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CONTENTS
PAGE
ABSTRACT
INTRODUCTION
givenoff by crushing
mineralscontaining
fluidinclusions
(5, p. 39; 8, 28), or
upon heating to decrepitation(30). Seldom,however,have these studies
beencombinedon the samesample,to obtaininformationon the concentration
of saltsin fluid inclusions.The first two papersin this series(23, 24) were
basedon a methodof obtainingan indirect estimateof the concentrationof
saltsin inclusions
from the depression
of the freezingpointof the fluids,as-
suminga knowledge of the approximate
composition of the salts. It wouldbe
highlydesirableto havea directmethodof extractionand analysisof fluid in-
clusionswhichwouldyield boththe composition and concentration
of the salts
in solution. For large fluid inclusionsthis determinationis not difficult,and
oneof the very earlypublications on fluid inclusions(8) describes
work of this
kind, involvingdrilling into a large fluid inclusionin quartz.
Another method,basedon analysisof the amountof water obtainedduring
decrepitationof a samplein a gasabsorptiontrain, followedby leachingof the
evaporatedresidueof solublesaltsfrom the decrepitatedsample,was reported
in this journal (21, p. 265-266). As the authorpointedout, however,this
methodhas somerather serioussourcesof ambiguity,suchas possiblelossof
ionsby diffusioninto the mineral surfacesfollowingdecrepitation.
The smaller the inclusionsthat can be studied,the wider the variety of
samplesthat canbe used,as smallinclusionsare far more abundantthan large
ones. This paperreportson a procedureinvolvingcrushingin a high vacuum,
follo•vedby carefulleachingand microanalysis; the resultsare usablein terms
of both concentrationof the salts and their composition,for single fluid in-
clusionslessthan 1 millimeterin diameter. It is bestsuitedfor samplescon-
tainingoneor a groupof reasonably largefluidinclusionshavinga total volume
of about 10 cubicmillimeters (10 mg or 0.01 ml), but also has beenusedsuc-
cessfullyon samplescontainingonly the normal small, but abundant,inclu-
sionsin about this sametotal volume. Although the methodis essentially
simple,it requiresconsiderable care in its execution.
SampleSelectionaud Preparation
As it is desirablewith thisprocedureto havethe fluidinclusionsin as small
a sampleof mineralas is possible,it is generallynecessaryto isolatefrom the
bulk of the specimensmall portionsof the mineral containingthe desired
inclusions.Althoughnormaldiamondsawsand rubber-bonded carborundum
cutoff wheels can be used for much of this work, the nature of some museum
material requires the use of thinner wheelsand more gentle cutting. This is
best obtainedthrough the use of continuousrim diamondcutoff wheels,made
by powdermetallurgyproceduresfor lapidaryuse. A very usefulsize is 4
inchesin diameterand only 0.015 inch thick. On delicatecrystalsor crystal
groups,it is sometimespreferableto usea commercially availablemicro sand-
blast unit. Although this is not designedfor deep cuts through hard min-
erals,it doesgive exceedinglygentleabrasiveaction,and with it very small
piecescan be cut out of the crystalswithout fracturing. Dark minerals of
STUDIES OF FLUID INCLUSIONS III 355
Vacuum
Gauge To High Vacuum--
--
Electric Furnace
yrex
Manometer
Copper
Copperff
sample ff
To Toepier
Backing Pump
tube
// D
FIG. 1. Vacuum line for recovery of gasesfrom fluid inclusions.
Relative deuterium
concentration in
Sample No. Run No. Mineral Location percent (variation
from Lake Michigan
water)
Garfield --9.8
H60-43 15/-3 Quartz crystals from miarolitic
cavities in granite of the An- quadrangle,
tero Formation of Stark and Colorado
others (26a)
Leachi•g
The object of the leachingprocedureis to dissolveout for analysisthose
water-solublesaltsthat were left behindby the evaporationof the water solu-
tion on crushingin the vacuumtrain. Obviouslyit is desirableto dissolveas
muchas possibleof thesesaltswith as little as possibleof the mineral. As the
total amountof saltsinvolved,per sample,may vary from 0.1 to a maximumof
only about3 mg, contaminationis a very seriousproblem.
