JOURNAL OF GEOPHYSICAL RESEARCH, VOL. 105, NO.

B1, PAGES 783-794, JANUARY 10, 2000

Rock magnetic properties related to thermal treatment

of siderite: Behavior and interpretation

YongxinPanandRixiangZhu
Instituteof GeologyandGeophysics,
Chinese
Academyof Sciences,
Beijing

SubirK. Banerjee
Institutefor RockMagnetism
andDepartment
of GeologyandGeophysics,
Universityof Minnesota,
Minneapolis

J. Gill and Q. Williams

EarthScienceBoard,Universityof California,SantaCruz

Abstract. Detailedanalysesof rock magneticexperimentswere conductedon the oxidation

productsof high-puritynaturalcrystallinesideritethat were thermallytreatedin air atmosphere.
Susceptibilitiesincreasesharplybetween400ø and 530øC indicativeof somenew ferrimagnetic
mineralphasegeneration.Both a drop(between540ø and 590øC)on the heatingcycleand a
dramaticincrease(from 590øCto 520øC) on the coolingcycle occurredand are well consistent
with the characteristicof magnetite.A distinctHopkinson-typesusceptibilitypeak indicatesthat
hematiteis the terminalproductif sideriteis heatedto 700øCover and over. It hasbeenrevealed
in detailthatthe originalinversemagneticsusceptibilityfabric contributedby the crystalline
anisotropyof sideritein siderite-bearing specimens is changedto a normalmagneticfabricduring
incrementalheatingover410ø-490øC.This is a resultof dominantcontributions from the
distributionanisotropyof newly transformedferromagnetic minerals.A strongchemical-viscous
remanentmagnetizationcouldbe producedduringsideriteoxidationin an externalfield. Rock
magneticexperimentalresultsshowthat magnetite,maghemite,andhematiteare the
transformation productsof high-temperature oxidationof sideritein air. Maghemitewas not
completelyinvertedto hematiteevenat temperatureashigh as 690øCduringincrementalthermal
treatments.The mineral transformationprocesseswere confirmedby conventionaloptical
microscopicobservation,X-ray diffractometryandM6ssbauerspectroscopic analyses.These
resultsindicatethat the rock magneticmethodsusedhereare reliableand highly sensitivein
detectingvery smallmagneticphasechangesin rocks.We concludethatthesetemperature-
dependentvariationsof magneticpropertiescanbe usedas criteriafor identificationof sideritein
rocksandsediments. Furthermore,it is clearthatgreatcareshouldbe exercisedin thermal
demagnetization of siderite-bearing
rocksin paleomagnetic,magneticanisotropy,and rock
magneticstudies.

1. Introduction propertiesboth at the ordinary ambient and elevated thermal

environmentsare very important for reliable interpretationsin
Recently,a substantiallyincreasednumberof observations of paleomagnetism,magneticfabric, and environmentalmagnetism
magnetic minerals other than magnetite in natural rocks has investigations.
initiated studies of their fundamental magnetic properties
Siderite (FeCO3) is an authigenic iron-bearing carbonate
[Courtillot, 1996]. It has been shown that the magnetic commonin many diverse sedimentarysettings,particularlyin
susceptibility of weakly magnetic rocks can be affected
marineandlacustrineenvironments [Ranganthan and Tye, 1986;
considerablyby the presenceof paramagneticminerals whose
Baker and Burns, 1985; Ellwood et al., 1988]. Thermal
susceptibilityis temperaturedependent[e.g. Rochette, 1987; decompositionand oxidation of the mineral siderite has been a
dover et al., 1989,' Hrouda and delinek, 1990; Hrouda, 1994].
topic of considerableinterestfor many yearsbecauseof both its
Dramaticchangesof anisotropyof magneticsusceptibility(AMS)
commercialimportanceand scientificquestionsregardingthe
andpaleomagnetic directionduringheatingof siderite-containing
progression of alterationproducts[BaginandRybak,1970,'Nagy
sampleshave also beennotedin earlier studies[e.g., Ellwood et et al., 1975; Zakharovand Adonyi 1986; Criado et al., 1988;
al., 1986, 1988]. Therefore knowledge of alterationsof iron-
Dubrawski,1991].Nevertheless, decomposition of sideritein air
bearing paramagneticminerals and associatedrock magnetic is still poorly documented. For instance,debatesstill remainas to
the occurrence andstabilityof the transitional
spinelphasessuch
as magnetiteand maghemitein sideriteoxidation[e.g., Hus,
Copyright
2000bytheAmerican
Geophysical
Union.
1990]. Pure (paramagnetic)sideritecrystalshave a very large
Papernumber 1999JB900358 anisotropy, the c-axis correspondingto the maximum
0148-0227/00/1999JB900358509.00 susceptibilityaxis [Rochette,1988]. Demagnetizationof low-
783
784 PAN ET AL.: ROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE

