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Petrographic analysis of fluid inclusions

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CHAPTER 2: PETROGRAPHIC ANALYSIS OF FLUID INCLUSIONS
Robert H. Goldstein
University of Kansas
Department of Geology
1475 Jayhawk Blvd., 120 Lindley Hall
Lawrence, Kansas 66045, USA
gold@ku.edu
INTRODUCTION
Chapter 1 of this volume (Bodnar 2003a)
introduced the subject of fluid inclusion research
and dealt with the various processes that lead to
the entrapment of fluid inclusions. This chapter
deals with the practicalities of petrographic
observations that can be made in a fluid inclusion
study. Careful attention to petrography, in a fluid
inclusion study, can prevent many of the mistakes
typically made by neophyte inclusionists and can
save oodles of time and wasted journal space in
the long run, protecting researchers from pursuing
the wrong path in a research project. This chapter
organizes strategies for beginning a fluid
inclusion study, discusses the pitfalls and
problems typically faced within the first parts of a
fluid inclusion study, and concentrates on what
should be accomplished before microthermo -
metry is attempted. The chapter relies heavily on
the previous work of many excellent researchers,
as summarized by Roedder (1984), and includes
the modified approaches developed in Goldstein
& Reynolds (1994). It is not designed to do all
things relating to petrography and does not
attempt a complete literature review of the
subject, but is designed as an introduction to the
subject of fluid inclusion petrography in keeping
with the goals of this volume. It also refrains
from interpreting the specific geologic
environments of entrapment and reequilibration
of fluid inclusions interpretable from petrography
alone (e.g., Roedder 1984, Goldstein 1993,
Goldstein & Reynolds 1994, van den Kerkhof &
Hein 2001, Diamond 2001). These subjects are
reserved for later chapters (Bodnar 2003b, 2003c,
Diamond 2003a, 2003b, Anderson 2003, Burruss
2003) where necessary phase equilibria are
introduced.
Normally, petrography is regarded as the
most important part of any fluid inclusion study.
The reason for this is that geology, as a science, is
an historical one, and at the most basic level,
petrography is how we put the pressure,
1
temperature and fluid composition data, attainable
from fluid inclusions, into an historical context.
This means that the most basic objective of any
fluid inclusion study must be to determine the
timing of entrapment of fluid inclusions. Fluid
inclusions may be entrapped during or after
mineral growth. Obviously, those inclusions
trapped during minera l growth are those most
likely to be representative of the conditions of
mineral growth and those trapped after mineral
growth may record later conditions. Most
geologic samples, however, consist of an
assemblage of various minerals that have grown
and recrystallized at different times, and each
crystal may consist of many growth zones,
recording many events of mineral growth spread
out over geologic time. When minerals are
fractured, deformed or recrystallized, it is
common for fluid inclusions to be trapped after
mineral precipitation. Individual samples may
record hundreds or even thousands of events of
fracturing and subsequent fluid inclusion
entrapment. Clearly, if the entrapment of fluid
inclusions can be put in sequence, then a detailed
history can be interpreted that will help the
researcher in interpreting a detailed geologic
history of a set of samples. Thus, for most
studies, the researcher must establish cross-
cutting and superpositional relationships for the
mineral paragenesis and for fluid inclusion
entrapment.
Groups of inclusions that can be defined,
by petrographic means, as the most finely
discriminated events of fluid inclusion entrapment
are called fluid inclusion assemblages (Goldstein
& Reynolds 1994). The fluid inclusion
assemblage approach is discussed in detail at the
end of this chapter. As an approach to fluid
inclusion work, it replaces previous methodologies
in which fluid inclusions were treated as
populations of data to be treated statistically. It is
only by defining fluid inclusion assemblages that
the geologic history can be ascertained from a set
of samples. Fluid inclusion petrography and the
identification of fluid inclusion assemblages is
also the most important approach for evaluating if
fluid inclusions have been altered significantly
after their entrapment, though necking down after
a phase change (Bodnar 2003c) or through
thermal reequilibration (Bodnar 2003c).
Petrography is the easiest method for
evaluating how many fluid phases were present at
the time of fluid inclusion entrapment, and under
what conditions of pressure and temperature
inclusions were entrapped. These techniques will
be covered in later chapters (Bodnar 2003b,
2003c, Diamond 2003a, 2003b), after the phase
equilibria of fluid systems has been presented.
Moreover, simple petro graphic approaches are the
easiest for identifying fluid compositions. It is
remarkable how much information one can glean
about the history of pressure, temperature, and
composition of fluids with just a good
petrographic microscope (Goldstein 1993).
The results of the petrographic part of a
fluid inclusion study are an essential part of
almost every application of fluid inclusion
research. Thus, most research papers using fluid
inclusions should have a petrography section,
presenting the overall paragenesis, evidence for
timing of entrapment of fluid inclusions, fluid
inclusion assemblages, phases observed and their
distribution. Unfortunately, petrography is the
part of the study that is commonly, albeit
mistakenly, given short shrift by some
researchers, significantly weakening their stories.
In a fluid inclusion research project,
petrography is commonly the part of the study
that takes the most amount of time and requires
the most objectivity. It is normally the part of the
fluid inclusion study in which researchers
evaluate whether or not they have the fluid
inclusions necessary for answering the particular
questions posed at the beginning of the research.
After spending time doing a fair amount of
petrography on a sample, we sometimes "bail out"
of the study because the inclusions needed to
answer the problem are just not there or are too
small to work with. In practice, the petrographic
part of a fluid inclusion study requires patience,
sometimes a bit of stubbornness, and often times
the spirit of a gambler. Time is what you are
gambling; after searching twenty samples and
finding no useful fluid inclusions, one always
2
wonders about number twenty-one. Is that the
one that will have the beautiful fluid inclusions
you need?
SAMPLING PHILOSOPHY
The philosophy behind taking samples
for a fluid inclusion study begins with an
understanding of the scientific question that has
been posed in the study. This scientific question
commonly is posed even before the samples have
been examined petrographically. When the
scientific question has been defined specifically,
it tends to govern how sampling proceeds.
How sampling is approached will be
dictated, to some degree, by the scope of the
proposed study. For example , a large regional
study will require a different approach than a
local study, but for almost all studies, sampling
must be done with the paragenesis in mind. All
researchers must strive to sample cross-cutting
and superpositional relationships in the field or
from hand specimens. Examples typically
include various cross-cutting relationships
derived from fracture-fills, simple centripetal
filling of cavities with space-filling mineral
phases, mineral phases cross-cut along clast
boundaries, and cement stratigraphic relationships
(Meyers 1974; Goldstein 1990) in which the
chemical zonation of mineral phases can be
correlated and compared to specific stratigraphic
surfaces or geologic events.
In some studies, the scientific question
posed requires that the spatial distribution of
samples be even more important than paragenesis.
For example, many studies may choose to
compare the thermal history of the hanging wall
to the footwall in deformed successions. Samples
taken in close and distant proximity to a particular
fault may be the key that identifies the conditions
of faulting. Oriented samples may need to be
taken to identify fabrics associated with particular
phases of deformation interpreted from the
regional and local geology. Samples taken above
and below diagenetically important stratigraphic
surfaces, such as unconformities or surfaces of
evaporation likewise are important. Vertical or
lateral sampling through a succession may serve
to delineate the temperature, pressure or
compositional gradients that were present in the
system.
In practice, sample selection may
involve searching tens or even hundreds of
samples before the appropriate fluid inclusions
are found to solve the scientific question posed.
A researcher can increase the likelihood of
finding workable fluid inclusions by sampling the
more coarsely crystalline phases, and by looking
for areas of cloudiness in the crystals before
polished sections are prepared. Most fluid
inclusion researchers realize, however, that there
is an aspect of luck involved in fluid inclusion
work, and that sometimes we are lucky and find
the samples with the inclusions we need right
away; at other times, we may never find the
inclusions we need to answer the research
question posed.
Thus, the number of samp les required
probably will be different for each study. Some
fluid inclusion studies may only require a single
sample. Others may require hundreds before the
question posed can be answered, and for other
studies, there is no number of samples large
enough to answer the question posed because the
necessary inclusions are just not there.
Sample selection caveats
Most rock and mineral samples are just
fine, but some types of samples simply are not
appropriate for a fluid inclusion study. Such
samples should be avoided at all costs as they
typically will provide ambiguous results.
Inclusions that have experienced significant
amounts of overheating in the laboratory or on
outcrop, typically are not appropriate for fluid
inclusion study, because the heating process may
have destroyed or reequilibrated the fluid
inclusions. Likewise, some samples that have
experienced prolonged deep-freeze conditions on
outcrop may also be altered, because some
aqueous inclusions tend to leak after they have
been frozen.
Samples to be avoided are those that
have been altered by heating on outcrop or though
some laboratory treatment. For example, one
should avoid well cuttings in which the drying
procedure is unknown. Most cuttings from oil
and gas wells have been dried at unknown
conditions. Unless the inclusionist was on the
well site to collect the samples, or if samples had
never been dried, it is normally best to avoid well
cuttings altogether. Many inclusionists tend to
work with oil and gas industry drill core. There is
a trend, however, to analyze entire core segments
for porosity and permeability as opposed to the
3
small plugs that most researchers are accustomed
to. The process of "whole-core analysis" or "full-
diameter analysis" typically heats the core sample
to between 110°C and 230°C. More recently, a
lower temperature treatment has been made
available that prevents such heating of cores.
Samples of core that have been through whole-
core analysis can be recognized even if the
records on what has been done to the core have
been lost. Typically, core segments that have
been analyzed have been sawn into six-to-ten-
inch segments with saw cuts perpendicular to the
core. The sawn ends may be marked with an "X"
and some notations. Large vugs may be stuffed
with wadding. Core segments that have been
analyzed may have a different color than those
that have not been analyzed. Plugs that have been
taken for porosity and permeability analyses have
also been heated and should also be avoided.
Many inclusionists wonder if old thin
sections and thin-section rock blanks can be used.
Unfortunately, the answer to this is no in most
cases. Almost all old thin sections and thin-
section blanks have been heated on a hot plate
during preparation, and this may have
reequilibrated the fluid inclusions. Likewise,
resin-impregnated samples may have been heated
to cure the impregnation medium and should be
avoided unless the procedure for curing is known
to have been held at low temperature. Further,
any thin section or rock blank that has been acid
etched for staining typically will have lost most of
the fluid inclusions. Acid etching appears to
attack the sample in such a way as to
preferentially breach inclusions. So, can old thin
sections be used at all? Although the answer to
this question is generally no, we have used old
thin sections for high-grading samples that might
contain the fluid inclusions appropriate to answer
the scientific question posed in the study, and to
help work out the overall paragenesis. This has
saved time and money in the long run, reducing
the number of specially prepared samples for
fluid inclusion analysis.
Samples that have been subjected to
electron-beam imaging should also be avoided if
possible. It is well known that samples that have
been studied in optical-stage-mounted cold and
hot cathodoluminescence systems have been
heated significantly (Barker 1992). Similarly,
samples that have been in a scanning electron
microscope or electron micro probe also may have
been damaged, but this depends very much on the
operating conditions used in the work.
A sample from a poorly chosen outcrop
could produce fluid inclusions that have
reequilibrated. For example, we have found that
roasting in the sun can reequilibrate low-
temperature fluid inclusions in soft minerals like
gypsum. Similarly, outcrops can be scorched by
forest or grass fires, heating the outermost parts of
the outcrop and reequilibrating some fluid
inclusions. Some low-temperature and low-
salinity fluid inclusions may even freeze with
extremely cold outcrop climate, causing many
inclusions to leak.
In conclusion, it is clear that sample
selection is an important part of any fluid
inclusion study and must be given careful
consideration. In all cases, the scientific question
posed in the study must be considered. Samples
must be taken in the paragenetic and geologic
context necessary for answering the question
posed. The possibility of alteration of the fluid
inclusions also must be considered.
SAMPLE PREPARATION
Fluid inclusions are small and easily
breached through heating or fracturing of the
sample. Thus, preparation techniques must be
gentle ones in which samples are handled
carefully and treated as fragile objects.
Moreover, optics in the sample must normally be
optimized so that the tiny fluid inclusions can be
resolved. Preparation techniques may include
creating cleavage fragments, "quick plates" or
doubly polished thick sections (polished plates).
Techniques of preparation are designed to avoid
heating the sample or deforming it mechanically.
Doubly polished thick sections
Most fluid inclusion petrography is done
on doubly polished thick sections. Polishing both
the upper side and lower side of thick sections of
rock samples can greatly improve optics.
Thickness can be adjusted to maximize optics of
the particular size and orientation of the fluid
inclusions in a sample. There are eight tasks
required for preparation of doubly polished
plates: (1) impregnation of the rock sample; (2)
cutting the rock sample down to size; (3) grinding
the surface to be mounted; (4) polishing the
surface to be mounted; (5) mounting the polished
rock to glass; (6) cutting the rock billet off of the
4
glass; (7) grinding the mounted rock down to
proper thickness; and (8) polishing the surface of
the thick section.
Doubly polished thick sections – Impregnation
Many porous rock samples will have to
be impregnated to achieve stability during cutting,
grinding, and polishing to prevent plucking of
mineral grains and to prevent pore spaces from
trapping grit. Well-indurated, low-porosity
samples will not require any impregnation at all.
Impregnation should be avoided in samples that
will require microthermometry above 250°C
because most epoxies will start to degrade at
temperatures near 200°C.
Most impregnation uses epoxy resins.
These typically come in clear forms but a dye
may be added to make the resin more visible
under the microscope. Effective impregnation
can be aided by pumping and releasing a vacuum
to draw the epoxy into the pores. Any
impregnation technique that involves heat or high
pressure should be avoided, however. High-
pressure impregnation techniques generate
fractures that can produce an exploded texture,
making petrographic analysis difficult. High-
temperature-curing epo xies could cause thermal
reequilibration of fluid inclusions. Cold-curing
epoxies used with vacuum impregnation seem to
work in most cases. Only small quantities of
epoxy should be mixed for impregnation to avoid
severe exothermic reactions that could cause
reequilibration of fluid inclusions. For cold-
curing epoxies, complete curing may take several
days.
Doubly polished thick sections – Cutting
The rock sample is sawn twice, once for
shaping the rock billet to be mounted on the glass,
and then again to cut the rock sample off the glass
backing, leaving a thin plate of rock to be ground
and polished later. Cutting of rock samples
typically uses a liquid-cooled diamond rotary
saw. With all sawing of hard brittle materials,
there is a significant risk of thermal or mechanical
damage that must be managed. Diamond rotary
saw blades work by grinding a slot through the
sample rather than slicing the sample. Thus, to
avoid significant heating during cutting, such
blades must use ample liquid coolant and the
sample must be advanced slowly. Some high-
speed trim saws tend to batter the sample badly
and may produce multiple fractures that induce
leakage of fluid inclusions. To avoid this, some
precision high-speed trim saws may be adjusted
so that the blade will neither wobble nor bounce.
If the saw cannot be adjusted, advance the sample
more slowly or leave a little extra rock to be
hand-ground off of the sawn face until the
damaged area has been removed. The best
alternative to typical rock and cutoff saws is to
use a low-speed trim saw. Low-speed saws
produce almost no damage to samples, but they
have one severe drawback, they may take more
than half an hour to make a single cut.
Doubly polished thick sections – Grinding
The grinding procedure must be done
twice; once to prepare the billet for polishing and
mounting, and then again to achieve the proper
thickness of the thick section and to prepare it for
polishing. The first coarse grinding step should
remove at least 0.5 mm from any face of the rock
that has saw-blade marks. Progressive steps of
fining of grit size should remove all scratches
from the previous grinding step. Remember, do
not push hard on a sample during grinding. Some
commercially available thin-section lapping
machines use cut diamo nd disks and a micro-
meter-driven armature that is passed back and
forth over the diamond disk. The greatest source
of damage to thick sections is from feeding the
sample into the diamond disk too rapidly,
inducing fractures which damage fluid inclusions.
So remember, if using such equipment, go slowly.
Grinding on a flat lapping wheel, with a
slurry of loose carborundum grit, works fine.
Grinding by hand, with wet carborundum
sandpaper, mounted on a flat surface, can also
work well, but it is time consuming. In both
cases, the sample must be ground with
progressively finer grits, and must be cleaned
thoroughly to avoid contamination.
Diamond-impregnated laps also may be
used for grinding the sample. This equipment
cuts using sharp tips of protruding diamonds,
producing relatively large fragments of rock that
have been removed from the surface being
ground. If these fragments are not immediately
removed from the lap, the surface being ground
will tend to get scratched by the rock fragments.
To keep these fragments from scratching the
surface, use a hard, steady, stream of water on the
lap. Keep the lap rotating at 700 to 1000 revol-
5
utions per minute for best results.
After the final grinding step on the thin
section billet (about a 15 µm-sized diamond
abrasive or 1000 grit carborundum abrasive), the
surface should be free of visible scratches, and it
may even appear to have the beginnings of a
satin-like semi -polish. Once this satin semi -
polish is achieved, the rock sample can be cleaned
thoroughly and can then go to the polishing step
before mounting.