Ordinarydemineralized water is completelyinadequate for the leachingand
filter preparation,and so must be passedthrough a speciallaboratory de-
mineralizerwhich yields water of one million ohms-cm -a resistivity (manu-
facturedby Betz LaboratoriesInc., Gillinghamand Worth Streets,Phila. 25,
Pa.). Although suchdemineralizedwater probablycontainsmore organic
matter than water redistilledin a fusedsilicastill (13), this doesnot affectthe
analysis,and the high electricalresistivity permits better control of the
leachingand analysisstepsas describedbelow.
High-gradeanalyticalfilter paperswere foundto havefar too muchsoluble
chlorideto be used for filtering the leach solutionfrom the crushedmineral.
Asbestosfilters were used instead,preparedas follows: High-grade acid-
washedchemicalfilter asbestos is first preparedby extendedboilingwith de-
ionizedwater, filtering,and repeatedwashingwith deionizedwater. A slurry
of this asbestoswith deionizedwater in a polyethylenebeakeris usedto make
a thin filter pad approximately20 mm in diameterin a porcelainGooch
crucible. The pad is washedwith large volumesof deionizedwater and then
checked for the presence
of solubleionizablematerialsby testingthe electrical
conductivity of high-qualitydeionizedwater beforeand after passingthrough
the filter, usinga high-sensitivityconductivitybridge. Any appreciable in-
creasein conductivitythroughcontactwith the filter indicateseither that the
360 ROEDDER, IA'GR./IM, ./IND H,4LL
Analysis, ppm
Leach solution M1 ppm by conductivity
Na Ca
Microa•mlysis
The major problemin the analysisof the fluid inclusionleachsolutionsis
the combination of very smallsamplesizewith very low concentration.Con-
centrationbeforeanalysisis practicallyalwaysruled out becausethe volumeof
the solutionis usuallytoo smallto gain any advantage. Methodswere chosen,
therefore,that couldbe usedto determineone tenth of a part per million of
eachion if a total of 20 ml of solutionwere availablefor analysis.
The following determinationswere made: sodium,potassium,calcium,
magnesium,boron, chloride, and sulfate, and lithium if the concentrationand
amountof solutionavailablefor analysispermitted. Sodium,potassium,lith-
ium, and calciumwere determinedflamephotometrically at the wavelengths
specified. The BeckmanDU spectrophotometer with flame attachmentwas
usedwith an oxygen-hydrogen burner of mediumbore. Magnesium,boron,
chloride,and sulfatewere determinedcolorimetrically
usinga BeckmanDU
spectrophotometer
for absorbancemeasurements.
Separatealiquots of the solution were taken for each determination. If
only 20 millilitersof solutionwere availablefor analysis,the aliquotstaken
would be approximatelyas follows: for magnesium,5; for chloride, 3; for
sulfate,2; for boron,2; andfor the flamedeterminations,
8. A description
of
the methodand other pertinentinformationfor eachelementfollows:
362 ROEDDER,I•\;GI?./tM,
,4ND H,4LL
oCodium.--Measurement
wasmadeat 589.3m•. Standards wereprepared
from reagentgradeNaC1,dried at 110ø C. The solutions
presented
no
problemfor this determination.
Potassiu•.•.--Measurement
wasmadeat 766.5m•. Standards
werepre-
paredfrom reagentgradeKC1, dried at 110ø C.
The sodiumcontentmaybe highenoughin somesamples(> 30 ppm) to
causeinterference
in the potassiumdetermination.This canbe checkedafter
thepreliminarydeterminationby preparinga standardcontaining
theapproxi-
mateconcentrationsfoundfor both potassium and sodiumand comparingit
with a potassiumstandard.If thereis a difference,
the potassium
shouldbe
determinedagain using mixed standards.
