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Geology

Metal fractionation between magmatic brine and vapor, determined by

microanalysis of fluid inclusions
C. A. Heinrich, D. Günther, A. Audétat, T. Ulrich and R. Frischknecht

Geology 1999;27;755-758
doi: 10.1130/0091-7613(1999)027<0755:MFBMBA>2.3.CO;2

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Metal fractionation between magmatic brine and vapor,

determined by microanalysis of fluid inclusions
C. A. Heinrich
D. Günther*
A. Audétat
T. Ulrich
R. Frischknecht
Eidgenössische Technische Hochschule, ETH Zürich, Isotope Geology and Mineral Resources,
ETH Zentrum NO, 8092 Zürich, Switzerland

ABSTRACT
The major and trace element compositions of individual fluid inclusions from a range of
magmatic-hydrothermal ore deposits were analyzed by laser-ablation inductively coupled
plasma-mass spectrometry, to explore the behavior of ore-forming components during fluid
phase separation (“boiling”) in high-temperature saline fluid systems. Data from 13 samples
showing unambiguous evidence for coeval trapping of a liquid brine and a coexisting vapor
phase identify two groups of elements with drastically different geochemical behavior. Na, K, Fe,
Mn, Zn, Rb, Cs, Ag, Sn, Pb, and Tl preferentially partition into the brine (probably as Cl
complexes), whereas Cu, As, Au (probably as HS complexes), and B selectively partition into the
vapor. Fluid phase separation is probably a major, previously underestimated process in the
chemical differentiation that contributes to the extreme range of selective element enrichments
in magmatic-hydrothermal systems, from deep plutons through porphyry-style and greisen
deposits to epithermal mineralization and volcanic fumaroles.

INTRODUCTION ditions of mid-crustal plutons up to the Earth’s

Hydrothermal systems associated with inter-
mediate to acid magmatism give rise to a wide
range of ore deposits with variable element ratios,
from Cu-, Mo-, or Au-rich porphyries and skarns
(e.g., John and Ballantyne, 1998), to Sn-, W-, or
rare earth element (REE)–rich veins and greisen
replacements (Eadington, 1983), to more distal
lower temperature deposits rich in Au, Ag, As,
and Hg (Rye, 1993). The high degree of selective
metal enrichment results from the fact that sev-
eral element-fractionating processes are super-
imposed in large magmatic-hydrothermal sys-
tems, from the early partitioning of elements
during partial melting in the mantle, through the
separation of minerals and volatile phases during
magma ascent and crystallization, to the selective
precipitation of ore minerals by subsolidus reac-
tions between fluid and rock (e.g., Hedenquist
and Lowenstern, 1994; Shinohara and Heden-
quist, 1997). “Boiling” is an important process
driving precious-metal deposition in epithermal
deposits (e.g., Drummond and Ohmoto, 1985),
but the role of fluid phase separation as a mecha-
nism to actively segregate metals at higher tem-
peratures has not been systematically explored.
We know, however, that liquid brine and lower
density vapor can coexist from the solidus con-
*Present address: Laboratory for Inorganic Chem-
istry, Eidgenössische Technische Hochschule, ETH
Zentrum, 8092 Zürich, Switzerland.
surface (Bodnar et al., 1985; Fig. 1), and that low-
meteoric water
density gas-like fluids have a significant metal-
transporting capacity (e.g., Lowenstern et al., 1 km
1991; Wahrenberger et al., 1999). In this paper EPITHERMAL
DEPOSIT
we present new microanalytical data on the magmatic
vapor? 2 km
concentrations of ore-forming and other elements
in coexisting brine and vapor fluids from a range PORPHYRY
of intrusion-related deposits. These data indi- DEPOSIT 3 km
cate that chemical segregation of ore-forming brine-vapor
separation
elements by separation of brine and vapor is a ± refluxing
ubiquitous process, likely to affect the evolution 4 km
of magmatic-hydrothermal systems and the com-
deep external fluids
position of ore deposits across a wide range of 5 km
pressure (P) and temperature (T ).
brine + vapor
or supercritical fluid
LA-ICPMS MICROANALYSIS OF LARGE PLUTON 6 km
FLUID INCLUSIONS
We have optimized excimer laser-ablation Figure 1. Schematic section illustrating
inductively coupled plasma-mass spectrometry characteristic fluid environments of hydro-
thermal systems associated with calc-alkalic
(LA-ICPMS) for quantitative measurement of magmatism, where vapor-like fluid of low
multielement concentrations in fluid inclusions density and more saline liquid (brine) may
(Günther et al., 1998). Our instrumentation per- coexist. Large pluton at depth may exsolve
mits the controlled opening of individual inclu- one or two fluids upon crystallization. Por-
phyry Cu, Mo, and Au deposits are formed
sions that have been previously characterized by
by focused flow of high-temperature mag-
nondestructive petrographic and microthermo- matic brine and vapor through volcanic
metric analysis (Audétat et al., 1998). Apparent necks or veins. Au-, As-, Cu-, or Hg-rich epi-
salinity (NaCl equivalent wt%) provides an thermal ores are deposited in near-surface
internal standard for each inclusion, by relating environment from fluids of intermediate to
low salinity. Based on geologic relationships
element ratios from LA-ICPMS to a corrected documented by Dilles and Einaudi (1992;
Na concentration in the inclusion. In fluid inclu- Yerington, Nevada), and Hedenquist et al.
sions of ~20 µm diameter, absolute concentra- (1998; Lepanto, Philippines).