A similar satin semi -polish should be
achieved before polishing the thick section,
however, before finishing the grinding step, an
immersion liquid and cover slip should be applied
to check the samp le’s thickness under a
petrographic microscope (see quick plates below).
It is best to repeat this procedure many times
during the grinding processes before the proper
thickness is achieved, as it is easier to grind off
rock than to put it back on.
Many commercial thin-section pre-
paration labs ask researchers what thicknesses
should be used in preparation of polished sections
for fluid inclusions. This question is essentially
impossible to answer. There is no such thing as a
single appropriate thickness because inclusion
sizes range widely and clarity of mineral phases is
variable. Sections prepared to a single standard
thickness are either too thick, making petrography
difficult, or they are too thin, and most of the
fluid inclusions have been breached. Thus, it may
be difficult to have fluid inclusion samples
prepared using commercial labs. Normally, we
prepare fluid inclusion sections "in house" and
repeatedly check the sample thickness during the
grinding process.
Doubly polished thick sections – Polishing
The thick section must be polished on
both sides, which means that the polishing
procedure must be done on the rock billet before
it is mounted and on the surface of the doubly
polished thick section once it has achieved
appropriate thickness.
After an even, satin semi-polish has been
achieved during the grinding procedure, the rock
surface can be polished. Many labs use loose
diamond abrasives of various sizes on a felt lap or
use bonded diamond abrasives on a substrate.
High-speed laps at 1000 to 2000 revolutions per
minute work well. Rapid polishing with loose
diamond abrasives normally requires great
pressure to the surface to obtain results in a
relatively short time. This can be counter-
productive when attempting to polish rocks with
minerals of variable hardness, because the soft
minerals typically are gouged or undercut
producing an uneven surface. Rocks composed
of soft minerals can be polished in less than 2
minutes with a single polishing step of 3 µm or
less. Rocks with hard minerals normally are
polished in 3 steps (10-6 µm, 3 µm, and 1 µm).
Fluid inclusion samples require excellent
polishes. To evaluate the quality of the polish
quickly, hold the polished rock surface opposite
to the top surface of an incandescent light bulb.
Tilt it in such a way that the reflection of the light
bulb is visible. If one can read the writing on the
bulb in the reflection, the polish is probably fine
for most fluid inclusion work.
Doubly polished thick sections – Mounting
Before mounting the polished billet of
rock to a glass backing, the polished surface must
be washed well with acetone, alcohol, or a
detergent solution. Either frosted or unfrosted
thin-section glass can be used, but polished rock
surfaces typically stick best to frosted glass. In
all cases, the polished sample and thin-section
glass must be checked for flatness before
mounting.
Three approaches can be used for
mounting the polished rock sample to the glass
backing:
(1) Many researchers use a mounting glue that
can be dissolved later, because they intend to
remove the doubly polished thick section before
subjecting it to microthermometry. Most use any
of the superglues (cyanoacrylate) for this because
they are soluble in acetone. Others, unconcerned
about heating the sample, use a variety of resins
and waxes that require heating. There are several
reasons why inclusionists would use a removable
mounting glue. Hard-rock geologists typically
heat fluid inclusion samples to temperatures
above 200°C for microthermometry. As
mounting resins develop a dark color at such high
temperatures, optics are negatively affected by the
mounting resin. Moreover, some fluid inclusion
heating/freezing stages employ principles of
thermal conduction in their operation. For these
stages, thin chips of flat polished rock should be
used. To remove the polished thick section from
the glass backing, cyanoacrylate glues should be
6
immersed overnight in acetone. For the more
durable polished thick sections, remain ing glue
can be removed from the polished rock surface by
delicately rubbing it over acetone-soaked paper a
few times. For more fragile thick sections,
dissolution of the glue may cause disintegration
of the rock, making subsequent work difficult.
For such low durability samples, either method
(2) or (3) would be appropriate.
(2) Many researchers prefer to leave the
polished thick section mounted to the thin-section
glass. For this approach, the standard thickness
thin-section glass remains permanently attached
to the polis hed thick section and makes for a
highly durable, but thick sample. This technique
is most appropriately applied if samples are not to
be heated above about 200°C for micro-
thermometry and if a gas flow stage is to be used
in which thermal gradient effects are not an issue.
Petrographic epoxies that cure with UV light
work well for permanent mounting. They seem to
be very strong and do not require heat for curing.
(3) A few researchers prefer a double-mounting
procedure in which the rock is mounted onto a
thin piece of cover slip glass with permanent UV-
curing epoxy; the cover slip glass is temporarily
mounted on standard thin-section glass with
cyanoacrylate. This method allows the polished
rock sample and cover slip combination to be
removed from the thin-section glass as a unit. It
results in a polished thick section made more
durable by having a backing of cover-slip glass.
The sample is thin enough to be used in a thermal
conduction stage, but it still suffers from the
problem of not being able to be heated above
about 200°C for microthermometry.
Cleavage fragments
Cleaving mineral fragments is a "quick
and dirty" method for producing thin chips of
mineral with parallel sides. Chips must be
cleaved cleanly to produce reasonable optics for
fluid inclusion observations. In some minerals, a
well-cleaved surface produces a natural "polish"
essentially free of pits and irregularities. Further,
there is no preparation technique gentler then
making cleavage fragments. To produce these
chips, simp ly cleave fragments from a coarse
single crystal of a mineral specimen with a razor-
sharp blade. Aim to produce a thin chip with
parallel walls. This technique can be used
effectively on cleavable minerals with particularly
large crystals, such as calcite, dolomite, halite,
fluorite, gypsum and anhydrite. Although
cleavage fragments have a great advantage over
other techniques in ease of preparation and
potential for preservation of fragile inclusions, it
is quite difficult to work on cleavage fragments
and to retain the necessary paragenetic framework
essential for most fluid inclusion studies.
Quick plates
A "quick plate" can be prepared as a
time saver. Quick plates are thick sections
prepared with the same procedures as those
described for doubly polished thick sections,
except that the final polish is not applied. Instead,
once an appropriate thickness is achieved, an
immersion oil, with a similar index of refraction
to the mineral studied, is applied to the upper
surface. Immersion oil with index of refraction of
about 1.51 works for many common minerals;
kerosene is used commonly for fluorite, and some
carbonates require an oil with a refractive index
of 1.60. The oil on the upper surface creates a
pseudo-polish that will allow the sample to be
examined petrographically. The presence or
absence of fluid inclusions can be noted. If fluid
inclusions appear to be present, a final polish can
be applied. If inclusions are not present, the
FIG. 2-1 –Photomicrograph illustrating pseudo-inclusion composed of epoxy resin (arrow). Note dark
color of inclusion reflecting blue dye in epoxy resin. Sample composed of calcite in modern beach
rock from St. John, USVI.
7
researcher can move on to other materials and can
save the time of the polishing step.
Pseudo-inclusions
Many mineral samples have
microporosity or microfractures that can be filled
or partially filled with one of the many liquids
used during sample preparation. In many cases,
these partially filled cavities may have an
appearance just like that of a real fluid inclusion,
however, rather than being filled with geological
fluids, they are filled with uncured or poorly
cured resin, solvent, aqueous liquid, or oil-based
cutting coolants (Fig. 2-1). These pseudo-
inclusions may appear to be no different from any
other fluid inclusion at room temperature,
commonly containing a small bubble and
dominant liquid phase. When heated, the bubble
may homogenize and the pseudo-inclusion may
be mistaken easily for a natural fluid inclusion.
Normally, pseudo-inclusions can be
recognized for what they are. Over time or over
many heating runs, the inclusions tend to leak.
During cooling runs, the solvent and resin-filled
inclusions exhibit behavior inconsistent with
aqueous fluids, with the bubble slowly growing
and deforming during cooling. The best method
available
to distinguish between natural fluid inclusions
and pseudo inclusions, however, is to modify
preparation techniques. The addition of dies to
impregnation resins, glues and cutting oils (Fig.
2-1) works well, as does the use of UV-
fluorescent liquids during sample preparation
(Dutkiewicz & Ridley, 2003).
IMAGING APPROACHES
Thorough petrographic analysis of a
sample containing fluid inclusions normally
requires extensive transmitted-light microscopy.
Transmitted light microscopy is used most
commonly in identifying the origin of fluid
inclusions and the phases present. In recent
years, however, other petrographic approaches
have proven to be essential components of many
fluid inclusion studies. These include back-
scattered electron imaging, cathodoluminescence
imaging, EDS/ WDS-element mapping, UV epi-
illumination, laser confocal scanning microscopy,
and infra-red microscopy.
Transmitted-light microscope
Most fluid inclusion petrography
requires long hours using a transmitted-light
microscope. The setup and adjustment of this
microscope is all important in doing good
petrographic work on fluid inclusions, because
fluid inclusions are typically tiny, irregular in
shape, and buried within cloudy minerals.
Normally, a good fluid inclusion
microscope has a binocular head or trinocular
head. Usable oculars are 12.5X, 15X, or 16X, or
use 10X oculars with a 1.25X or 1.6X
magnification changer. Commonly it is useful to
have a video camera attached to the trinocular
head and a monitor set up next to the microscope.
Analog and some digital cameras work well, but
beware of digital cameras that give a jumpy or
blurred image in real-time video. Objectives
should include a 2X or 4X for low-magnification
work and a 10X objective for scanning samples
for fluid inclusions. A 40X or 50X objective
works well for more detailed observations on
fluid inclusions. Doubly polished thick sections,
prepared for fluid inclusion work, will not have a
cover slip, so be sure to buy your high
magnification objectives without a cover slip
correction or with a variable correction collar
adjustment. For work on a heating/ freezing
8
stage, special high-magnification 32X to 100X
objectives will be used and they will need to be
matched with a long-working-distance condenser.
A biological-style X-Y stage is a useful modific-
ation for most microscopes, allowing for rapid
scanning of polished thick sections. A high-
intensity quartz halogen light source is normally
required, thus, most student-grade microscopes
and old microscopes are not very good for fluid
inclusion work. This light source should be
adjusted properly, so that the filament is centered
and properly focused. Either a rotatable analyzer
or polarizer will be necessary to eliminate double
refraction in some minerals, particularly
carbonates. Strain-free optics normally are not
essential for most fluid inclusion work.
Doing transmitted-light microscopy
Once you have prepared doubly polished
plates, you may find it useful to make a map of
the polished section. Do this digitally by
scanning the thin section on a flat bed or slide
scanner with a transmitted light or transparency
attachment. Excellent, inexpensive scanners with
transmitted light sources are commercially
available. An inexpensive color printer can be
used to make an excellent paper map of the
polished thick section on to which you can record
spatial information on occurrence of fluid
inclusions.
Take care of your polished thick sections
as they are stored. Be sure they have not been
heated. You might even consider storing your
samples in a refrigerator to encourage nucleation
of bubbles in metastable fluid inclusions.
Once you sit down at the microscope to
work with your doubly polished thick sections, be
sure to get into the habit of adjusting your
microscope as the first thing you do. Normally,
keep the rotatable analyzer in the path at all times
and remove the polarizer. That way, any strain in
the optics does not lead to birefringence. In
carbonates or other minerals that show strong
double refraction, one of the images can be
eliminated by rotating the analyzer. The ordinary
ray will produce the best image.
For high-magnification objectives, the
microscope must be adjusted to produce
convergent illumination by inserting the flip-in
condenser cap. Initial adjustments are made with
the condenser (iris) diaphragm fully open. Go to
one of the lower-magnification objectives at first
and focus the microscope on your sample. Then,
close down the field diaphragm (below the
substage). Adjust the focus of the substage
condenser up and down until you can see the
straight polygonal sides of the iris image. Then,
use the two centering screws on the substage to
move the image to the center of the field of view.
This illumination is commonly referred to as
Kohler illumination. Now, open the field
diaphragm to fill the field of view and adjust the
iris diaphragm on the substage to achieve the
contrast you like. Be aware that normally, the iris
diaphragm is left close to wide open, but this is a
matter of personal preference. If the iris
diaphragm has been closed too much, the
inclusions will appear to have too much contrast.
Once all of these adjustments have been made to
the illumination on the mic roscope, you are good
to go.
When studying polished thick sections,
remember that it is best to scan initially at lower
magnification to get an idea of the overall
paragenesis. Fluid inclusions normally will be
observable using the 10X objective. Studying
fluid inclusions at this low magnification is most
helpful in evaluating where the largest and most
common inclusions can be found. It is also useful
in evaluating the distribution of fluid inclusions in
a sample to determine their origin and timing of
entrapment. You will need to use higher-
magnification objectives to see the fluid
inclusions in more detail and to evaluate the fluid
and solid phases present.
As a beginning fluid inclusionist, beware
of several significant pitfalls. Many beginners
have a tendency to focus on the top of the
polished thick section rather than deep within it.
Of course, not a single fluid inclusion should be
identifiable on the top surface of the polished
thick section, as inclusions are preserved only
when totally sealed within an enclosing mineral.
In some cases, beginners misidentify pits in the
polished surface as fluid inclusions, even finding
things that look like bubbles. Some have even
attempted to base entire studies on those pits, only
to find out that when heated or frozen, no phase
changes were observable. For those new to
inclusion work, it is best to change the focus on
the microscope so that they can resolve the upper
surface, then change the focus downward to
resolve the lower surface. All inclusions should
9
be at levels of focus between the two surfaces;
and objects that are resolvable on them are
probably not fluid inclusions. To get some
practice, it is a good idea to cut a polished thick
section of something likely to have fluid
inclusions (like quartz in granite) and then
practice a few times until you are sure you know
what fluid inclusions should look like.
Other beginning fluid inclusionists tend
to make the mistake of searching for only one
type of fluid inclusion, but this common mistake
comes from inexperience, not knowing the tre-
mendous variety of inclusions that might be found
in a particular sample (Fig. 2-2). For example,
many beginners tend to tune their eyes to find
only negative-crystal-shaped inclusions contain-
ing a liquid phase and a small bubble, commonly
dancing around the inclusion interior in pseudo-
brownian motion. They soon learn that fluid
inclusions may come in all sizes and shapes and
may contain a variety of observable fluid and
solid phases. Some may contain only a single
fluid phase, and that phase may appear bright or
dark in transmitted light. The inclusion may
appear to be full of gas, or the gas phase may
dominate the inclusion, with only a tiny rim of
liquid remaining. The inclusion may be all liquid,
or the liquid may dominate the inclusion, sharing
the vacuole with a small bubble. Three immisc-
ible fluid phases are quite common in inclusions,
and solid phases also may be found. Thus, some
of the best advice available for beginning
inclusionists is to learn as much as possible about
the various types of inclusions. This chapter is
meant merely as an introduction to this endeavor,
and each inclusion researcher should become
familiar with the body of literature available in
their particular field of fluid inclusion research.
Transmitted-light microscopy with the spindle
stage
A transmitted-light microscope, with
rotating stage, can be outfitted with a spindle
stage to provide three-dimensional information on
fluid inclusion distribution, shape, and volume
(Anderson and Bodnar 1993). A spindle stage
that is designed for fluid inclusion work, consists
of a horizontally mounted goniometer and spindle
on to which a small (normally less than 1 mm)
mineral sample is mounted. The mineral sample
sits in an oil-immersion cell, and it can be viewed
through the microscope optics as it is rotated 360°
FIG. 2-2 – Photomicrograph illustrating the wide variety of inclusion types potentially observable in a
single field of view in quartz. The dark cloudy material consists of hundreds of fluid inclusions, some of
which were trapped during growth of the host crystal and others which were trapped during many events
of microfracturing and healing. Sample donated by A. Lacazette. Lemont diamonds, vein-filling quartz
crystals, Pennsylvania.
around a vertical and horizontal axis. This three- entrapment of fluid inclusions just below the
dimensional view affords the inclusionist an surface imaged. The BSE technique is a gray-
opportunity to improve volume estimates over scale image of the polished surface of a mineral
those made from two-dimensional analyses. specimen, producing a spatial representation of
Measurements can be made on shape and size of average atomic number in the mineral, with high
an inclusion, as well as on the solid, gas, or liquid atomic number appearing bright and low atomic
phases within it. The orientation of inclusion number appearing dark (Fig. 2-3). As the image
shapes and planar arrays of inclusions can be is produced in the SEM, the resolution can be
measured with respect to micro- or high, easily capable of resolving sub-micrometer-
macrostructural features, and optical or scale growth zoning and fracture fills.
crystallographic orientation. Such measurements Pieces of polished thick sections work
may prove useful for fracture studies and for well for this type of imaging. Normally, samples
distinguishing between primary and secondary must be mounted onto an electrically conductive
fluid inclusions. stub and coated with a conductive film such as
carbon or gold. BSE images easily show contrast
Back-scattered electron imaging between different minerals, but the most useful
Back-scattered electron (BSE) imaging images are those produced by examining the
can be accomplished on a scanning electron textures observable by imaging the compositional
microscope or electron microprobe outfitted with variation within a single mineral crystal.
a separate back-scattered electron detector. The Because of their compositional variability, we
technique is not used to image fluid inclusions have had great success in imaging carbonate min-
because it images the surface, but it may be erals using this technique. To make such images,
essential in determining the timing and origin of the operating conditions must be set to maximize

