
the fracture and the fracture heals as shown in down is simply the process by which inclusions
Figure 8-10 to produce numerous synthetic fluid mature and does not involve reequilibration of the
inclusions trapped at constant and known PTX type discussed in this chapter.
conditions. The microthermometric behavior of Inclusions that undergo necking down at
the resulting inclusions is consistent with the constant temperature and pressure, and in the one-
known formation conditions. In this case, necking phase fluid field, are of no concern in discussions

225
of reequilibration processes that lead to incorrect
microthermometric results. However, if the
temperature and/or pressure change during the
reequilibration process, or if two or more fluids ±
solids are present in the fracture during necking
down, the resulting inclusions likely will provide
incorrect compositional and microthermometric
data. Figure 8-11 is a schematic representation of
necking down in a decreasing temp erature system
in which phase separation to produce a vapor
bubble occurs during cooling. The original
inclusion at time T0 contains only liquid. During
cooling to temperature T1 a vapor bubble
nucleates in the inclusion. During cooling from
temperature T1 to T2 , the original inclusion necks
down to produce two inclusions. One inclusion
(inclusion a) contains the larger vapor bubble that
formed during initial cooling, and the other
inclusion contains only a small vapor bubble that
formed after the two inclusions were separated.
With continued cooling, the larger inclusion
undergoes necking down again to produce two
smaller inclusions, one containing the bubble that
was present at the moment necking occurred
(inclusion b) and the other (inclusion c)
containing a smaller bubble that nucleated after
necking during cooling from T2 t o T3 . At room
temperature (T4 ) the three inclusions show very
different liquid to vapor ratios, and would
homogenize at different temperatures. Thus, if an
FIA is comprised of inclusions that have
undergone necking down in a changing temper-
Fig 8-11. Necking down of an originally large,
liquid -filled inclusion (T0 ) to produce three
smaller inclusions. None of these inclusions
would record the correct formation temperature.
See text for details. (Modified from Roedder,
1962).
226
ature and/or pressure system, or in the presence of
two or more phases, the fluid inclusions will show
variable phase relations and a range in
homogenization temperatures. Such inclusions
should be avoided during microthermometric
studies if the goal is to determine the original P-T
formation conditions.
REEQUILIBRATION OF MELT
INCLUSIONS
Compared to fluid inclusions,
compositional reequilibration of melt inclusions is
much more common. Anderson (1974) was one of
the first to consider the reliability of melt
inclusions and the various post-entrapment
changes that might lead to reequilibration.
Nielsen et al. (1998) address the relative
advantages of microscope heating versus batch
heating of mineral grains to homogenize melt
inclusions, and also discuss volatile loss and
contamination of melt inclusions from alteration
products. Manley (1996) discussed the use of melt
inclusion morphology as an indicator of the
timing of inclusion formation during the eruption
event. Qin et al. (1992) developed a general
theoretical model for diffusive reequilibration of
melt inclusions, and applied this model to
evaluate water loss from melt inclusions
following entrapment, as well as reequilibration
of trace element concentrations in melt inclusions.
Gaetani & Watson (2000) evaluated Fe-Mg
exchange between melt inclusions and host
olivine, and Danyushevsky et al. (2000) provide
data from natural melt inclusions in olivine that
have reequilibrated by Fe-loss.
A complete consideration of the melt
inclusion reequilibration process is beyond the
scope of this chapter. The reader is referred to the
sources listed above, as well as references therein,
for a more complete discussion of this problem.
HOW TO AVOID LABORATORY RE-
EQUILIBRATION OF FLUID INCLUSIONS
For most fluid inclusions, compositional
reequilibration during laboratory studies is
unlikely if care is taken during data collection.
Exceptions include hydrogen loss (or gain) by the
inclusions during microthermometry and
compositional reequilibration of melt inclusions
during heating. The main type of reequilibration
that one has to be concerned with during
laboratory studies of most fluid inclusions is
volumetric reequilibration. Fluid inclusions tend
to reequilibrate volumetrically when the internal
pressure exceeds the strength of the host mineral
and, as noted above, this value depends on the
mineral hardness as well as the inclusion size and
shape and fluid composition. In most cases,
heating to some temperature above room
temperature (and above the homogenization
temperature) is required to generate pressures
sufficiently high to cause most inclusions to
reequilibrate. Low temperature (Th =150°C)
aqueous inclusions may also reequilibrate during
cooling studies to measure ice-melting
temperatures. In this case, formation of ice during
cooling, which occupies approximately 9 % more
volume than the liquid water it formed from, can
generate high pressures and cause the inclusion to
stretch. Lawler & Crawford (1983) coined the
term "freeze stretching" to describe this
phenomenon.