Data Repository item 9963 contains additional material related to this article.

Geology; August 1999; v. 27; no. 8; p. 755–758; 4 figures. 755

 Downloaded from geology.gsapubs.org on September 6, 2014
tions of major and trace elements are obtained
that range from tens of weight percent for Na, K,
and Fe down to detection limits below 10 ppm
for heavy trace elements such as Bi or Tl
(Günther et al., 1998). Recently detection limits
were further reduced to ~0.1 ppm for inclusions
of similar size, by using He as a transport gas
and by element-specific tuning of the ICPMS
(Ulrich et al., 1999). Analytical precision is
better than ±20% for most elements, but in-
creases close to the detection limit, or if an
element mainly ablated from a daughter crystal,
is integrated over the total ICPMS signal. Esti-
mated accuracy for trace elements such as Au is
within half an order of magnitude for a single
analysis, which is acceptable when concentra-
tions varying by seven orders of magnitude
(0.03–300 000 ppm) are investigated.
SAMPLE MATERIAL
The majority of the samples are from the
Sn-W mineralized Mole Granite in eastern
Australia (Eadington, 1983; Audétat et al., 1998)
and the porphyry-Cu-Au deposit of Bajo de la
Alumbrera in northwestern Argentina (Ulrich
et al., 1999). Additional samples were selected
from the porphyry-Cu-Au deposits of Grasberg
(McDonald and Arnold, 1994) and Bingham
(John and Ballantyne, 1998), a W-Sn vein of
Zinnwald (Tischendorf and Förster, 1990), and
the early mesothermal stage of a Pb-Zn-Cu vein
in the Madan district of Bulgaria (Petrov, 1985).
We selected quartz samples that contain trails of
fluid inclusions showing unambiguous textural
evidence for simultaneous trapping of coexisting
liquid and vapor (Fig. 2, Table 11 ). Such boiling
1GSA Data Repository item 9963, Table 1, is available
on request from Documents Secretary, GSA, P.O. Box
9140, Boulder, CO 80301-9140, editing@geosociety.org,
or www.geosociety.org/pubs/drpint.htm.
50 m
756
trails represent former fractures that were filled
partly with saline liquid and partly with vapor,
prior to healing and entrapment of the two fluids
as separate inclusions.
Cu-As-Au ENRICHMENT IN THE
VAPOR PHASE
Figure 3 shows results from 5 of the 13 samples,
selected to show the range in elemental fraction-
ation behavior. In each diagram, the average con-
centration of each element in the vapor inclusions
is plotted against the corresponding concentra-
tion in the coexisting brine inclusions. Error bars
denote uncertainties estimated from the scatter
(1σ) of all analyses of each inclusion type in a
sample, or upper limits where element concen-
trations were below detection. Results from all
samples (see footnote 1) indicate two consistent,
distinct trends in element behavior, despite varia-
tions in absolute concentrations: (1) liquid-parti-
tioning elements include Na, K, Fe, Mn, Zn, Rb,
Cs, Pb, and commonly Ag, Tl, Bi, Ba, Sr, Sn, W,
U, Ce; (2) vapor-partitioning elements always
include Cu and, where detected, As, Au, S, Sb, B,
and sometimes Li. Elements from the liquid-
partitioning group typically show identical con-
centration ratios between liquid and vapor in
each sample, as indicated by the lower dashed
45° line in the log-log plots of Figure 3, but abso-
lute concentrations and the ratio of any metal
concentration in the vapor (V) to its concentra-
tion in the liquid (L), MV/ML, vary significantly
between samples. Of the vapor-partitioning ele-
ments, Cu consistently plots above the line repre-
senting the average MV/ML ratio of the liquid-
partitioning elements (e.g., Fig. 3D). In 9 of 13
samples, the absolute concentration of Cu is
higher in the vapor phase, as much as 24 times
compared with the saline liquid (Fig. 3, A–C, E).
Arsenic shows the same tendency to be fraction-
ated by the vapor phase, although sometimes to a
A B
liquid
vapor halite
brine
liquid
lesser degree than Cu. The same is true for B, Sb,
and Li in some of the samples. S, for which
ICPMS has relatively poor sensitivity, has been
semiquantitatively analyzed in one of the Mole
Granite samples. Here it occurs at a level of about
1 wt% in the vapor, but at most 0.1 wt% in the
brine. In the sample from the Grasberg porphyry
Cu-Au deposit, Au is variably enriched in the
vapor, on average by the same factor as Cu and
As (Fig. 3E; Ulrich et al., 1999).
TENTATIVE THERMODYNAMIC
INTERPRETATION
High ratios of Cu to other heavy metals in
magmatic vapor have previously been observed
by Sawkins and Scherkenbach (1981), Heinrich
et al. (1992), Bodnar (1995), and Damman et al.
(1996), but geochemical interpretations remained
ambiguous for lack of clear temporal relation-
ships between the contrasting fluid types. The
data presented here leave no doubt that selective
enrichment of Cu and some other elements in the
low-density vapor is a result of equilibrium frac-
tionation between coexisting fluid phases.
To explore the thermodynamic factors that
may cause this effect, we evaluated the degree of
element fractionation for each boiling assem-
blage using the following ratio:
CuV M V
Q= , (1)
Cu L M L
where Cu and M represent the concentrations of
Cu and a liquid-partitioning metal, M, in the
superscripted fluid phases.
Average values of Q were calculated from
liquid-partitioning elements that were well
above detection in both inclusion types (M = Na,
K, Fe, Mn, Zn, Rb, Cs, Pb; see footnote 1). The
value of Q (unlike individual concentration
values or the distribution coefficient of one ele-
gas
Figure 2. Photomicrograph
of boiling trail (A), healed
20 m fracture that trapped co-
existing brine (detail in B),
and vapor (C) in quartz at
high temperature (Bajo de
C la Alumbrera porphyry Cu-
Au deposit, Argentina).
gas
20 m
GEOLOGY, August 1999
 Downloaded from geology.gsapubs.org on September 6, 2014