10

FIG. 2-3. Back-scattered electron image of
baroque (saddle) dolomite illustrating
compositional zoning in the crystal.
Courtesy of K. Wojcik. Pennsylvanian of
Kansas.
contrast. At lower magnifications, the best
images are produced by using the largest aperture
available (120 micrometers is common) to maxi-
mize the energy hitting the sample. To achieve
sharp focus at higher magnifications, smaller
apertures will have to be used and the brightness
and contrast may need to be adjusted accordingly.
(Machel et al. 1991). Other elements
incorporated into the crystal lattice may lead to
quenching of cathodoluminescence.
On optical-stage-mounted CL systems, resolution
is commonly quite low. The geometries of these
systems require that an electron beam be
accelerated through a vacuum chamber onto the
surface of an uncoated polished sample. Standard
microscope optics are used to view the
luminescence through a viewing window at a
fairly large working distance. Most optical CL
systems are designed to work well with up to a
10X objective, but do not work very well at
higher magnifications where the luminescence
intensity is low. Thus, optical-stage-mounted CL
systems, while useful in identifying growth
history (Fig. 2-4), fracturing, and
recrystallization, are not particularly useful for
imaging minerals at the scale of fluid inclusions
(Boiron et al. 1992).
CL detectors installed on SEM and
electron microprobe systems, however, are
capable of resolving CL textures at the scale of
fluid inclusion entrapment. Whereas, several CL
detectors are available, only the highest efficiency
systems can be used to image at the scale
necessary for fluid inclusion work. The best

Cathodoluminescence
Cathodoluminescence (CL) microscopy
can be accomplished with a special detector
installed in an SEM or electron microprobe, or it
can be accomplished using a cold or hot cathode
CL stage, mounted on an optical microscope
(Marshall 1988; Barker & Kopp 1991). The
technique is not used to image fluid inclusions,
but is useful in imaging the growth, fracturing, or
recrystallization history recorded as
compositional variations observable on a polished
surface. Observing thes e textures may be
essential in determining the timing of entrapment
of fluid inclusions trapped just below the surface.
The CL technique produces a color or gray-scale
image of mineral luminescence produced by
electrons bombarding the polished surface. FIG. 2-4. Cathodoluminescence photomicrograph
Mineral cathodoluminescence may be activated illustrating growth-zoning in calcite. Sample
by intrinsic properties of the mineral, defect illustrates crinoid ossicle overgrown by calcite
structures, dislocations, or activators trapped as cement. Modified from Mallarino et al. (2002).
trace and minor elements within the lattice

