Fundamentals of Fluid Inclusion

Studies

Lorena Ortega
lortega@ucm.es

5-7th December 2017 1

About me

Lorena Ortega (lortega@ucm.es)

• Senior Lecturer at Complutense University of Madrid

• Dean at the Faculty of Geology

Teaching subjects: Ore mineralogy and Ore deposits

Research experience: Mineralogy, geochemistry and fluid

inclusions in hydrothermal ore deposits
• Sb-Au vein-type deposits in Spain
• Au, Ag, Zn-Pb epithermal deposits and Cu mantos in Chile
• Fluid-deposited graphite in Spain and UK

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My trainner in Fluid Inclusions

Thanks to Jacques Touret, my professor!!!

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What are we going to do:

• Introduction: what are fluid inclusions and what can

you do with it?
• Fluid inclusions petrography
• Fluid inclusions: physical chemistry
• Collecting data: petrography, microthermometry,
Raman
• Data presentation
• Application to Ore Deposits: case studies
• PLEASE ASK QUESTIONS
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 1. Introduction

• What are fluid inclusions?

• Fluid inclusions studies: what do you
need and what do you get?
• Fluid inclusions references
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 Inclusions in minerals 3

There are three types of inclusions that may occur in minerals: 4

(1) Mineral inclusions

(2) Melt inclusions
(3) Fluid inclusions
10 µm

25 µm

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What are fluid inclusions?

A small volume of fluid, trapped and closed in a solid

mineral phase. They are formed when:

• a mineral forms in the

presence of a fluid
phase, and some of
the fluid is trapped as
defects in the growing
crystal
• mineral precipitation
occurs in the process
of healing fractures in
existing minerals

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and...

They are the only direct

evidence of the role of fluids in
rock-forming processes and
hydrothermal ore-forming
processes

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When observed under microscope, most fluid inclusions contain
more than one phase

The fluid phase may be liquid or vapor, and may include aqueous
solutions and volatiles such as CO2, CH4, N2, etc.
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Where are fluid inclusions found?

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Increasing microscope magnification... x5

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Increasing microscope magnification... x10

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Increasing microscope magnification... x20

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Thinking about performing a fluid inclusion study?

What do you need?

• A research problem that can be solved with fluid inclusions
• Representative samples that are related to you research problem
• Enough sample material for fluid inclusions, microprobe analyses, etc.
• Fluid inclusions samples: double polished 200 µm thick wavers
• A good microscope
• A heating/freezing stage
• and, very important:

Time!!!
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Thinking about performing a fluid inclusion study?

What do you get from fluid inclusions

• Composition of a fluid present during a geological event

(mineralisation, diagenesis, metamorphism, etc.)

• P-T conditions of fluid trapping

• In hydrothermal ore deposits:

wIdentification of fluid circulation episodes
wInformation about the processes involved in ore
precipitation

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Fluid inclusion literature

The first comprehensive book about

fluid inclusion research (1984) is still A true practical guide
a useful source of information for although difficult to find
inclusionists nowadays
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Fluid inclusion literature

✓ ✓

A very useful book for fluid The result of a fluid inclusion

inclusions researchers, even if you short course held in 2003. It
are not dealing with diagenetic summarizes current knowledge in
minerals the field. 17
Fluid inclusion literature

Yardley B. and
Bodnar R.
(2014)
Geochemical
Perspectives
vol. 3, 160 pp.

Hurai, V., Huraiová, M, It is not exactly a book about FI, but it is an

Slobodnik, M., Thomas R. easy-reading and interesting summary for
(2015) Elsevier, 489 pp. those interested in geological processes
involving fluids. 18
What other resources are available?