temperatureremanenceon siderite-bearingmarinesedimentsafter Geophysics,Chinese Academy of Sciences.The magnetic

cooling in zero field and in a 2.5 T field both displayed large susceptibility
(r) and AMS of all specimens
were measuredon
remanencelosses from 20 K to 40 K [Housen e! al., 1996]. KLY-3s spinnerKappabridge(AGICO, Czech Republic)both
Sideriteis in fact antiferromagnetic
with a Neel temperatureT•vof before and after thermal treatment. The successive variations of
38 K [Jacobs,1963]. It is paramagneticat ordinarytemperatures; susceptibility
with bothlow andhightemperatures weremeasured
thereforeit carriesno natural remanencein rocks and is usually on a BartingtonMS2 and KLY-3s/CS-3(L). Stepwisethermal
overlooked by most paleomagnetists.However, siderite is treatmentsof specimens wereconducted in a MMTD60 (Magnetic
compositionallyunstableand susceptibleto oxidation [Seguin, Measurement)thermal demagnetizerat 150ø, 200ø, 250ø, 300ø,
1966] and can acquire chemical remanentmagnetizationin its 350ø, 380ø, 400ø, 410ø, 420ø, 430ø, 450ø, 490ø, 510ø, 520ø, 530ø,
oxidation process.In even a small stray field, the chemical 550ø, 580ø, 610ø,640ø, 680ø, 700ø and720øC(keepingspecimens
remanencewas strongenoughto overshadowthe naturalremanent for 40 minutesat eachhold interval).The impartingof an IRM
magnetization of the samples being studied, effectively and back-fieldremovalof a saturatedisothermalmagnetization
terminatingthe thermal demagnetizationrun [e.g., Zhou e! al., (SIRM) wasconducted on a 2G660pulsemagnetizer in fieldsup
1991;DunlopandOzdemir,1997;Pan et al., 1998].Ellwoodet to 2.7 T. Remanences were measuredon a 2G-755R cryogenic
al. [1989] useddifferent methodsto characterizethe behaviorsof magnetometer in a field-freespace.Curiebalanceanalyseswere
siderite and ankerite. Hus [1990] found that room temperature performedin the tectonophysics laboratoryat the ChineseSeismic
oxidation of siderite created hematite, which acquired a field- Bureau.
controlled, very stable crystalline remanent magnetizationand The sample oxidation productsof heated sideriteused for
concludedthat siderite heated in air did not show magnetic magnetic measurement experiments were analyzed by
interactionsbetween the dissociationproducts hematite and conventionalmineralogicalmethods.The XRD analyseswere
maghemite.Hirt and Gehring[1991] studiedthe low-temperature performedby meansof D-MAX2400 X-ray diffractometer.The
bulk susceptibilityand isothermalremanentmagnetization(IRM) differentialthermalanalysis(DTA) andthermalgravityanalysis
of the Northamptonironstoneand concludedthat siderite-rich (TGA) were measured on a Shimadzu DTG-50H thermal
sampleswere mineralogicallystablein air over years,in contrast analyzer. The M6ssbauer spectroscopyanalyses at room
to Ellwood e! al.'s conclusion.In fact, precise knowledge of temperature were conducted on a conventional constant-
magnetic properties associatedwith the thermal treatment of acceleration
spectrometer
with 25mCi57Co(Pd)source.
sideritein air is lackingat present.
In this study, we use natural crystalline,high-purity siderite 2.2. Results
specimensto investigatemagneticpropertiesand mineral phase
variations associated with its oxidation in thermal treatments in 2.2.1 Magnetic susceptibility(•:) measurements.Mean bulk
air. For tke sake of further identifying mineral transformations,a susceptibilityof cylinder specimensat room temperatureis
groupof conventionalmineralogicalmethodswasusedin addition approximately (3.5+0.5)x10'3SI. Variations of volume