11
systems produce image resolution at the
micrometer scale (Fig. 2-5). Mineral surfaces
must be polished, mounted on a conductive stub,
and lightly coated with carbon. Imaging works
best with non-phosphorescent minerals such as
quartz, rapidly producing color or gray-scale
images at high resolutions. Phosphorescent
minerals, such as carbonates, require digital beam
control and may take long periods of time to
produce an image. For low-magnification CL
work on an SEM the best images are produced by
using a large aperture. To achieve sharp focus at
higher magnifications, or to avoid problems with
charging, smaller apertures will have to be used
and the brightness and contrast may need to be
adjusted accordingly.
UV epi -illumination
Any fluid inclusionist who is likely to
work in sedimentary rocks should have an optical
microscope with an epi-illuminator outfitted with
a mercury vapor arc lamp and ultraviolet (UV)
exciter filter designed to transmit the 365 nm
wavelength (Burruss 1981, 1991, Guilhaumou et
al. 1990, Kihle 1995). The UV light is reflected
through a dichroic reflector and then is focused
through the objective on to the sample. As the
UV light is focused through the objective before
FIG. 2-5 – SEM-cathodoluminescence photo-
micrograph of fine-scale growth zoning in
quartz overgrowths in sandstone. Detrital
quartz grains (dq) are overgrown by complexly
zoned quartz cement showing concentric
growth zoning, sector zoning, recrystallization
fabrics, and fracture fills. Arrow points to
micrometer-scale growth zoning. Jurassic
Khatatba Sandstone, Egypt. Modified from
Rossi et al. (2002).
12
it hits the sample, the higher the magnification of
the objective, the more intensely focused is the
UV light, leading to resolution at micrometer
scale. For the best images one should use a
polished thick section without a cover slip. A
glass cover slip will absorb too much UV
radiation, thus precluding much fluorescence. A
polished surface will allow for the best optics.
UV epi-illumination may excite
fluorescence in certain minerals. Where mineral
fluorescence has been observed, it has proven to
be useful in documenting growth, fracturing, or
recrystallization history recorded as
compositional variations observable in the
mineral (Fig. 2-6). Resolving such textures are
important for determining the timing of
entrapment of fluid inclusions. As in
cathodoluminescence, mineral fluorescence may
be activated by dislocations or activator elements
trapped as trace and minor elements within the
lattice. Organic compounds may also lead to
mineral fluorescence.
The subject of oil-filled fluid inclusions
will be covered in detail later in this volume
(Burruss 2003) and briefly introduced here in the
FIG. 2-6 – Image of growth zoning in calcite
taken with UV epi-illumination. Jurassic Ascla
Formation, Spain. See Rossi et al. (2001).
context of UV-epi-illumination. Many oil-filled
fluid inclusions fluoresce brightly because of the
presence of aromatic hydrocarbons and nitrogen-,
sulfur-, and oxygen-bearing compounds (Bertrand
et al. 1985, Hagemann & Hollerbach 1986,
Khavari Khorasani 1987). The color of
fluorescence of oil-filled inclusions can be used to
distinguish different compositions, and roughly,
to assess relative differences in maturity and API
gravity (Fig. 2-7, also see Fig. 1 in Burruss 2003,
this volume). The timing and origin of various
generations of petroleum fluid inclusions have
been successfully determined using this approach
(e.g. Burruss et al. 1980, 1985, Burruss &
Goldstein 1980, Burruss 1981, McLimans 1987,
Guilhaumou et al. 1989, 1990, Bodnar 1990,
FIG. 2-7 – Photomicrograph in UV epi-
illumination illustrating brightness of different
colors of fluorescence from oil-filled fluid
inclusions of differing composition. White
arrows point to dull blue-colored fluid
inclusions. Other bright objects are yellow-
and bright blue-fluorescing fluid inclusions.
Mississippian Fayetteville Shale, Arkansas.
See Burruss et al. (1980).
13
Kihle, 1993, Rossi et al. 2001, 2002). Petroleum
fluorescence color typically varies from yellow to
blue colors with increasing maturity and API
gravity (McLimans 1987, Tsui 1990, Stasiuk &
Snowdon 1997). This correlation works best
when comparing one genetically related suite of
oils from a single basin.
Volatile-poor hydrocarbon inclusions
appear dark brown in transmitted light. These
inclusions commonly do not fluoresce or only
fluoresce weakly. Hydrocarbon liquids that have
condensed from a gas phase (condensates )
typically either do not appear to fluoresce or
fluoresce very weakly. Aqueous, carbonic, and
gas inclusions do not emit visible fluorescence.
Several words of warning should be
communicated to potential UV-epifluorescence
petrographers. The first to keep in mind is that
images normally may have a fuzzy appearance.
This is in marked contrast to cathodo-
luminescence. In cathodoluminescence, images
are generated only from the uppermost microns of
the sample surface, because minerals are such
good insulators to electron penetration, whereas
UV light penetrates to significant depths in the
sample, leading to luminescence generation from
depths in the sample that are not in focus.
Moreover, UV excitation makes the sample itself
an unfocused light source. One can imagine the
effect of numerous tiny "light bulbs" within a
sample; not only do the "bulbs" light up, but they
illuminate the area around it, creating a halo of
light and making boundaries of fluorescent
objects difficult to resolve. Finally, beware of the
many "false friends" in UV epi-illumination
(Burruss 1991). Mounting and impregnation
media commonly fluoresce in UV, and polished
thick sections are full of irregularities to reflect
background fluorescence. So, an inclusionist may
see objects that appear to be brightly fluorescing
in a sample that could just as easily be an open
fracture or a pit, as a fluid inclusion filled with
oil. Beware that dust and lab tissue also tends to
fluoresce brightly. Thus, it is always useful to go
back to transmitted-light illumination to see what
the fluorescent object is.
EDS/WDS element mapping
The energy-dispersive system (EDS) on
an SEM or electron microprobe or the
wavelength-dispersive system (WDS) on an
electron microprobe can be used as imaging tools
as well as analytical tools. The techniques are
used to map the compositional variation within
minerals, to help in determining the timing and
origin of entrapment of fluid inclusions (e.g.,
Wilson and Cline (2002) and Wilson et al. (in
press)). Because the techniques use an electron
beam, only the surface is imaged and fluid
inclusions are not visible. Both techniques are
essentially element-mapping techniques,
producing a gray-scale image of the spatial
distribution of a particular major or minor
ele ment on a polished surface of a mineral
specimen (Fig. 2-8). The resolution can be high,
with capabilities of resolving micrometer-scale
growth zoning and fracture fills.
Small pieces of polished thick
sections work well. Normally, samples are
mounted on to an electrically conductive stub and
coated with a conductive film such as carbon or
gold. To make such images, the accelerating
potential (kV setting) must be optimized for the
element of interest. When imaging major
elements, a satisfactory image can be produced in
FIG. 2-8. Wavelength-dispersive system map of
distribution of Mg in calcite, Yucca Mountain,
Nevada. Higher Mg concentration appears
bright. Produced using a JEOL JXA-8900R
electron probe microanalyzer collected with a
single pass, dwell time of 20 ms, accelerating
voltage of 15 kV, and a 20 nA probe current.
Image courtesy of Nick Wilson. Modified from
Wilson & Cline (2002). See Wilson et al. (in
press).
14
minutes, but a high-resolution image of
distribution of a minor element may take hours or
tens of hours to produce.
Infra-red microscopy
The infra-microscope can be used to
image fluid inclusions in dark or opaque minerals
that are transparent to infra-red radiation (e.g.
Campbell et al. 1984; Campbell & Robinson-
Cook 1987; Richards & Kerrich 1993; Luders et
al. 1999). Infra -red microscopes must be
specially adapted for infra -red transmission and
detection. Some minerals that are transparent in
infra -red are some compositional types of pyrite,
sphalerite, hematite, molybdenite, tetrahedrite-
tennantite, pyrargite, energite, chalcocite, stibnite,
cinnabar and wolframite. The technique is
probably best applied to relatively large fluid
inclusions because of the low optical resolution at
such long wavelengths and dark appearance of
fluid inclusion walls (Wilkinson 2001).
Confocal scanning laser microscopy
Confocal scanning laser micro scopy is a
technique commonly used in biology, but only
applied in one area of fluid inclusion research.
The technique takes advantage of the
fluorescence of petroleum inclusions when
excited with a laser. It is used to produce a
quantitative three-dimensional reconstruction of
the liquid and gas volumes within two-phase
oil/gas inclusions (Pironon et al. 1998; Aplin et
al. 1999). The technique uses a confocal pinhole
to reject all light other than that at the focal plane.
The system scans to produce a series of two-
dimensional images, which are then reconstructed
to produce a three-dimensional image of the
inclusion. Accuracy of the volume determination
has been reported as better than 95 %, with spatial
resolution better than 0.5 µm (Pironon et al.
1998).
FLUID INCLUSION APPEARANCE
Introduction
Most fluid inclusion petrography is done
with the transmitted-light microscope. Before a
neophyte inclusionist begins transmitted-light
petrographic analysis, it is useful to consider how
various types of inclusions might appear. This
consideration is extremely important for the
beginner, because normally, the untrained eye
tends to see only that which it recognizes, and
may pass over potentially useful inclusions as Various combinations of phases may be
artifacts, inclusions that have leaked during observable within fluid inclusions. Many
preparation, or just some sort of unknown object inclusions may contain just a single observable
that makes the inclusionist say "hmm?". liquid or gaseous phase. In inclusions with more
Fluid inclusions turn out to be quite than one fluid phase, the wetting properties and
commo n in most samples, observable in most density control the distribution of the phases,
doubly polished thick sections using a 50X normally with the lowest density fluid floating to
objective. Inclusion size varies, but commonly, the center or top of the inclusion and the higher
all inclusions in a sample may be smaller than a density phase appearing in the exterior part of the
micrometer, making their detailed study difficult inclusion. Commonly, two fluid phases are
because of limitations of optical resolution. present. In aqueous inclusions, this normally
Larger inclusions, commonly in the 1 to 20 consists of a dominant liquid phase and a small
micrometer range, are the basis for many fluid vapor or gas bubble (Fig. 2-9). The bubble
inclusion studies. Significantly larger inclusions normally appears quite dark compared to the
can be found, but these are much less common; surrounding liquid because of the difference in
imagine the probability of finding a 30 refractive index between it and the surrounding
micrometer fluid inclusion intact, in a doubly liquid, and because of its common spherical
polished thick section that is not much thicker shape. The bubble may be lodged in a corner of
than a standard thin section! the inclusion, may have floated to the top of the
The appearance of the outer margin of inclusion, or may be dancing around the inclusion
fluid inclusions is controlled by inclusion shape in pseudo-brownian motion. Normally, it is
and the difference in refractive index between the important to remember that the inclusion is being
mineral and the fluid. For the most part, the viewed as a two-dimensional representation of a
difference in refractive index makes the relief
high enough to easily image the outer wall of the
inclusion. For some hydrocarbon liquids,
however, Burruss (1981) has pointed out that the
inclusion fluid could have a similar refractive
index to the enclosing mineral, making it difficult
to image the inclusion in transmitted light. A
similar relationship has been observed between
fluorite and some highly saline, aqueous inclusion
fluids (Samson 1990). Van den Kerkhof & Hein
(2001, p. 32) have compiled a useful table of
optical properties of inclusion fluids, enclosing
minerals, and common solid phases found within
fluid inclusions. For most inclusions, the com-
bination of inclusion shape and difference in
refractive index between mineral and fluid control
how bright or dark the inclusion appears in
transmitted light. Inclusions with flat upper and
lower surfaces transmit light well and appear
bright, whereas negative crystal, irregular, and
globular inclusions have a focusing and
defocusing effect on the light, which when
combined with relief, could lead to irregular
illumination of the inclusion interior or even total
internal reflection. Refractive indices are such
FIG. 2-9 - Photomicrograph of large aqueous fluid
that aqueous and hydrocarbon liquid in clusions
inclusion in fluorite, S. Illinois. Inclusion
typically appear bright and gas- filled inclusions
consists of two phases, a dominant liquid phase
typically appear dark.
and a bubble of gas.