Several websites including:

• Fluid Inclusion Laboratory Leoben, Ronald Bakker
(http://fluids.unileoben.ac.at/Home.html). This website includes
free software for composition and isochore calculations
• Fluid and Melt Inclusions, Phil Brown
(http://www.geology.wisc.edu/~pbrown/fi.html)
• Virginia Tech Geosciences Fluid Research, Bob Bodnar
(http://www.geochem.geos.vt.edu/fluids/index.shtml)
• Journal articles

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2. Fluid inclusion petrography

- Fluid inclusions classification

- Homogeneous and heterogeneous trapping
- Roedder’s rules
- Post-trapping modifications
- Fluid inclusion assemblages
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Fluid inclusion research: procedure
KEY
POINT

• Fluid inclusion petrography: identify fluid inclusion

assemblages

• Microthermometry (density, composition)

• Raman microspectroscopy (more info on composition)

• Data visualisation (histograms, x-y diagrams)

• Interpretation: answer to your research question(s)

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Observing fluid inclusions

What is needed and what to do?

• A good binocular microscope with 5×, 10×, 20× and 40× objectives

• Excellent polished samples

• Fluid inclusions are small, you need to use the 20× or 40× microscope
objective

• Use the condenser lens and change the contrast by moving the condenser
lens up/down

• Make good photographs and make good drawings. You must be able to find
your fluid inclusions when doing microthermometry, Raman, etc.

• Most importantly: you need time

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Fluid incusions: petrography

• Descriptive classification (single fluid inclusions)

• Genetic classification: Primary and secondary inclusions
• Roedder´s rules
• Trapping conditions: homogeneous and heterogeneous trapping
• Post-trapping modifications
• Explosion/implosion decrepitation
• Identification of fluid inclusion assemblages

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Fluid inclusion classification: descriptive

• Size
• Shape (irregular, regular, negative crystal shape)
• Number of phases
• Solid (S)
• Liquid (L)
• Vapour (V)
• Fluid/gas (F)
• Relative size of vapour/gas phase
• Colour: clear, dark, very dark/black

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Negative crystal shape
Driven by tending towards lowest surface energy

Quartz
http://m.palaminerals.com/inclusions/
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Negative crystal shape (quartz)

Furua Granulite Complex, Tanzania

Sample from Coolen (GUA 1980)

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Negative crystal shape (quartz)

Furua granulite (M. Coolen)

Gakara (Burundi)

Van den Kerkhof and Hein (2001)

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Negative crystal shape

Fluid inclusion with negative cubic

crystal shape in halite
Fluid inclusion with negative tetrahedron S. V. Vovnyuk and G. Czapowski, 2007
crystal shape in sphalerite
Lüders et al. 2002

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Regular and irregular shapes

Fall et al. 2011 – Geoch. Cosm. Acta

Bakker & Dopler 2016 Chem. Geol.

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Fluid inclusions shape

Regular, irregular, negative crystal shape.

Which one is which?
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Fluid inclusions description at room temperature

Number and state of

phases F (L?, V?)

LV<50%

LV>50%

L2+V

LVS5 LVS LVS

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Daughter crystals

crossed nicols

Use the polariser to

identify birefringent
minerals!

(Koivula, p. 391)

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Volume fractions for different fluid inclusion shapes

(after Shepherd et al. 1985)33

Volume fractions for different fluid inclusion shapes

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Volume fractions in inclusions

Exercise:

What is the volume

fraction of the bubble in
each inclusion?

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Volume fractions in inclusions

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Volume fractions in inclusions of different orientation

Liquid-vapor ratios as seen

through the microscope in a
fluid inclusion waver in which
all inclusions contain 25 vol.%
vapor

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Volume fractions in inclusions

What is the volume fraction of the bubble?

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 Volume fractions in inclusions

Do these fluid
inclusion have the
same relative
bubble size?

Source: www.es.utoronto.camagmaticresearch
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Colour: aqueous and gaseous FI under the microscope

Gaseous fluid inclusions

Aqueous fluid inclusions look darker
look brighter Observation possible
due to different
refractive indices:

Qtz n = 1.54-1.55
Water n = 1.33
Liquid CO2 n = 1.20
Air n = ~1.00

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Fluid inclusions classification: genetic

Trapped during the growth of the host mineral

Primary inclusions
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Primary fluid inclusions

Primary fluid inclusions formed on imperfections on crystal surfaces during

precipitation and contain the fluid present at the moment of sealing.