ment between the two fluids, D = CuV/CuL ) does

not depend on assumptions for the internal
standardization of our analyses using micro-
thermometric data for Na. However, the Q values
are minimum estimates for the actual exchange
constant between the two end-member fluids,
because minor coentrapment of brine in the
vapor-dominated inclusions is possible (Fig. 4).
Minor admixture of brine in the vapor inclusions
would also smooth out differences among the
surprisingly similar distribution coefficients of
all liquid-partitioning elements in each sample
(lower dashed 45° lines in Fig. 3).
Considering the phase relationships in the
system NaCl-H2O (Bodnar et al., 1985) and
limited experimental data on metal chlorides in
two-phase hydrothermal systems (Hemley et al.,
1992), one might expect that selective fractiona-
tion of minor components between salt + water–
dominated fluids is most significant in a window
of intermediate P-T conditions. If the degree of
metal fractionation was primarily controlled by
P, T, and the density or salinity contrast between
the coexisting fluids, then Q should be largest at
low P, where the solvus in the NaCl-H2O system
is widest, and decrease toward higher pressures
(at any temperature) to finally approach 1 at the
critical curve along the crest of the solvus. The
variation of Q derived from the natural brine and
Figure 3. Elemental concentrations in vapor
vapor pairs only partly reflects such variations in and coexisting brine inclusions for five sam-
physical conditions or fluid properties. Consid- ples from boiling magmatic-hydrothermal sys-
ering only the samples from the Mole Granite tems. Note consistent fractionation of Cu (and
(patterned rectangles with Q values marked in Au, As, Sb, and B where detected; squares) in
Fig. 4), there is a tendency to greatest fractiona- favor of vapor phase, relative to consistently
liquid-fractionating elements (circles). Fraction-
tion in samples representing low P and large ation constant Q refers to equation 1 in text.
differences in salinity between the two fluids.
The entire data set including the porphyry
Cu-Au deposits, however, does not show any
relationship between Q and the physical parame-
ters (P, T ) or bulk properties of the NaCl-H2O–
dominated fluids.
These observations indicate that chemical
factors, related to components other than NaCl-
H2O, control the degree of metal fractionation
between the coexisting fluids. Metal speciation in
the two fluids mainly depends on complexing
ligands. Of the two geologically most important Figure 4. Pressure vs. composition phase
ligand components, Cl has a strong tendency to diagram of NaCl-H2O model system; thin lines
fractionate into the saline liquid, whereas S delineate two-phase region in which lower
preferentially fractionates into the vapor phase salinity vapor and high-salinity liquid (brine)
(Drummond and Ohmoto, 1985). coexist. Small rectangles indicate composi-
tions and pressure-temperature conditions of
We suggest that the liquid-partitioning ele- two-phase fluid entrapment estimated from
ments enter the chloride-rich brine due to prefer- microthermometric measurements of brine
ential Cl – complexation, whereas HS – complexa- inclusions. Horizontal lines extend to lowest
tion is responsible for the selective fractionation salinity measured in coexisting vapor inclu-
sions, which probably cotrapped some prefer-
of Cu, Au, and possibly As and Sb into the vapor entially surface-wetting brine. Numbers in
phase. This explanation is consistent with limited bold italics are minimum values for equilib-
experimental data by Hemley et al. (1992), rium fractionation constants (Q, equation 1).
Mountain and Seward (1999), and recent obser-
vations on synthetic fluid inclusions (Frank et al.,
1998). Our analyses of Au in fluid inclusions
confirm the prediction of Heinrich et al. (1992)
that the high stability of Au(I) bisulfide (Benning