15
three-dimensional object. Thus, the area of the
inclusion occupied by the bubble appears greater
than the volume occupied by the bubble (Fig. 2-
10).
Fluid inclusions also may contain solid
phases together with the fluid. These include
aqueous inclusions containing crystals that have
precipitated during cooling, solid hydrocarbons
precipitated from oil, solids accidentally
entrapped in inclusions as they were formed, and
melt inclusions containing mostly glass or
crystalline solids.
The following summary describes many
of the common petrographic characteristics of
fluid inclusions. It in no way is meant as a
complete summary of all possibilities, but is
designed to inform the neophyte inclusionist
about the many possible combinations of phases
observable. The interpretations of these must be
reserved for a later part of this book, after details
of phase equilibria and reequilibration of fluid
inclusions have been covered in more detail (see
Bodnar 2003b, c; Diamond 2003a, b; Burruss
2003; Anderson 2003).
Solid phases
Fluid inclusions commonly contain solid
phases along with the fluid. The terminology
used here refers to these
materials as solid phases, to include both
minerals and organic solids, and to exclude fluids.
Some solid phases were trapped as accidents of
nature (accidental, or trapped, solids), where a
solid contaminant may have settled or
precipitated on the surface of a growing crystal
and then was incorporated as part of a fluid
inclusion when the host crystal grew around it.
Alternatively, daughter solids are solid phases
actually precipitated from the inclusion fluid after
entrapment as it cooled, or as its composition
changed through some process of alteration of the
fluid chemistry. Fluid inclusions, bearing an
aqueous phase, may have a daughter solid that has
precipitated in optical continuity with the wall of
the inclusion, and which has the same mineralogy
as the host crystal. This common type of
daughter solid forms after inclusion entrapment,
but because it is essentially unrecognizable in
most inclusions, there normally is no need to
mention it as a separate phase in a study.

FIG. 2-10 - Two-dimensional views of four fluid inclusions, each with the same volume and each
containing 10 volume % gas bubble. Length (l) and width (w) refer to dimensions visible in two-
dimensional view. Height (h) refers to the dimension that cannot be seen. For the cube and two
prisms, the bubble is assumed to be spherical. For the flattened prism, the bubble is flattened and
assumed to be cylindrical in shape. Notice how shape and orientation have an important effect on
estimation of bubble volume from a two-dimensional view.

16
 Where solid phases are found within fluid
inclusions, among the most important
determinations that can be made is evaluating if
the solid phases are daughter or accidental solids
(Roedder 1984). Petrographically, accidental
solids can be distinguished from daughter solids
by examining phase ratios among inclusions
along the most finely petrographically
discriminated group of inclusions (fluid inclusion
assemblage; FIA). If solid phases have
precipitated as daughters in those fluid inclusions,
all trapped at the same conditions, one would
expect a consistent ratio of solid to fluid (Fig. 2-
11) where nucleation had occurred. If solids were
trapped as accidents, then the ratios should not be
consistent (F ig. 2-11). Furthermore, accidental
solid inclusions can be identified if the ratio of
solid to liquid is too large to be consistent with
solubility relations for the fluid system (Fig. 2-
12a, b) or if the solid phase is one unlikely to
have precipitated from the fluid (Fig. 2-12c; such
as an organic particle in an aqueous inclusion).
The most common daughter solid in aqueous fluid
inclusions is a single crystal of halite or other salt
(Fig. 2-12d), which has precipitated in the
aqueous fluid inclusion as it cooled. Highly
saline fluids are well known in sedimentary
systems and represent residual evaporite brines or
brines formed from dissolution of evaporite
minerals. In hydrothermal systems, it may be
boiling that concentrates salts. In igneous
systems, residual magmatic fluids can be highly
saline and daughter minerals may be common. In
fluid inclusions in, for exa mple, pegmatite
minerals, the inclusion may appear to be jammed
full of various daughter minerals (Fig. 2-12e).
There are a myriad of different possibilities for
the chemistry of precipitation of daughter solids;
even oil inclusions may precipitate organic
daughter solids as they cool.
Daughter solids that have precipitated
from an inclusion fluid during cooling typically
will re-dissolve into the fluid upon heating. If the
solids in a finely discriminated group of
inclusions all appear to dissolve at the same
temperature, then it is clear that the solids were,
in fact, daughters. In some systems, however, a
fluid inclusion assemblage may all contain solid
phases that have the same solid-to-fluid ratio
among inclusions, but still, the solids do not
dis solve or melt upon heating. These could be
interpreted as kinetic inhibition of melting or that
17
FIG. 2-11. Schematic diagram illustrating
petrographic characteristics of daughter solids
and accidental solids. Diagram portrays field
of view in a minera l containing primary and
secondary fluid inclusions. The primary fluid
inclusions are oriented in growth direction and
concentrated along a concentric growth zone.
The ratio of fluid to solid (solids are black
squares) varies among the primary inclusions
indicating that solid phases are accidental
solids. The secondary fluid inclusions
illustrated are trapped along a healed fracture
that cuts across all of the growth zones. Note
where solid phases are present (dark squares),
the ratio of fluid to solid is consistent among all
of the fluid inclusions. This is evidence that the
solid inclusions are daughters. Inclusions that
lack solids in this group of inclusions have not
overcome the nucleation kinetics that would
allow formation of the daughter minerals.
an irreversible reaction has occurred in the fluid
inclusions that has permanently changed their
chemistry. Permanent changes could involve
closed- or open-system alteration of the fluid
chemistry. An example of open-system alteration
of fluid chemistry is hydrogen diffusion (Hall et
al. 1991; Mavrogenes & Bodnar 1994) which can
cause precipitation of daughter minerals that do
not re-dissolve upon heating. Examples of
closed-system alteration are the disequilibrium
reactions that involve organics, where organic
solids are found in oil inclusions and the ratio of
oil to solid is consistent among all inclusions in a
finely discriminated group (Fig. 2-12f). The solid
organic matter will not re-dissolve in the oil
FIG. 2-12. (A) Photomicrograph of large sulfide mineral (S) with small inclusion (arrow) that formed during
later crystal growth as the solid phase was engulfed. S. Illinois fluorite. Note that ratio of solid phase to
fluid is inconsistent with solubility relations so the solid phase is an accidental solid as opposed to a
daughter. (B) Cluster of calcite crystals settled on surface of growing crystal (base) during precipitation of
calcite in speleothem (modern, Nevada). Thorn-shaped fluid inclusion (above cluster) formed in calcite
crystal as crystal growth proceeded around crystal cluster. Note that ratio of solid phase to fluid is
inconsistent with solubility relations so the solid phase is an accidental solid as opposed to a daughter. (C)
Photomicrograph of large particle of solid organic matter with small aqueous primary fluid inclusion that
formed as crystal grew around the organic particle. Selenite gypsum, central Spain. Such solid particles of
organic matter are unlikely to precipitate from an aqueous fluid. Particle is an accidental solid as opposed
to a daughter. (D) Fluid inclusion with halite crystal. Each fluid inclusion trapped in this fluid inclusion
assemblage has the same ratio of halite to fluid, indicating the halite is a daughter solid. (E) Fluid inclusion
in pegmatitic quartz jammed with daughter minerals, Capitan, New Mexico. (F) Combined transmitted
light and UV epi-illumination of oil inclusions with meniscate areas of dark brownish solid phase (arrrow)
that does not dissolve into liquid phase upon heating. Each inclusion of the fluid inclusion assemblage has
the same ratio of solid to liquid. The solid is a daughter that formed through an irreversible chemical
reaction in the oil. Quartz overgrowth from Jurassic Khatatba Formation, Egypt (modified from Rossi et
al. 2002).

18
during heating, pointing to a closed-system
irreversible change in the chemistry of the oil
after it was entrapped.
Silicate melt inclusions
Silicate melt inclusions are best known
from phenocrysts in volcanic rocks but also have
been studied in plutonic rocks and mantle
xenoliths. Recent reviews (Lowenstern 1995;
Sobelev 1996; Frezzotti 2001) and Anderson
(2003) in this book discuss silicate melt
inclusions in detail. The tremendous variety of
petrographic characteristics of these inclusions
are far beyond the scope of this chapter. Here,
the readers are merely made aware of their
existence. Silicate melt inclusions are samples of
magma normally trapped during crystal growth.
In volcanic phenocrysts, these inclusions may
consist of glass, daughter minerals, one or more
bubbles of gas, or devitrified glass (Fig. 2-13).
Aqueous inclusions
Typical aqueous inclusions include those
trapped at low temperature, consisting of a
FIG. 2-13 – Silicate melt inclusions from
phenocryst, Miocene Cabo de Gata volcanic
complex, SE Spain. Note contraction bubbles
in inclusions.
19
single liquid phase (Fig. 2-14a ) and those trapped
or reequilibrated at higher temperature, normally
consisting of a liquid phase containing a small gas
bubble (Fig. 2-14b). The liquid phase typically
has a bright appearance in transmitted light. The
gas phase normally appears dark. In hydro-
thermal systems, dark inclusions, dominated by
gas may be surrounded by a thin rim of
aqueousliquid, representing entrapment of steam.
Daughter solids are common in aqueous
inclusions. If steam was entrapped, normally at
high temperature and relatively low pressure,
inclusions cool to contain a large bubble of water
vapor and a tiny meniscus of liquid water that
formed around the margins during cooling (Fig.
2-14c)(cf., Diamond 2003a).
Oil, oil-aqueous, condensate, bitumen
Inclusions containing solid and liquid
hydrocarbons are common in diagenetic systems.
Most commonly, oil inclusions appear bright and
colorless in transmitted light (Fig. 2-15a). These
may appear to be identical to aqueous inclusions
in transmitted light, but in UV epi-illumination,
the fluorescence of the oil makes the
compositional distinction clear (Fig. 2-15b).
Some oils in inclusions have a yellowish or
brownish color in transmitted light. Fluid
inclusions containing liquid oil also may contain a
small amount of brownish bitumen-like solid
clinging to the inclusion walls (Fig. 2-12f). The
solids either were entrapped as accidental solids
or formed as daughter solids. Most commonly,
oil inclusions consist of two fluid phases, a
dominant liquid phase and a small gas bubble
(Fig. 2-15a, b). As in aqueous inclusions, the gas
bubble typically appears dark. In oil inclusions
containing a gas bubble, the bubble is more likely
to be in pseudo-brownian motion than in aqueous
inclusions with the same volume ratio of gas to
liquid. When heated during microthermometry,
these inclusions typically homogenize to the
liquid phase. In contrast, some two-phase
inclusions are dominated by the gas phase, with
only a thin rim of liquid oil around the exterior of
the inclusion (Fig. 2-15c). The liquid oil phase is
analogous to a "condensate" liquid that has When
heated during microthermometry, these inclusions
homogenize to the gas phase.
Single phase inclusions are also
common. Many of these consist of liquid oil and
condensed out of the gas phase during cooling.