to rock magnetic means. Besides, a set of experimentswas susceptibilitywith temperature,K(T), oftenallow identification
of
designed to examine the secondary remanent magnetization most paramagneticminerals [Rochette e! al., 1992] whose
producedby the sideriteoxidation. susceptibilityvariesaccordingto the Curie-Weisslaw: r=C/(T-O).
C is a constantproportional to the amountof paramagnetic ions,
and 0 is the paramagneticCurie constant, linked to the
2. Experiment Results concentrationof ions in the mineral and to the type magnetic
interaction. Low-temperaturemeasurementsof the powdered
2.1. Sample Description and Instrumentation
for the Measurements
siderite-bearing specimens, starting from liquid nitrogen
temperature (-196øC), show that r decreaseslinearly with
Big fresh block samplesof natural crystallinesiderite were increasingtemperaturetill room temperatureat which time the
collectedfrom a newly cut undergroundsidewall at Dalizi iron susceptibilityreached nearly two -thirds of preheatingvalues
mine in Jilin province,the northeasternChina [Li and Yin, 1983]. (Figure 1). From the prior work of Jacobs[1963] the value of 0
Sideriteblock samplescould be easily chosenbecauseof the for powderedsideriteis approximately0 K. Thereforethe ratio of
presenceof well-crystalline coarse-grainssideriteand their very susceptibilitiesat-196øC to room temperatureshouldequal the
highpercentage in the deposit.X-ray diffraction(XRD) analysis inverse ratio of absolute temperatures(i.e., 297/77=3.8). Our
andthinsectioninspection indicatethepresence of approximately results (3:1) are similar to this calculated value, indicating
95% siderite with accessoryquartz and calcite in the block characteristics of paramagnetism.
samplesstudied.In the laboratory,cylindricalsideritespecimens High-temperature susceptibilitieswere measured every 2
(with 2.5 cm in diameterand2.2 in height)weredrilledfrom the secondsaspowderedsideritespecin•enswere successively heating
block sample,and syntheticsiderite-bearing cubic specimens up to 700øC and back to room temperaturein air atmosphere
(with 2 cm sides)werealsomadefor rockmagneticexperiments. (Figure 2). Susceptibilitieson heating cycles decreasedbefore
The cylindricalsideritespecimens are composed of nearly95% reaching 250ø-300øC, indicating the dominant contributionof
siderite.The siderite-bearing cubicspecimens were madeby a paramagnetic siderite. After 400øC, however, susceptibilities
mixtureof evenlydispersed powdersiderite(<280-74 pro),which increased sharply, indicative of the generation of new
waspreciouslycrushedin an agatebowl, with nonmagnetic kaolin ferrimagneticmineralphase.The changein shapein susceptibility
clay matrix in the weight ratio of 1:15. Separatetemperature- at 540ø-590øC indicates the Curie temperatureof magnetite.
dependentrock magnetic checks for blank clay specimens Susceptibilityvalueswere significantlyenhancedafter a thermal
demonstrated thatmagneticinfluencescausedby the clay matrix treatment run to 700øC.
in thermaltreatmentwerenegligible. Repeated stepwiseheating of the same specimento high
All magnetic measurements were conducted at the temperatures indicates that paramagnetic susceptibilitieson
paleomagnetism laboratoryat the Institute of Geology and heating and cooling cycles are reversibleto 300øC (Figure 3a),
 PAN ET AL.: ROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE 785

1.0 the beddingplaneswhile Kma x axeswent to the beddingplanes.