GEOLOGY, August 1999 757

 Downloaded from geology.gsapubs.org on September 6, 2014
and Seward, 1996) should cause Au to preferen-
tially partition into a vapor phase rich in S. The
observation that the tendency for vapor fractiona-
tion of Cu is greatest in Sn-W veins (Fig. 4) could
reflect the predominance of reduced S in such
granite systems. In porphyry Cu-Au systems, Q
is consistently smaller, perhaps because much of
the S in such systems occurs in oxidized form as
SO2 (Burnham and Ohmoto, 1980), which is in-
effective for Cu and Au complexation.
GEOCHEMICAL IMPLICATIONS
The geological consequences of brine-vapor
separation as a mechanism to segregate elements
and selectively enrich certain metals in different
types of ore deposits could be profound, but are
still poorly understood. Brine and vapor not only
have contrasting densities, but also vastly differ-
ent viscosities. These contrasts in physical prop-
erties will facilitate the separation of big volumes
of fluids and promote large-scale selective element
transport—particularly in the dynamic environ-
ment of magmatic-hydrothermal systems in
continental and suboceanic settings.
In magmatic fluids of intermediate to high
salinity, Fe probably occurs in excess over S
(Hemley et al., 1992), and simple cooling of
such a fluid will deplete the solution in S by pre-
cipitation of Fe-(Cu)-sulfides. As a consequence,
some or all of its Au will precipitate, as indicated
by the intimate association of Cu and Au in
porphyry Cu-Au deposits (Ulrich et al., 1999).
Vapor separation from brine is an effective
mechanism to generate a fluid with high sulfide
content, but relatively low concentration of Fe.
Cooling of a vapor rich in S-Cu-As-Au at ele-
vated pressure (or its condensation into nonmag-
matic water at lower temperature) will generate
a fluid of liquid-like density and a salinity below
~10 wt%. Such a fluid will precipitate some
Cu-Fe-sulfides upon cooling but, due to its sul-
fide excess, will be able to transport a high con-
centration of bisulfide-complexed metals such as
Au down to low temperatures. High-sulfidation
epithermal Cu-As-Au deposits (Fig. 1), the deep
fluid reservoir of low-sulfidation epithermal sys-
tems (Berger and Henley, 1989), and the enig-
matic Carlin-type Au deposits (Cline et al.,
1997) all show some geochemical and geologic
characteristics that could be explained with the
input of an Au-rich magmatic vapor.
ACKNOWLEDGMENTS
We are grateful to M. Einaudi, J. Hedenquist,
S. Matthai, T. Seward, H. Shinohara, and V. Wall for in-
spiring discussions and reviews. We thank J. Angera, P.
Ashley, and P. Petrov for samples and help in the field.
Support by Eidgenössische Technische Hochschule
Zürich, the Schweizerische Nationalfonds, and MIM
Exploration is appreciated.
758
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GEOLOGY, August 1999