FIG. 2-14. (A) Photomicrograph of aqueous fluid
inclusions in speleothem calcite, Nevada. Most
inclusions are liquid filled with the exception of
a single two-phase fluid inclusion (arrow).
Thorn shape and orientation in growth direction
(upward) is used as evidence for a primary
origin. (B) Photomicrograph of typical two-
phase aqueous inclusions, trapped at high
temperature as a single liquid phase or
reequilibrated at high temperature. Inclusions
oriented horizontally across field of view
represent entrapment along a healed
microcrack. Tiny fluid inclusions trapped
along another healed microcrack are observable
in the upper right of the photomicrograph.
Fluorite, S. Illinois. (C) Three fluid inclusions
dominated by gas with tiny meniscus of liquid
water along base of each inclusion. Inclusions
were entrapped at high temperature as aqueous
vapor and small amount of liquid water
condensed during cooling.
20
Most hydrocarbon liquids have a refractive index
higher than the aqueous liquid, but in some, the
composition of the hydrocarbon is such that the
relief is essentially nonexistent and the central
globule is only identifiable in UV epi-
illumination. Most commonly, oil-aqueous
inclusions are found with three fluid phases, an
aqueous liquid occupying the exterior of the
inclusion, liquid oil inside it, and a bubble of gas
inside the oil (Fig. 2-15e). In unusual inclusions,
with uncommon wetting characteristics, the oil
globule may cling to the wall of the inclusion or
the oil may wet the wall altogether.
Single phase “gas”
Many sample suites are just loaded with
fluid inclusions that appear to contain only a
single fluid phase. These also have a relatively
dark appearance owing to their high relief, which
commonly discriminates them from aqueous
liquid inclusions (Fig. 2-16). Such dark
inclusions might have a variety of compositions
consisting of methane, carbon dioxide, nitrogen,
or a variety of other compounds that we normally
think of as volatiles at room temperature (e.g.,
van den Kerkhof & Thiery 2001). At room
temperature, it is best to avoid thinking of these
inclusions as gas even though they appear to exist
as a single low-density phase of compounds we
normally associate with gas. At room tempera-
ture it is better to think of the phase present
simply as a fluid. The fluid simply exists at
pressure-temp erature conditions above the homo -
genize ation temperature or critical point and it
may have homogenized to liquid, to gas, or
through critical behavior (see Diamond 2003a, b,
this volume).
Inclusions such as these may be common
in sedimentary rocks, where they are dominated
by methane. Metamorphic rocks may contain
common methane-carbon dioxide-nitrogen in-
clusions.
CO2 -rich fluids, CO2 -aqueous
Carbon dioxide-rich fluid inclusions are a
particularly common type of inclusion, present in
metamorphic rocks, granitoid vein systems, and
mesothermal gold deposits. One end-member
appears as a single dark fluid phase that exists at
room temperature at conditions above its
homogenization temperature (as described
above). Commonly, however, carbon dioxide-
 FIG. 2-15. (A, B) Paired transmitted light (A) and
UV epifluorescence (B) photomicrographs of
oil-filled fluid inclusions in quartz overgrowth,
Note that in transmitted light, oil inclusions
along contact between detrital grain and
overgrowth are clear and colorless. In UV ill-
umination, the inclusions fluoresce brightly.
Sample donated by S. Bu rley. (C) Three con-
densate fluid inclusions marked by white arrows.
Note inclusions have only a thin rim of liquid oil
and are dominated by gas. During heating, the
inclusions homogenize to gas. (D) Photo-
micrograph of quartz overgrowth, Khatatba
Formation, Egypt. Bright fluid inclusions trapped along contact between overgrowth (og) and detrital
grain (dg) are aqueous inclusions. Dark inclusions in overgrowth are composed of bitumen-like solids (b).
(E) Transmitted light photomicrograph of fluid inclusion containing three fluid phases and a solid phase.
Fluorite from S. Illinois. Aqueous liquid (a), liquid oil (o), and a gas bubble (g) are observable. Also note
small body of bitumen observable within the oil phase.
rich inclusions contain multiple fluid phases. (Fig. 2-17). Two-phase inclusions are also
Three fluid phases are common, in which the common. These may consist of an outer area of
outer part of the inclusion is occupied by a single, carbon dioxide liquid and an inner area with a gas
commonly bright, phase of aqueous liquid; inside bubble, or an outer area with aqueous liquid and
the aqueous liquid is a slightly darker area of an inner area with carbon dioxide existing as a
liquid carbon dioxide; and inside that is a bubble single fluid phase.
of gas, commonly in pseudo-brownian motion

21

FIG. 2-16. Transmitted light photomicro graph of
three dark fluid inclusions in quartz filled with
a single “gas” phase. Gas inclusions commonly
(but not in all cases) have a dark appearance in
transmitted light.
FIG. 2-17 – (A) Synthetic (Synflinc) three-phase fluid inclusion in quartz consisting of aqueous liquid (a),
liquid carbon dioxide (lc) and gas (g). (B) Natural three-phase fluid inclusion in topaz consisting of
aqueous liquid (a), liquid carbon dioxide (lc) and gas (g)
22
CLASSIFICATION OF FLUID INCLUSION
ORIGIN
Introduction
This section deals with what many
inclusionists regard as the single most important
step in a study of fluid inclusions. It is the task of
determining the origin of the inclusions present
and creating a paragenesis for their relative timing
of entrapment. It is at this stage of a study that
the inclusionist normally decides whether to
continue or abandon the study. The decision is
made by evaluating if inclusions exist to answer
the scientific question originally posed in the
research. Unfortunately, it is some times the part
of an inclusion study in which the researcher
makes mistakes. We have seen many novice
researchers misinterpret the origin of fluid
inclusions because of an unwillingness to admit to
themselves that the inclusions they needed just
were not there! And finally, all inclusionists must
remember that this phase of the inclusion study
may be among the most time consuming. The
best advice is to be patient. Take the time
necessary to do the petrography correctly, and
you should be rewarded with a project that works
out well and provides results on history of temp -
erature, pressure, and fluid composition
unattainable by any other means.
The methodology for classifying the
origin of fluid inclusions is petrographic in nature
and was summarized by Roedder (1979; 1984).
Inclusion origin relates closely to modes of fluid
inclusion entrapment (see this volume, Bodnar
2003), which is a field that is developing rapidly

FIG. 2-18. Comp osite sketch of primary (p),
secondary (s), pseudosecondary (ps) and
inclusions of indeterminable origin (i) in a
hypothetical view within a single crystal.
as improved imaging techniques are applied.
Terms that are normally used in classifying the
origin of fluid inclusions are primary, secondary
and pseudosecondary (Fig. 2-18). In reality, there
is a fourth term that should be applied in any
realistic study of fluid inclusions, those in which
origin cannot be determined. Origin of inclusions
is most commonly determined using transmitted-
light petrographic study of polished thick
sections, however, any petrographic tool that is
useful in mapping compositional variation in a
crystal, such as BSE, CL, and EDS/WDS element
mapping, normally provides far more information
about a fluid inclusion’s relationship to growth,
recrystallization, or fracturing history. In addition
to indeterminable, three terms are used to classify
the origin of fluid inclusions, namely primary,
secondary, and pseudosecondary.
1) The term primary normally is used to
refer to inclusions entrapped during and as a
direct result of crystal growth.
2) Secondary fluid inclusions are those
trapped after crystal growth is complete, normally
when fractures or deformation features cut across
all growth zones of a particular mineral phase and
heal to trap inclusions. The implication of this
healing is that it is by a process that does not
require introduction of new ions to fill the micro-
fracture, but employs ions redistributed from the
23
fracture surface that have dissolved and re-
precipitated to achieve a state of lower surface
free energy.
3) Pseudosecondary fluid inclusions are
those entrapped before crystal growth is
complete, but not necessarily as a direct result of
crystal growth. They are similar in origin to
secondary fluid inclusions in that they normally
are trapped along micro fractures or other
deformation features that have healed. Unlike
secondary fluid inclusions, however, their
entrapment is followed by further crystal growth.
Importantly, this three-fold classification
of inclusion origin bears no implications as to
whether the inclusions have leaked and refilled,
or reequilibrated in some other way. It is simply
a classification of the origin of the fluid inclusion
vacuole; reequilibration, the process of alteration
of composition or density of the fluid in the
vacuole, must be considered separately (see this
volume; Bodnar 2003c). Perhaps even more
importantly, the terms used in classifying
inclusion origin could just as easily have the word
"petrographically" in front of each (i.e.
petrographically primary, secondary, pseudo-
secondary, or indeterminable). This is because
the classification represents petrographically
based interpretations about timing of the
formation of the inclusion vacuole and does not
refer to the actual timing of entrapment of the
fluid within the inclusion vacuole.
Thus, it is always important to remember
that classification of inclusion origin is a
petrographic interpretation and not data. The data
must be presented as an essential part of any
research report, and interpretations can only be
presented as the logical result of those data. Any
paper that interprets the origin of fluid inclusions
without documenting the petrographic data
leading to the interpretation of inclusion origin
should be viewed as seriously flawed. Therefore,
when writing a research report requiring an
understanding of the timing of entrapment of fluid
inclusions (most studies), that report should
devote a significant amount of effort to justifying
why a particular origin has been interpreted. It is
not enough to say that inclusions are primary by
the criteria of some author. The criteria must be
specifically cited and supported with
photomicrographs, where journal format allows.
Primary inclusions
Criteria for recognition
The only criterion that is applicable in
identifying fluid inclusions as primary is
petrographic evidence for a relationship to growth
of the crystal. This evidence may take many
forms. One of the most important is the shape
and orientation of the inclusions relative to
growth of the crystal. If inclusions have a
particular shape and orientation consistent with
entrapment during growth of the crystal, then this
can be used as strong evidence for a primary
origin (Fig. 2-19a, b). Such inclusions commonly
are elongate in the direction of growth of the
crystal and have flat bases and tapering tips.
Entrapment on the leeward (later growth) side of
an obvious defect (such as a fractured surface)
after subsequent crystal growth is another useful
criterion (Fig. 2-19c). Entrapment of a fluid
inclusion in the wake of an obstruction, that has
poisoned the surface to growth and allowed
formation of a fluid-filled cavity, also serves as a
criterion for primary origin. Such obstructions
include solid phases (accidental solid) (Fig. 2-
12b) and fluid phases (immiscible gas or liquid).
Distribution of a concentration of inclusions
along a single growth zone is used commonly as
evidence for a primary origin. Similarly, if fluid
inclusion size, shape, orientation or concentration
vary by concentric growth zone, then the
inclusions are best assigned a primary origin (Fig.
2-19d). Likewise, if fluid inclusions are
concentrated in a particular growth sector or
associated with the position of particular growth
faces, then this is used commonly as evidence for
primary origin (Fig. 2-19e). Concentric and
sector growth zoning can be observable in
transmitted light by observing variation in
inclusion density or mineral color, but it is most
easily identified by observing the compositional
variation in the crystal using BSE, CL, or
EDS/WDS element mapping. Where observed,
primary fluid inclusions are normally not those
trapped along healed fracture surfaces and are
commonly, but not always, three-dimensional
arrays as opposed to two-dimensional planar or
curviplanar arrays of fluid inclusions.
Primary inclusions - examples
Primary fluid inclusions will have a
myriad of characteristics depending on the
minerals in which they have been trapped, the
24
mechanism of entrapment, and the particulars of
the geologic setting. The following sketches and
photomicrographs are meant to illustrate just
some of the wide ranges of possibilities for
primary fluid inclusions as viewed in transmitted
light. For each inclusionist working in a
particular mineral and geologic setting, it is a
good idea to examine the criteria that other
authors have used to identify primary inclusions
in the same mineral and similar setting. Primary
fluid inclusions in calcite (F ig. 2-20), dolomite
(Fig. 2-21), ankerite (Fig. 2-21), quartz (Fig. 2-
22), feldspar (Fig. 2-23), halite (Fig. 2-24),
anhydrite (F ig. 2-25), gypsum (Fig. 2-26), and
fluorite (Fig. 2-27) are presented.
Primary inclusions - warnings
There are several criteria that traditionally have
been misused over the years in ascribing a
primary origin to fluid inclusions. One should
beware that inclusions described as primary using
these criteria may, in fact, not be primary at all.
For example, many inclusionistshave described
inclusions as appearing to be "isolated" in a
crystal, meaning that the inclusion does not seem
to be related petrographically to any other
inclusions around it. Many of these so-called
isolated inclusions turn out to have formed along
fractures and were not trapped during growth of
the crystal within which they appear to be
isolated. The only examples of isolated
inclusions that we are confident in identifying as
primary in transmitted light are some that are very
large in relation to the size of the crystal. One
should take great care in working with such
inclusions, however. Some of these large
inclusions were trapped as the core growth zone
of a crystal dissolved out and was later cemented
during a later phase of crystal growth. We have
even seen examples in which the entire euhedral
core of a dolomite rhombohedron was occupied
by a fluid inclusion. This inclusion was
surrounded by a euhedral, rhombohedral growth
zone, which could only have formed by
overgrowing a preexisting core zone of dolomite
that had been dissolved later and refilled with
fluid. In such a case it might be easy to
misidentify the timing of entrapment of the fluid
inclusion as early, whereas in fact its entrapment
was quite late in the paragenesis.
Many inclusionists have improperly
classified fluid inclusions as primary using the
FIG. 2-19 - (A) Photomicrograph of Mississippian speleothem calcite. Note many dark, vertically elongate
fluid inclusions, some of which are aligned. This elongation and alignment in growth direction is used as
evidence for primary origin. Growth zoning runs horizontally and is observable along the base of the
figure. Dark diagonal features are cleavage. (B) Photomicrograph of single large fluid inclusion in calcite
with characteristic thorn shape from narrowing during growth of the crystal. Growth direction is from base
to top. Modern speleothem, Nevada. (C) Sketch of fluid inclusions trapped in crystal that has overgrown
an earlier growth zone with a microcrack that has interfered with later growth, causing entrapment of fluid
inclusions (modified from Roedder 1984). (D) Alternating clear and cloudy concentric growth zones in
chevron halite. Cloudy zones are rich in fluid inclusions and clear zones are poor in fluid inclusions.
Permian Nippewalla Group, Kansas. Courtesy of K. Benison. (E) Sketch of fluid inclusions concentrated
in center of starved growth face of a crystal. Modified from Roedder (1984).
criterion of apparent random three-dimensional inclusions. These crystals are shot through with
arrangement of fluid inclusions in a crystal. tens or hundreds of healed fractures that are so
Whereas it is possible that primary fluid densely distributed that the arrangement of
inclusions may have such a distribution, we have inclusions appears random.
found many examples in which there are so many Finally, many inclusionists have improp-
secondary and pseudosecondary fluid inclusions erly assigned a primary origin to inclusions based
in a crystal that they simply appear as a cloudy simply on their negative crystal shape. Whereas
area with no particular planar arrangement of in some samples, it may be true that the primary

25
FIG. 2-20. Compilation of examples of primary fluid inclusions in calcite. All sketches are as viewed in
transmitted-light microscopy. Photomicrographs are in transmitted light. Some images are modified from
Goldstein and Reynolds (1994).