We note that the movement rates of the principal axes were
affectedby the grain size of siderite;they obviouslyslow down
• 0.8
with increaseof grain size (seeFigures6a to 6c). AMS resultsof
blank specimensremainedstable(Figure 6d) and they manifest
o• 0.6 _ that the exchangeof principal axes resultedfrom alterationsin
siderite.Contraryto the very high anisotropydegreein a natural
crystalasreportedby Jacobs[1963],the anisotropy degree(P) of
._N 0.4 siderite-bearingspecimenswas very low (generallyfrom 1.02-
E 1.05). The P was constantuntil 250øC, then decreasedto a
o minimum value at 410øC [P•I], and then increasedremarkably
z 0.2
with further temperatureincrease (Figure 7a). The shape
parameterq changedfrom q>0.69 to q<0.69 (Figure7b) while T
0.0 , I , I , I , changedfrom-I<T_<0 to 0<T_<I,respectively. In otherwords,in
-200 -150 -100 -50 0 thermaltreatmentsAMS ellipsoidsof siderite-bearingspecimens
Temperature (øC) changedfrominitialprolateto an oblateellipsoid.
2.2.3. Curie temperature analysisand isothermal remanent
Figure 1. Low-temperaturesusceptibilitybehavior for nine magnetization(IRM). Curie temperatureanalysison a fresh
siderite specimens upon heating from the liquid nitrogen powderedsideritespecimen wasperformedin air atmosphere. It
temperature(- 196øC).
showsan apparentlyparamagneticsignal upon initial heating
(Figure8). A pronounced increasein magnetizationbetween450ø
and560øCindicatesthe creationof a ferrimagneticmineralphase,
followedby irreversiblecurveswith ferrimagnetic characteristicswith a Curie temperatureof approximately580øC, which is
in subsequenthigher temperatureheating runs, suggestingbasicallyconsistentwith the susceptibility results(seeFigure2).
continuousoxidation effects. In the 400 ø, 450 ø and 530øC runs, On coolingbelow the Curie temperature, a strongmagnetization
susceptibilitieson coolingcyclesare obviouslyhigherthan increasedsmoothlyand continuouslydown to room temperature.
heatingcycles,indicatingthe transformation of sideriteto a Clearly,magnetiteis createdin thethermaltreatmentof siderite.
strongly magneticphase(Figures3b,3c,and3d).On thecontrary, The stepwiseacquisitionof SIRM in fields up to 2.7 T were
in the 580ø, 630ø, 680ø, and 720øCruns,susceptibilities on the conducted on siderite-bearingcubic specimens that were
coolingcurvesarebelowtheheatingcurves,suggesting thatthe incrementallyheatedto differenthightemperatures. The SIRM of
new magneticphasewith a Curietemperature of approximatelyspecimens heatedto 400øCwas clearlyincreased and about90%
590øCwasoxidizedto relativelyweakermagneticphases(Figures of the saturatedIRM could be acquiredin a field of 200 mT,
3e, 3f, 3g). Finally,a muchlowersusceptibility phasewith a suggestinga soft magneticmineral has been createdin the
distinctHopkinson-type peakaround670øCwas formedduring specimen.A maximum value of SIRM was observedon
the 680øCrun (Figure3h). Susceptibility variationsmeasured at specimens heatedat the 490øCrun (Figure9). Then the SIRM
roomtemperature on siderite-bearingspecimens after stepwise decreased.The unsaturatedtrend of IRMs on the specimens
thermaltreatments (Figure4) arein accordwith thestepwise •c(T) heatedto over680øCsuggests thata hardmagneticmineralphase,
curveresults(Figure3). probablyhematite,has been createdin the highesttemperature
Ther(T) curvesmeasured ona specificspecimen thatwasfirst oxidationproducts.
heatedto 510øCand then repeatedlyheatedto 700øC for five Figure 10 shows progressiveacquisitionand subsequent
successiverunsalsoindicatethatwith prolongedheating siderite reverse-fieldremoval of the SIRM on siderite-bearingspecimens
is decomposed and oxidized completely,changingfrom a stepwiseheatedafter 530ø, 580ø, 640ø, 680ø, 700ø, and 720øC
paramagnetic
phaseto a verystrongly
magnetic
phaseandfinally
to a magneticphasewith low susceptibility
and a distinct
100.00
Hopkinson-type
peakaround670øC(Figure5).
2.2.2 Anisotropy of Magnetic Susceptibility (AMS).
Seventeensiderite-bearing cubic specimenswere heatedin a
•,10.00
MMTD60 thermaldemagnetizer in a zero field up to 680øCat
intervalsdescribedearlier in section2.1. For comparison,three
blankcubicspecimens wereheatedandmeasured at thesametime 1.00
..,-x.
o ß