The potassium shouldbe at least0.1 ppmfor directmeasurement.
Lithium.--Measurement was madeat 670.8 m/•, usingthe blue sensitive
photomultiplier
tubeto gain extra sensitivity. Li2COa,acidifiedwith HC1,
was usedfor the standardlithium solution. The limit of determination,with
reasonablyaccuracy,is about0.01 ppm.
Calcium.•Measurement wasmadeat 422.7m•. Calciumcarbonate, acidi-
fied with HC1, was used for the standard calcium solution. It was standard-
izedby precipitating
calciumoxalate,ignitingit and weighingthe calciumas
calcium oxide.
The solutions
obtainedon leachingfluorideand sulfidemineralsmaypre-
sent a problem, as both fluoride and sulfate depresscalcium in the flame.
Testsshowedthat asmuchas 7 ppmof fluoridecouldbe toleratedbut that 10
ppmdefinitelyinterfered. Leachares from the fluoritesthat havebeenanalyzed
containedabout5 ppm of fluoride. If the calciumis 5 to 10 ppm, as muchas
30 ppm of sulfate can be tolerated, and most of the sulfide leachatesare
within theselimits. A_checkon interferencecanbe madeby comparinga cal-
cium standardwith a standardcontainingboth calciumand sulfateor calcium
and fluoride of the approximate concentrationin the leachate. If there is
interference,the calciumshouldbe determinedusingstandards that alsocontain
the interferingion.
The concentrationof calcium should be at least 0.05 ppm for direct
determination.
Ma•lnesium.--A colorimetricmethod involving 1-azo-2-hydroxy-3-(2,4-
dimethylcarboxanilido)-naphthalene-l'-(2-hydroxybenzene)
as the color rea-
gent was used (19). The reagent and a borax solution for buffering were
addedto an aliquotthat was just acid to phenolphthalein,
and dilutedto 25 ml
with ethyl alcohol. A'bsorbance was measuredat 505 m•. The methodcan be
used to measure0.5 to 10 •g of magnesium.
Even as little as one ppm of iron, copper,or aluminumcausessubstantial
interference,and suchsolutionscannotbe used directly. The interfering ions
were extractedwith 8-quinolinolin chloroform (18); the color can be de-
velopedusingthe extractedsolutionwithout additionaltreatment.
The extractionprocedurewas modifiedas follows: The entire extracted
solutionwas usedfor color developmentinsteadof an aliquotof this solution;
an extractionpH of 5 insteadof 7 was necessary;and a 1 to 1 ratio of aqueous
solutionto chloroformsolutionwas neededfor completerecovery.
STUDIES OF FLUID INCLUSIONS III 363
RESULTS OBTAINED
Prelimi•mryBulk Crushing7
Ru•s
During the developmentperiod a seriesof samplesrepresentinga variety
of geologicalenvironmentswere run to explore the potentialitiesand limita-
tions of the method. As it was desirableto try out the leachingprocedure
first, and to obtainan estimateof the ionic ratios to be expected,severallarge
sampleswere run by simplecrushingin air, followedby water leaching. The
sampleswere carefully picked and electrolyticallycleanedand the leaching
operationwas madeas similar to that describedaboveas the larger sample
sizewouldpermit. The larger leachsamplesizemadeit possibleto take opti-
mumaliquotsfor eachanalysisas well. The samplesusedin thesepreliminary
runs were as follows:
½ •e Leachate
analysis •o
ø Atomic
ratios
• • (ppm) • • ••
S•=p•e
No.* • Na • C• • C• • SO• • • •/N• C•/N••/N• m/N••/N• SO•/• C•/•
•59-k3 k078 388 •0.0 0.77 9.5 0.38 2•.k .... 0.39 •.44 54 0.0450.5•6 0.056k.59 --- 0.009 •5
ER59-1h 7• 106 6.8 0.548.8 0.2914.5 .... 0.26 31.19 •6 0.0470.743O.OhO
1.38 --- 0.009 18
•fRtm•
• 538185
6• 25322.91.23.8
16.70.• 4.60.97
1.044.9
35.50.01
O.O115.•
7.2 90.01
63.0491
61 0.031
O.115
0.030 O.Ohl
0.131 1.27
1.300.•
0.055 O.001O.161
0.103 2.8
2.4
501 251 18.6 0.98 4.9 0.92 39.8 0.O1 •.2 69.hl 70 0.0310.15 0.0471.59 0.001 0.054 3.2
•61-3&4 600 550 5.5 1.2 1.6 0.22 ll.6 0.06 0.Th 20.92 2& 0.15 0.1660.0381.370.023 0.032
Bl•k --- 138h0.02 0.02 0.05 0.02 0.Oh •.005 0.04 0.19 0.3• 0.6 1.h 0.9 1.3 ( 0.5 0.5 1.5
*Thetop six ar•lyses are all of samplesfromMississippiValley-type deposits.