26
 FIG. 2-21 (above). Compilation of
examples of primary fluid
inclusions in dolomite and
ankerite. All sketches are as
viewed in transmitted-light
microscopy.

FIG. 2-22 (left). Compilation of

examples of primary fluid
inclusions in quartz. All sketches
are as viewed in transmitted-light
micro scopy. Photomicrographs
are in transmitted light. Some
images are modified from
Goldstein and Reynolds (1994).

27
FIG. 2-23. Examples of primary fluid inclusions in authigenic feldspar. Shaded regions represent detrital
phases and clear regions represent authigenic replacements and overgrowths. See examples in Pagel et al.
(1986) and Nedkitne et al. (1993). Modified from Goldstein and Reynolds (1994).

FIG. 2-24. Compilation of examples of primary fluid inclusions in halite. All sketches are as viewed in
transmitted-light microscopy. Modified from Goldstein and Reynolds (1994).

28
 FIG 2-25. Sketches of primary fluid
inclusions in anhydrite as viewed
in transmitted-light microscopy.
Modified from Dix and Jackson
(1982).

FIG. 2-26. Sketches of

primary fluid inclusions in
gypsum as viewed in
transmitted-light micro-
scopy. After Lowenstein
(written communic ation,
1993) and modified from
Gold stein and Reynolds
(1994).

FIG. 2-27. Sketches of primary fluid

inclusions in fluorite as viewed in
transmitted-light microscopy.
Modified from Roedder (1972,
1984).

29
inclusions have a negative crystal shape and that
the secondary inclusions have more irregular
shapes, we have seen just as many examples in
which the reverse was true. Moreover, among a
population of fluid inclusions along healed
fractures, it is common to see that some have
negative crystal shapes and some do not. Thus,
inclusion workers should not use negative crystal
shape as a criterion for identification of primary
inclusions.
“Primary” inclusions entrapped during recryst-
allization
Many fluid inclusions, interpreted as
primary from transmitted light petrography, were
trapped when mineral phases recrystallized. In
many geologic and mineral systems,
recrystallization is a dissolution-reprecipitation
process that may take place on the scale of a sub-
micrometer fluid film, or on the scale of
wholesale dissolution of a large portion of a
crystal followed by later precipitation within the
void that was created. It is well known that
variation in composition, defects, and crystallinity
affect the likelihood that a certain growth zone
will be attacked by processes of recrystallization.
Mineral specimens with hollow cores or
preferentially dissolved growth zones are
observed commonly as proof of this (Fig. 2-28).
Dissolved growth zones could easily be filled by
further precipitation in optical continuity with the
original (Fig. 2-29a). Because internal
precipitation (a form of recrystallization) is
commonly quite irregular, bearing many growth
facets converging from many directions,
precipitation in dissolved areas is a common
mechanism for entrapment of fluid inclusions
(Fig. 2-29b). In some samples, inclusions trapped
during recrystallization are the only primary
inclusions present. These inclusions are primary
to the recrystallization of the crystal, so they are
still correctly considered primary, however the
fact that the inclusion was entrapped during
recrystallization commonly goes unrecognized.
In transmitted light petrographic study,
entrapment of fluid inclusions from
recrystallization typically is indistinguishable
from normal crystal growth. An inclusionist
might observe fluid inclusions concentrated in a
particular concentric growth zone of a crystal and
correctly interpret those inclusions as primary.
The first reaction would be to interpret that those
30
inclusions were entrapped when that concentric
growth zone precipitated, but in many examples,
the inclusions were entrapped because that
growth zone was less stable than surrounding
zones; it tended to recrystallize preferentially
while the surrounding growth zones remained
stable. Given this scenario, any inclusion data
could incorrectly be placed in a paragenetic
position that is too early, and thus the geologic
history interpreted could be incorrect. CL and
BSE imaging are two of the best solutions to
problems in identifying entrapment of fluid
inclusions during recrystallization. As CL and
BSE imaging are sensitive to compositional
variations in the crystal, recrystallization should
appear as textures that cut across the original
growth zonation of the crystal. Such cross-
cutting relationships are easily observable as
compositionally different patches within the
normally growth-zoned crystal, or as other areas
of compositionally different crystal that clearly
cut across the original growth zoning (Fig. 2-30).
Entrapment of fluid inclusions from
recrystallization is actually quite common and
potentially important for a wide variety of
minerals, including relatively soluble as well as
insoluble mineral phases. Halite is known to
contain large fluid inclusions trapped during
recrystallization of the original (Lazar & Holland
1988; Horita et al. 1991; Bien et al. 1991).
Dolomite and calcite recrystallize or certain
growth zones dissolve to be filled with more
stable carbonate minerals at a later time (Fig. 2-
31; Gao & Land 1991; Wojcik et al. 1994;
Montañez & Read 1992; Aissaoui 1988). It is
now common practice to consider
recrystallization as part of any study of carbonate
diagenesis. Recrystallized dolomite and ankerite
commonly contain fluid inclusions and it is the
recrystallization that appears to have been
responsible for entrapment of primary fluid
inclusions in many cases (Abegg 1990; Gregg &
Shelton 1990; Shelton et al. 1992; Wojcik et al.
1992, 1994, Goldstein & Reynolds 1994, Luczaj
& Goldstein 2000, Rossi et al. 2002, Ceriani et al.
2002). Importantly, recrystallized carbonate
minerals may look perfectly normal using
transmitted light petrography. It is only where
compositional variation is apparent that
recrystallization can be identified. Normally this
requires BSE, CL, EDS, WDS, or composition-
specific staining to show the important textures.
 FIG. 2-28 (above). Photograph of
calcite specimen with preferential
dissolution of certain growth zones.
Later precipitation and entrapment
of fluid inclusions in these voids
could trap fluid inclusions that are
primary. As the inclusions would be
found in the inner parts of crystals,
the timing of fluid inclusion
entrapment could be misinterpreted
as earlier than it really was. Width
of photograph is 8 cm.

FIG 2-29 (left). (A, top) Dolomite

encased in anhydrite. Note how
core of dolomite (arrow) appears
dark because it has dissolved to
leave a rhombohedral-shaped void.
Permian of New Mexico. Courtesy
of K. Hartig. (B, below) Cathodo-
luminescence photomicrograph
showing patchy replacement of
interior part of dolomite rhomb -
ohedra. Fluid inclusions in this
dolomite were trapped during
incomplete filling of the dissolved
core of the dolomite. See Luczaj &
Goldstein (2000).

31
FIG. 2-30. Schematic illustration showing entrapment of fluid inclusions through preferential recrystalliz-
ation of a compositional growth zone in a crystal. Scale is microscopic view of a single crystal. (A)
Illustration of compositional growth zoning in a crystal as viewed in cathodoluminescence or back-
scattered electron imaging. (B) Texture observable with cathodoluminescence or back-scattered electron
imaging after internal growth zone has been dissolved and refilled with later phase of mineral. Fluid
inclusions are superimposed to illustrate relationship between recrystallized internal growth zone and
entrapment of fluid inclusions. (C) Same crystal as (B) and (C) as viewed in transmitted light. Note that
fluid inclusions are concentrated in a particular internal growth zone and would be interpreted as primary.
Using transmitted light petrography alone, the inclusionist would incorrectly identify the inclusions as
trapped during growth of an early zone of the crystal, whereas in reality, the inclusions were trapped very
late in the paragenesis during recrystallization of the early growth zone.
Recrystallization is also common in less to coarser quartz (Williams et al. 1985).
soluble minerals, even at low temperature. In Crystallinity tends to increase with age and
authigenically replaced detrital feldspars, fluid temperature (Murata & Norman 1976, Pisciotto
inclusions are fairly common in the recrystallized 1981, Kruge & Williams 1982, Isaacs et al 1983).
areas (Pagel et al. 1986; Nedkitne et al. 1993). Recrystallization in quartz can be driven by
Even quartz is prone to recrystallization. differences in crystallinity, dislocations,
Cryptocrystalline quartz or chalcedony commonly composition, or specific surface area. Differences
recrystallizes to microcrystalline quartz, and then in specific surface area may cause Ostwald

FIG. 2-31. Back-scattered electron image of Cretaceous sandstone from Libya. Quartz grains (q) are
cemented with dolomite (d). Arrow points to areas in dolomite in which patchy fabrics indicate
recrystallization of the dolomite that led to entrapment of fluid inclusions. Modified from Ceriani et al.
(2002).

32
ripening-driven coarsening of quartz (Williams et
al. 1985).
Commonly, one assumes a simple
mineral like quartz is quite uniform in
composition, however, this simply is not true.
For example, chalcedonic quartz is composed of
three varieties of quartz with physical properties
different from coarsely crystalline, “normal”
quartz. Experimental and empirical studies show
that even coarsely crystalline “normal” quartz
may be prone to recrystallization. For example,
microcracks and fluid inclusion vacuoles are sites
of dissolution and reprecipitation in quartz (van
den Kerkhof & Hein 2001). Fluid inclusions in
quartz change shapes through dissolution and
reprecipitation (necking down; Bodnar et al.
1985) to achieve shapes of lower surface free
energy. Microcracks in quartz heal through a
similar process in which high temperatures
increase the rate of healing, but even at low
temperatures (as low as 200°C), only a hundred
years or less is required (Brantley et al. 1990,
Brantley 1992). These observations, combined
with other evidence of increase in crystallinity of
quartz as a maturation process, suggest that quartz
may be subject to recrystallization at low
temperature as well as at high temperature.
Recrystallization of quartz and unstable
silica minerals appears to be an important
mechanism for entrapment of primary fluid
inclusions. In a study of sandstones cemented by
hydrothermal fluids, Goldstein & Rossi (2002)
and Rossi et al. (2002) found CL textures in
coarse quartz overgrowths, which indicated that
coarse quartz initially precipitated as opal-CT,
cryptocrystalline quartz, microcrystalline quartz,
and chalcedony (Fig. 2-32). Later, these unstable
growth zones recrystallized to normal quartz
overgrowths, trapping fluid inclusions in the
recrystallized areas. In some of the same
overgrowths, growth zones of dully luminescent
quartz are cut across by areas of more brightly
luminescent quartz. The bright areas follow
fractures, but their geometries are impossible for
normal fracture fillings, indicating dissolution or
replacement of earlier quartz. Fluid inclusions
appear to be concentrated in the more brightly
luminescent, recrystallized quartz. Similar
complex recrystallization fabrics are well known
in higher temperature and deformed quartz. Rusk
& Reed (2002) demonstrated fluid inclusion
entrapment in the Butte porphyry copper deposit
33
was related to a complex history of quartz
precipitation, fracturing, dissolution, and
recrystallization by the observation of various
textures observable only in CL. Van den Kerkhof
& Hein (2001) recently summarized other such
textures from high temperature quartz.
Importantly, in all of these low- and high-
temperature examples of fluid inclusion
entrapment associated with recrystallization of
quartz, transmitted light petrography generally
gives no hint that recrystallization has occurred.
The quartz may have uniform extinction and look
perfectly normal. The recrystallization is
identifiable with CL petrography alone.
In conclusion, many of the fluid inclusions that
are commonly classified as primary have been
entrapped during recrystallization of minerals.
Recrystallization may be one of the more
common mechanisms for entrapment of fluid
inclusions. As recrystallization can be a process
of dissolution and precipitation, it may generate
cavities that are incompletely occluded by
subsequent precipitation, trapping abundant fluid
inclusions. This process may attack only certain
compositional growth zones in a mineral, trapping
fluid inclusions that appear to be out of order in
the paragenesis established using transmitted light
alone. As the process appears to affect a wide
variety of minerals, it appears that all
inclusionists should start considering the
possibility of recrystallization in their studies.
Petrographic techniques that are useful in
evaluating the compositional variation in crystals
(BSE, CL, EDS, WDS, or composition-specific
staining) are those best applied in evaluating the
possibility of recrystallization.
Secondary inclusions
Criteria for recognition
Secondary fluid inclusions form after
crystal growth is complete and is a process of
healing of microcracks and deformation features.
Some prefer to classify different types of
secondary fluid inclusions based on origin and
transgranular versus intragranular occurrence
(Simmons & Richter 1976, Kranz 1983, van den
Kerkhof & Hein 2001). To identify fluid
inclusions as secondary, they must appear to
occur in arrays that cut across all growth zones of
a crystal (Fig. 2-18, 33). Fluid inclusions trapped
by healing of microfractures typically occur in
planar arrays or along curved surfaces that cut
FIG. 2-32. SEM-CL images of quartz overgrowths on detrital quartz grains (dq). Arrows point to abundant
relict structures of recrystallized precursor silica phases and cross-cutting relationships indicating
recrystallization. The recrystallization is one of the major controls on entrapment of fluid inclusions.
Modified from Goldstein and Rossi (2002).