whenthe siderite-bearing specimens were measured. Beforethe

first heatingrun, it was observedthat all 17 siderite-bearing
specimens showedthe maximumprincipalaxes Kma
perpendicular to thecompactionplanes (equivalent
x to be
tothebedding ••c•
'0.10
planesin sedimentary rocks),that is, inversemagnetic fabric 0.01
according to the definitionof Rochettee! al. [1992]. In the
followingincremental heatingruns,the inclinationsof Kmax axes
remainedin their originalpositionsuntil heatedduringthe 200øC 0.00 i i i i i i i
0 100 200 300 400 500 600 700 800
run. They then moved rapidly away from pole positionsto the
beddingplanesafter heatingduringthe 350ø-490øCruns,while Temperature(øC)
the axesof minimumKm•,movedin contrarydirectionsto the pole Figurc 2. Representativehigh-temperaturesusceptibility(•c-T)
positions(Figure 6). Finally, Kmi,axesbecameperpendicular to curve of powder siderite specimensheated in air. Solid (open)
circlesrefer to heating(cooling)data.
786 PAN ET AL.' ROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE

100.00 100.00

300 øC 400øC
10.00 - 10.00

1.00 - 1.00

0.10 - 0.10

0.01 - 0.01

0.00 0.00
' I ' I ' I "
0 200 400 600 800 0 200 400 600 800

100.00
100.00450øC 530øC
10.00
10.00'! .........
..

1.00
•.oo .

0.10 - 0.10

0.01 - 0.01

0.00 - 0.00
' I ' I ' I ' I ' I '
0 200 400 600 0 200 400 600 800

100.00 100.00

58oøc e 630 øC
10.00 - 10.00

1.00 - 1.00

0.10 - 0.10

0.01 - 0.01

0.00 0.00

0 200 400 600 8OO 0 200 400 600 800

100. O0 100. O0

10.00- 680øC g 10.00 720øC h

1.00 1.00

0.10 0.10

0.01 0.01

0.00 ' I ' I ' I '' 0.00

0 200 400 600 800 0 200 400 600 800

Temperature/øC Temperature/øC
Figure 3. High-temperaturesusceptibility(K-T) curvesof a sideritespecimenstepwiseheated to different
temperature
in air. Solid(open)circlesreferto heating(cooling)data.

runs. It shows that the SIRM was attained under 0.11 T and the
remanent coercivities (Hcr) are approximately 22-•23 mT,
consistentwith the characteristicsof magnetite(Figures10a and
10b). Evidently, inflectionpointson acquisitionand reverse-field
curvesshowthatbotha softcomponent(saturatedand lowerHcr)
and a hard component(unsaturated and higherHcr) coexistedin
the specimenafter 640øCruns(Figure 10c).The Scrof specimens
and contentof the low coercivitycomponentdecreasedwith the
treatment temperaturerise, indicating a soft magnetic phase
transformedinto the hard magnetic phase with the high
temperatureincrease(Figures 10d-1Of). The product after the
720øC run is very coercivewith Scr of 980 mT. Taking into
accountthe data on susceptibilities(e.g., Figure 3h), the hard
magneticphaseis explainedashematite.
To identify the ferromagneticmineralstransformedat high-
temperature treatments following Lowtie [1990], three-axis
different coercivity IRM componentswere magnetized in
successivelysmallerfieldsalongthreeperpendicular directionson
 PAN ET AL ßROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE 787

lOO

oo

ß ß o

e i e • eee#$

[] [] [] []

.Ol -

.OOl
o 1 O0 200 300 400 500 600 700 800
Temperature (øC)
Figure 4. Changesin the susceptibility
(•:) measuredat room temperatureof sevendifferentsiderite-bearing
specimensafter incrementalheating.Note that the squaresstandfor susceptibilities
of a blank clay matrix
specimen.