Growth
direction

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Primary FI: easy to recognize in zoned crystals

Quartz Dolomite
Optical Back scattered
microscope, Electrons Image
transmited (BSE)
light

Detrital quartz
(dq) + quartz
cement in a
Calcite sandstone

Cathodoluminiscence SEM-Cathodolumniscence
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Primary FI: Quartz

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 Primary FI: Calcite

Goldstein & Reynolds (1994)

Transmited light 45
Primary FI: Fluorite

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Primary fluid inclusions in not zoned crystals

Primary fluid inclusions may occur as isolated inclusions or as in

not oriented clusters, but it is difficult to ascertain that they are
truly primary

Be careful with those inclusions!!!!

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Primary fluid inclusion identification

Primary fluid inclusions

Single crystal Zoned crystal

Occurrence as individual fluid

Occurrence in growth zones
inclusions or 3D grouping

Occurrence after a healed crack of

Relatively large fluid inclusions
an older growth stage
Occurrence in the core of the
Isolated position away from others
crystals
Fluid inclusions contain a solid
Occurrence along the intersection of
phase, which is also a solid phase in
growth planes
the host mineral

(Roedder, 1984; Van den Kerkhof and Hein, 2001)

Unambiguous 48
Pseudosecondary fluid inclusions

Pseudosecondary fluid inclusions form when a crystal fractures during its

growth and original fluids are trapped in the rim of the crystal. They
commonly occur between distinct growth zone and end abruptly at growth
zone boundaries.

(V. Lüders)

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Fluid inclusions classification: genetic

After the growth of the host mineral, along fractures

Secondary inclusions
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Stages of healing of a microfracture in quartz

The final shapes of the inclusions have crystal faces as surfaces (negative crystal
shape). This is the most stable state as it has the lowest surface-free energy

(modified from Roedder, 1962)

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Stages of healing of a microfracture in quartz

Partial fracture healing, resulting in secondary fluid inclusions

Water

Gas

(modified from Roedder, 1962)

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Stages of healing of a microfracture in quartz

Partial fracture healing, resulting in secondary fluid inclusions

(modified from Roedder, 1962)

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Stages of healing of a microfracture in quartz

Partial fracture healing, resulting in secondary fluid inclusions

Water

(modified from Roedder, 1962)

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Secondary fluid inclusions

Secondary fluid inclusions form after crystal growth. They often occur
along healed fractures and may cut across growth zones.

Rhodochrosite gemstone from Wuzhou, Guangxi, China (Virginia Fluid Inclusion Lab)
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Secondary inclusions

In plannar arrays
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Secondary inclusions

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Secondary inclusions: trail terminology

A main distinction is made between intragranular and

intergranular inclusions.

1-3: Intergranular
4-6: Intragranular

Van den Kerkhof & Hein (2001)

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Multiple trails of secondary inclusions

Cross-cutting relationships
involving planar arrays of
secondary inclusions

Touret (1981) in Samson et al. 2003, p.47

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Time relationship with the host mineral

Primary / Secondary
Pseudosecondary

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Fluid inclusions and their origin: summary

Four possilities:
- Primary
- Secondary
- Pseudosecondary
- UNKNOWN

Goldstein & Reynolds, 1994

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“Roedder´s rules”

Obtaining valid information concerning the original trapping conditions for

fluid inclusions (primary or secondary) is based on three assumptions, referred
to as “Roedder’s Rules”:

1. The inclusion traps a single, homogeneous phase.

2. Nothing is added to, or removed from, the inclusion following trapping.

3. The inclusion volume remains constant following trapping,

i.e., represents an isochoric system. Volume = Mass / Density

Therefore, fluid inclusions evolve as closed systems after trapping,

Checking if our fluid inclusion assemblages obey Roedder`s rules is KEY

before proceeding with microthermometry
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How can we test “Roedder’s Rules”?