34

FIG. 2-33. Several planar arrays of secondary
fluid inclusions that formed in healed fractures.
Fluorite, S. Illinois.
across growth zonation. Where secondary fluid
inclusions are trapped along cleavage or twin
planes, the inclusionist should be careful to avoid
confusing these inclusions with inclusions of
primary origin. Such crystallographically
controlled planes of secondary fluid inclusions
are easily distinguishable from primary fluid
inclusions by the tendency for secondary planes
to cross one another and the tendency for primary
fluid inclusions to mimic crystal terminations.
The inclusionist should be aware that
there may be some ambiguity inherent in the
classification of fluid inclusions as secondary.
Remember that the basis for classifying fluid
inclusions as secondary is that they are not the
direct result of crystal growth and result from
“healing” of microcracks or deformation features
without the addition of new ions. This inherently
genetic classification commonly leads to some
ambiguity. Let us take the scenario of a rock that
has been fractured. The fractures are open pores
that are immediately filled with fluid. If the
35
fracture walls dissolve and reprecipitate to neck
the fracture down into an array of fluid inclusions,
maintaining the original volume of the fracture,
then the classification as secondary is just fine.
The fluid, however, may introduce new ions that
passively precipitate mineral within the fracture
(Fig. 2-34) and trap fluid inclusions. If that
mineral is the same one as that which surrounds
the fracture, the fracture filling will be in optical
continuity with the surrounding mineral and will
be invisible with transmitted light petrography. If
the mineral filling can be identified in CL or BSE,
then the inclusions could easily be classified as
primary, because they are the direct result of
mineral growth. In transmitted light, however,
they will appear as a planar array of fluid
inclusions that appears to cut across all growth
zones, and thus, they would be classified as
secondary. Once again, this scenario illustrates
the need for applying petrographic techniques
useful in evaluating the compositional variation
of the minerals studied. Applying only
transmitted light petrography normally will lead
to some ambiguity in classification of fluid
inclusions. The inclusionist should routinely use
CL, BSE or some other imaging technique useful
in imaging compositional variation.
Secondary inclusions - cross-cutting relation-
ships
Determining the timing of entrapment of
multiple planar arrays of secondary inclusions is
among the most important and difficult
petrographic techniques in fluid inclusion work.
As many samples are dominated by secondary
inclusions, and as secondaries have the potential
for recording nearly every stage in the P-T-X
history of a geologic setting, establishing the
relative timing of entrapment of various
secondary inclusions is essential. The technique
employed in establishing relative timing (Touret
1981) is a basic cross-cutting relationship, but a
particular type that is very difficult to apply. To
establish this relationship, two planar arrays
(inclusions along healed fractures) must lie along
cross-cutting paths. Each planar array should
contain inclusions of distinctive size, shape or
orientation so that the inclusions of one array can
be distinguished petrographically from inclusions
of the other array. If where the planar arrays
cross, an inclusion of one array is filled with the
fluid composition of the other array, relative
FIG. 2-34. Diagram illustrating potential ambiguity in discriminating between primary and secondary fluid
inclusions. (A) Schematic illustration of a quartzite as viewed in transmitted light. Quartzite develops
open fracture (white). (B) Schematic illustration of a quartzite as viewed in transmitted light. After the
fracture is healed or filled, a planar array of fluid inclusions is entrapped, normally classified as secondary.
(C) Schematic illustration of a quartzite as viewed in cathodoluminescence. Note concentric growth
zoning in fracture fill indicating fluid inclusions were trapped as a direct result of crystal growth through
the addition of new ions to the fracture. With this observation, inclusions would be classified as primary.
timing can be established (Fig. 2-35). In our identified in tectonic vein systems. In most
experience, finding such cross-cutting relation- systems, however, pseudosecondary fluid
ships is extremely difficult, and the inclusionist inclusions are difficult to identify.
should not expect to apply such relationships
without exceptional effort or good luck.

Pseudosecondary inclusions
Criteria for recognition
Pseudosecondary fluid inclusions can be
treated as identical to secondary fluid inclusions
because they essentially have the same origin
except that they are trapped before mineral
growth is complete. All criteria cited above for
identification of secondary inclusions apply to
pseudosecondary fluid inclusions except that the
fractures or deformation features do not cut across
all growth zones of the mineral. For
pseudosecondary fluid inclusions, planar arrays of
fluid inclusions end abruptly at a growth zone
boundary (Fig. 2-18). They are subsequently
overgrown by later mineral growth lacking fluid
inclusions trapped along the same fracture.
Recognition of pseudosecondary
inclusions requires that multiple planar arrays of
inclusions terminate against a growth zone. A
single planar array of inclusions terminating
against a growth zone is not sufficient to classify
inclusions as pseudosecondary, because all
fractures end somewhere, whether secondary or FIG. 2-35. Methodology for using cross-cutting
pseudosecondary. Consistent termination of relationships involving planar arrays of
multiple healed cracks is required. Pseudo- secondary fluid inclusions (e.g., Touret 1981).
secondary fluid inclusions are commonly

36
 there should be little need to treat fluid inclusions
Indeterminable inclusions
as statistical populations, as has been the common
In many samples, the origin of most of
approach up until about 1990. In a recent
the fluid inclusions cannot be determined because
meeting of inclusion researchers, those
the petrographic criteria are either not present or
inclusionists not using this concept were
are too ambiguous to make an unequivocal
questioned heavily, and a consensus seemed to
interpretation. The careful inclusionist must
arise that the FIA approach was preferred. There
always admit when he or she does not know the
are some excellent reasons for this. Applying the
origin of a fluid inclusion. It is best to err on the
fluid inclusion assemblage approach in a study
side of caution here and to avoid classifying fluid
allows for the most detailed analysis of
inclusions without a strong petrographic argument
temperature, pressure and fluid composition
for their origin. In earlier years of fluid inclusion
history. It allows the researcher to consider each
work, this was not done so well, and many fluid
growth zone and each event of fracture healing as
inclusion studies were published with results that
a separate event in geologic history, and avoids
did not make sense.
the lumping together of multiple events. Such a
detailed analysis is commonly essential for
understanding the geologic system being studied,
FLUID INCLUSION ASSEMBLAGES and may be the only way the fluid inclusion data
All studies of fluid inclusions employing
can be evaluated. The FIA approach is essential
petrography must attempt to discriminate the
for identifying alteration of fluid inclusions from
various events of fluid inclusion entrapment at the necking down after a phase change, stretching, or
finest level possible given the particular
leakage and refilling (Bodnar 2003c). It is crucial
petrographic relationships present in the samples.
in identifying the presence of multiple immiscible
Finely discriminated groups of petrographically phases at the time of inclusion entrapment, which
associated fluid inclusions are termed fluid
is so important for geobarometry and geotherm-
inclusion assemblages (Goldstein and Reynolds,
ometry (see this volume; Bodnar 2003b; Burruss
1994). Each fluid inclusion assemblage (FIA) is 2003; Diamond 2003a, b).
defined based on a petrographic association in
Applying the fluid inclusion assemblage
which all inclusion vacuoles of each FIA
approach requires that the researcher seek the
represent the finest temporal resolution possible petrographic resolution that will identify those
as to timing of initial closure of the inclusion
fluid inclusion vacuoles that formed at about the
vacuoles. Later reequilibration of the inclusion
same time. The most easily identifiable FIA
vacuole is not considered in this definition unless consists of all those fluid inclusions trapped along
there is petrographic evidence for it. In other
a single healed microfracture (F ig. 2-36). All
words, an FIA represents the fluid inclusionist’s
those fluid inclusions trapped along a single
finest petrographic ability to identify those growth zone comprise another example (Fig. 2-
inclusions sealed at a single time. The hard
36). As previously discussed, these finely dis -
reality of this, however, is that an FIA cannot
criminated events of fluid inclusion entrapment
truly be formed instantaneously, but must have may require petrographic techniques, such as CL
been formed over some interval of geologic time
and BSE, that would allow for the finest
as the multiple inclusions were sealed. The
discrimination of growth zonation. The FIA
inclusions in a particular FIA may have been approach represents the standard in the fluid
sealed over a time interval as short as days or
inclusion community, and therefore, it
over a time interval of thousands of years,
emphasizes the importance of careful petrography
depending on the mechanism of inclusion in any fluid inclusion study.
formation. Petrography gives us our best chance,
however, of identifying those inclusions formed
ACKNOWLEDGEMENTS
at the about same time, even though we can never
Many of the concepts presented
expect to be able to define instantaneous events of
in this paper were developed during
entrapment.
collaborations with T. J. Reynolds. His
We recommend use of the concept of the fluid
contributions were essential to this work. Daniel
inclusion assemblage in all fluid inclusion studies
J. Kontak and Alfons M. van den Kerkhof
with a basis in petrography. Using this concept,

37
FIG. 2-36. Diagram of the fluid inclusion assemblage "game". There are ten fluid inclusion assemblages that
can be identified in this sketch of a quartz overgrowth on a detrital quartz grain. For practice, identify each
one, classify its origin, and put all ten into a paragenesis of fluid inclusion entrapment. You should find
one FIA in the detrital grain that predates the quartz overgrowth, three primary FIAs, three
pseudosecondary FIAs, and three secondary FIAs.
provided reviews that improved the manuscript. Anderson, & D. Marshall, eds. Fluid
Cynthia L. Keeffe provided editorial assistance. Inclusions: Analysis and Interpretation.
Samples and figures were kindly provided by K. Mineral. Assoc. Canada, Short Course 32, xx-
Benison, S. Burley, A. Ceriani, K. Hartig, E. yy.
Hiemstra, A. Lacazette, T. Lowenstein, J. Luczaj,
A PLIN , A.C., M ACLEOD, G., LARTER, S.R.,
G. Mallarino, K. D. Newell, T. J. Reynolds, C.
PEDERSEN, K.S., SORENSEN. H., & BOOTH, T.
Rossi, N. Wilson, and K. Wojcik. Supported by
(1999): Combined use of confocal laser
the Haas Fund of the University of Kansas and
scanning microscopy and PVT simulation for
NSF Grants EAR-8721229, EAR -9218463, and
estimating the composition and physical
EAR-9527004.
properties of petroleum in fluid inclusions.
Mar. Petroleum Geol. 16, 97-110.
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