Yacuum-crushi;•g
The vacuum-crushingprocedureitselfwastestedby runninga seriesof 14
samples,selected
mainlyon the basisof suitability
andavailability.The first
sevenwere from Mississippi
Valley-typedeposits.The natureand sourceof
thesesamplesaregivenbelow,andtheanalytical resultsobtained
are givenin
Table 4. All but one of thesesamplenumbersare referredto in the second
paperin this series(24). Althoughthe samesamplematerialwas usedfor
bothinvestigations,
differingsamplerequirements generallyprecluded the
application
of bothprocedures in sequence to the sameinclusions.The ap-
proximateoriginalconcentrations
of salts(NaC1equivalent) in thesesamples,
as estimated
from the freezingtemperatnres (24) for similarinclusions
from
thesamesamples,arealsogivenin thetableforcomparison withtheanalytical
determination.
Mineral Flaor. Fluor. Pluer. Fluor. Y~uor. Sphal. Sphal. Calc. Qzz. Sphal. Spbal. Sph•l. Sphal. Sphal.
H20 visual est. • ng !0 10 4 i 1 ? 1.• 7 75 23.2 3 fv•O 2-3 5 5
Ha0
vacuum
anal.•mg
• 6.9 lost 2.6 O.L4 los5
I•' 18.5 1.4 i18
i-/ 2hl J.0 4.26 3.• 1.7 5.Z
D/H rel. to Lake ]!ich. •0.1 -- +2.1 +0.9 -- +3.5 +1.4 -- -5.2 +0. i +2.6 - .s -2.3 +0.5
Leach vol.• P• 105.8 •2.1 21.0 7.2 •L.1 69.0 %5.7 32.9 ll.1 31.1 49.0 119 hl.2 55.4
Leachate analysis• ppm
?Is 3.• 16.5 7.5 4.4 2.7 19.3 1.8 O.kl 2.8i C.'} 5.2 C.20 0 .ES 2.7
K 0.79 0.8• 0.54 0.3,• C .28 0.•2 0.09 C.1! 0.10 C .3• 0.27 0.18 0.1• 0.L 9
Ca 5.2 13.0 5.6 !,1 6.1 C. '•9 ) .0 0.12 2.1 1.% 0.29 0.25 1.6
Mg 0.46 1.62 0.58 <0.2 0.21 0.82 <0.05 !.O <0.2 C.35 0.25 0.i0 0.07 0.22
C1 7.! 12.8 1 •.a 8.0 6.0 2.• 3.• <0.5 1.2 _!.l 2.• 0. '9 0.82 6.•
$ <0.01 <0.0• <0,037 <0.55 r.z. 0.Ol C .02 <0.Ol n.d. <0.Dl <c.01 <o.01 <c.c1 O.C1
Original consentration• d/
weight • of solution -•
N• 4.0• •,8 5.5 5.(- 9.012 0,C 7 7,16 5.0 0.72 C,65 2.5
C .27 C .003 0.011 O.3! 0.ø-6 0.65 C.32 0.46
K
Ca 0.35
0.862/ 3.35./
0.72
• 0
•.38 1.8 <0.11 0.CC'6 1.7 1.3'• hO v C.5B i .50
I•g 0.56 o .38 <c .25 6.24 <0.13 0.Oi• <0.613 C.2• C.2• 0.36 0.16 0.21
C1 8.7 9.'•6 10.05 12. • <0.0!'• 0.063 12.26 9. • 1.76 1.9 •'.56
B <0.01 <0.024 <0,75 0 .CO5 C .05 <0.0003 n.a. <0,GO8 <0.01 <0.036 <0.02 0.O!