Does this inclusion obey Roedder’s Rules?

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How can we test “Roedder’s Rules”?

Does this inclusion obey Roedder’s Rules?

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How can we test “Roedder’s Rules”?

Does this inclusion obey Roedder’s Rules?

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Checking the rules: Homogeneous trapping

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Checking the rules: Heterogeneous trapping

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Checking the rules: Homogeneous trapping

P-T conditions of fluid entrapment:

If inclusions are trapped simultaneously in a single-phase field (liquid or
vapor), their composition and density will be identical, i.e. the relative
volumetric proportions of the inclusion phases at room temperature will be
the same.

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Checking the rules: Heterogeneous trapping

P-T conditions of fluid entrapment:

If fluid inclusions are trapped in a multi-phase field, the properties and the
relative volumetric proportions of the inclusion phases at room temperature
are variable.

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Heterogeneous trapping of fluid inclusions

Co-genetic pair of fluid inclusions Healed fracture in quartz containing

containing water with a methane bubble co-genetic CO2-rich inclusions
and liquid methane and an invisible rim equally distributed in the plane and
of water along the cavity wall (Armsfeld showing negative crystal shape and
Kellerwald, Germany, Hein et al., tiny high-salinity H2O inclusions
1994a,b) arranged in trails (Van den Kerkhof &
Hein 2001)
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Homogeneous or hetergoneous trapping?

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Post-trapping modifications

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Post-trapping modifications

Stretching èLeakage è Partial decrepitation èDecrepitation

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Post-trapping modifications

Implosion

(collapsing cavity)

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Post-trapping modifications

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Post-trapping modifications: Necking down

Many fluid inclusions have relative large surface areas when trapped.
Processes of recrystallization, generally termed “necking-down“,
immediately start to reduce the high surface energy in the system. resulting
in the development of fluid inclusions with varying proportions of liquid and
vapor.

Roedder, 1962
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Necking-down

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Post-trapping modifications: leakage

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Post-trapping modifications: decrepitation

Decrepitation = explosion

West-Uusimaa, Finland (T. Hartel)

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Post-trapping modifications: Implosion

Modified fluid inclusions are surrounded by small satellite inclusions.

Re-crystallization results in the reduction of the inclusion volume.

Sample from Muhokore, Burundi, Hein et

al., 1994; Van den Kerkhof & Hein 2001)
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Implosion or decrepitation texture?

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Units of information: FIAs

The unit of information is not

a single fluid inclusion, but
the fluid inclusion assemblage
(FIA)

FIA: group of fluid

inclusions trapped at the
same time

Any fluid circulation event is

represented by a number of
FIAs that may show the fluid
evolution with time
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Concept of fluid inclusion assemblage (FIA)

• If a group of fluid inclusions have been trapped at the same

time, the would show the same number of phases, the same
L/V ratio and similar microthermometric results.

• Identifying fluid inclusion assembages is the most important

aspect of any fluid inclusion study

Exercise:
(1) Identify all fluid inclusion assemblages;
(2) Indicate which one(s) is/are primary, pseudosecondary,
and secondary;
(3) Put the assemblages in chronological order from old to
young.
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Exercise: Fluid inclusions assemblages

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Summary of fluid incusions petrography

• Petrography is the most important aspect of any fluid

inclusion study
• Make 100% sure that you study the correct sample
• Identify all fluid inclusion assemblages.
• Describe the fluid inclusion types in each fluid inclusion
assemblage
• Identify specific phenomena including homogeneous
trapping, heterogeneous trapping, leaking, imposion,
explosion, etc. in each fluid inclusion assemblage

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What have we done?

ü Some definitions
ü Fluid inclusion research
üLiterature
ü Descriptive classification
ü Daughter phases
ü Homogeneous /heterogeneous trapping
ü Primary and secondary inclusions (genetic classification)
ü Fracture healing
ü Roedder´s rules
ü Post-trapping modifications
ü Explosion /implosion decrepitation
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