In the early days of fluid inclusion
studies, most polished sections were prepared
using Canada balsam or Lakeside cement or some
other adhesive that required the sample to be
heated to temperatures approaching 100°C. In
many cases, little care was taken to control this
temperature and samples may have been heated to
several hundred degrees to mount the sample on a
glass slide. Such high temperature would cause
fluid inclusions to stretch before they were placed
into the fluid inclusion stage, resulting in
erroneous microthermometric data. Today, most
workers take care to minimize heating of the
sample during polishing, and often use adhesives
such as Superglue that sets at room temperature
and requires no heating. In some extreme cases
involving very low temperature inclusions, the
samples must be stored in a temperature-
controlled room and transported in ice to avoid
stretching of the inclusions (c f. Wilson et al.,
2003).
Most workers believe that reequilibration
in the laboratory is not a problem as long as the
inclusions are not heated above the
homogenization temperature. This is because the
rate of pressure increase in the inclusion during
heating is much lower before the inclusion has
homogenized than it is after homogenization
occurs. And, for gas-free aqueous inclusions in
most minerals, the internal pressure is unlikely to
exceed a few hundred bars during heating, as long
as the homogenization temperature is below about
227
400°C. For higher homogenization temperatures,
the internal pressure can become sufficiently high
to reequilibrate inclusions in even some of the
more resistant minerals, such as quartz. For
example, a fluid inclusion containing a 25 wt.%
NaCl solution will have an internal pressure of
about 900 bars at a homogenization temperature
of 600°C (Bodnar & Vityk, 1994). According to
equation (1) above, this pressure is sufficient to
cause decrepitation of inclusions in quartz larger
than about 25 micrometers (Bodnar et al., 1989).
Many who study fluid inclusions from
medium- to high-grade metamorphic environ-
ments have experienced inclusion decrepitation
before homogenization occurs. This happens
because most inclusions from this environment
contain significant amounts of carbon dioxide,
resulting in elevated pressure in the inclusions,
even at room temperature. As an example, an
H2 O-CO2 inclusion containing 37 mole percent
CO2 and homogenizing at 263°C would have an
internal pressure of 2880 bars at homogenization
(Sterner & Bodnar, 1991). This pressure would
cause decrepitation of all inclusions larger than
about 3 µm in quartz (equation (1) above), and
any inclusions larger than this would decrepitate
during heating, before the homogenization
temperature is reached. Schmidt et al. (1999)
described application of the Hydrothermal
Diamond Anvil Cell as a pressurized fluid
inclusion stage to eliminate (or minimize)
decrepitation of high pressure inclusions during
heating to homogenization.
In some cases it may simply not be
possible to heat (or cool) a fluid inclusion without
causing reequilibration to occur. Not every fluid
inclusion is able to provide useful
microthermometric data. What is most important
to the fluid inclusionist is to be able to recognize
inclusions that reequilibrate during laboratory
studies. This can best be accomplished by
following one simple rule during microthermo -
metric analysis: Thou shalt collect no data from
any fluid inclusion that has not been observed
continuously during the very first heating (or
cooling) run. If one obeys this rule, the
probability of collecting data from inclusions that
have reequilibrated during laboratory analysis is
significantly reduced.
ACKNOWLEDGEMENTS
Much of the information presented in this
chapter represents studies by former students and
post-doctoral researchers and visitors to the Fluids
Research Laboratory. I wish to acknowledge Don
Hall, Mike Sterner and Max Vityk for their many
contributions that helped me to better understand
the reequilibration process. I also give special
thanks to Phil Bethke and Ed Roedder for
encouraging me as a student to pursue this
important area of fluid inclusion research. Alan
Anderson, Will Lamb , Iain Samson and one
anonymous reviewer are thanked for their
comments and suggestions for improving the
manuscript. The National Science Foundation,
Department of Energy, NASA, and the American
Chemical Society have supported work in the
Fluids Research Laboratory over the years. NSF
Grants EAR-0001168 and EAR-0125918
provided support during preparation of this
manuscript.
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