S0• 0.12 0.18 5 .C <c .53 •- .2
0.067 0.063 0.3 0.45 1.80 1.15_ 0.6•
Total by anal. 14.6 15.9 23. 20.8 17.5 0.23 0.28 22.7 16.7 62• h.8 11.7
Total
byfreezin•
e-/ 19.9- 20.1- 19.4- -- •6.6- 0.0 0.7 13.0- 13.0- 4.2- • .2- 12.0
20.7 21.5 19.6 !T .o -5. • 13.4 5.O 5.0
a_/All sampleswere checkedfor noncondensablegasesand for COsmnz,,e '.'aca•. tzaih. All wezeat o•' belowthe sensitzvzzythresholmsfo• the me,ohods
i.e.• < x•g noncondensablegasesand < 0.1 mgCO•.
•_/ This is expressedin ppnNaC1equivalent; it includesprobablysignificant •-r',ounts
of ions novanalyzedfor• suchas Y-• Si03=, C03=•andHCOa•and
possiblyminoramounts
of Fe+++, AI++• etc.
•_• Theratios a•e indicatedas beingmaxima
whereversolubility of th• host•lnera! or analytzcallimit of sensitivity in•erferel,
c_/This is givenin unitsof millimicroequivalents
per ml of leachate,•.•. 10-• eq./m2,as the analyses
are irostconve-i•n
ßly converted
•o :ill.micro
per ml. Its sign is pos•tzve where an excess of cat ions was found, and v.
d• Obtainedby correcting the water dilution factor (ragleach solution/ragHaCin insiuszons)for tae concenvrationof salts found.
e_•(Yotained
fromsimilar inclusionsin the sameoriginal stumplos
(ref. 24); ass,•.inga pureNaC1-Hm0
system.
f_• Includes0.02 Li.
•/ Includes 0.01 Li.
h_/Calculationsfrom.comparison
of the analysiswith that of •R59-15wo4ldindicate about2.6 m• Ha0.
i_/ Weightloss determination--seetext.
• t•sed on •n •sslun•i correction of 4.5 ppm. Ca in the leachate,from solution of
FUTURE STUDIES
CONCLUSIONS
1. Nearly completequantitativechemicalmicroanalyses
of the saltsin
solution,as well as their concentration
in the fluid of fluid inclusionsin the
milligramrange,can be obtainedby the methodsdescribed.
2. The technique
permitsanalyses
of smallsamples,
andhenceof individual
zonesor inclusiontypesthat cannotbe obtainedin larger amounts,as well as
specimens with very few or small inclusions.
3. For many purposes,the eliminationof ambiguityof inclusionorigin
throughthe use of small samplesoutweighsthe lossesin analyticalprecision,
accuracyand completeness.
4. A numberof samplesyieldeddata on concentrationas determinedby
analysisthat are very similar to thosebasedon freezing data on similar ma-
terial; othersamplesgavevaluesthat are discordant, in part inexplicably.
$. The compositionsof fluid inclusions
in severalMississippiValley-type
deposits,althoughrather similar to eachother, differ considerably from the
compositions
of inclusions
in ore and ganguemineralsfrom all othertypes
of depositsstudied.
6. Suchdatacanbe usefulin understandingthe environmentof deposition
of ores and in delineatingthe conditionsunder which such processesas
dolomitization have occurred.
U.S. GEOLOG•C^LSURW¾.
W^SnI•GT0• 25, D.C.,
September 18, 1,o62
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