100. O0

•, 10.00
high
temperature:
510øC a 100.00
] ,,, b

>, 1.00

ß 1.00
1
.--

Q. 0.10 •.
j
mill
i
0.10
• 0.01

0.00
' I ' I ' I '
0.01
1 '
O.001 I ' I ' I '
200 400 600 800 0 200 400 600 800
100.00
100.00
m 10.00 10.00

1.00 ø% 1.00
%,
,--
--
._

%, o©
:• 0.10 0.10 o

o©

• 0.01 0.01

0.00 0.00
' I ' I ' I ' ' I ' I ' I '
200 400 600 800 200 400 600 8OO

100.00 100.00

e f
0.00 10.00

1.00 • 1.00

0.10

0.01 0.01

0.00
' I ' I ' I:
200 400 600 800
0.00 i 0 200
I , • ,
400 600 800

Temperature (øC) Temperature (øC)

Figure 5. High-temperature
susceptibility
(•:-T) curvesof a sideritespecimenduringsuccessive
heatingto 700øC
(exceptfor the first run, 510øC),from Fifure 5a to 5f.
788 PAN ET AL.: ROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE

N N
+
+
+
+

-F
300
-F
0-250
+++++++ ++++++++ +++++++ 040•-++++++

N N

Figure 6. Exchangein the orientationof theprincipalaxesof the AMS ellipsoidafterheatingthe specimens. Solid
squaresandsolidcirclesrepresenttheKma XandKin,n,respectively,andthe thermaltreatmenthigh-temperatures are
indicatedbeside.(a, b, c) Siderite-bearingspecimens with sideritegrainsize of <74 gin, 74---154gm and 154---280
gin, respectively,(d) Blank clay matrixspecimenin comparison.

heatedsiderite-bearing specimens, thenthermallydemagnetized at of sideriteand the characteristicsof remagnetizations carriedby

intervalsof 100ø to 20øC. In the productsheatedafter580ø, 610ø
and 640øC runs, the magnetizationcarried by the medium
components (0.05-0.5 T), whichis the majorremanencecarrierin
heatedproducts,decreasedrapidly in the temperaturerange of
200ø-300øC.This may indicate an inversionof maghemiteto
hematite(Figure 11). The soft components (<0.05 T) exhibited
evidenceof magnetitewith unblockingtemperatures of 580øC,
while the hardcomponents (0.5-2.7 T) indicatedthe presenceof
hematite with a Curie temperatureof 670øC. In contrast,
productsheatedafter 720øCrunswere obviouslydominatedby
hematitewith distinctCurie temperature at 670øC(Figure 1l d),
while theirmagnetization reductionbefore300øCmightindicate
the existenceof a little maghemite.Thereforeit is clear that
maghemiteandhematiteare the mainmagneticmineralphasesat
high- temperature treatmentruns.It explainswhy the valuesof •c
andSIRM decreased whiletheHcrincreased with temperature
rise
after 540øC runs in stepwisethermal treatmentsas shown in
Figures5, 9, and 10.
2.2.4. Chemicoviscousreinanent magnetization (CVRM)
experiments. Taking account of the mineral phase
transformations of siderite,we examinenow the thermalstability
oxidationproducts of sideritethroughheatingof specimens in the
presence of an externalmagneticfield. One groupof cylindrical
sideritespecimens washeatedto 250øCfor up to 12 hourswith a
steady field of 50 •tT (referred to as the field-constant-
temperature, FCT experiment).Room-temperature remanences in
the FCT experimentswere measuredat 1-hour intervals.
Surprisingly,susceptibilities
werebasicallyunchanged in thetotal
12-hour-longheatingin FCT experiments(Figure 12a), in part
indicatingno magneticmineralchangeandshowingtherelatively
high stabilityof the crystalsiderite.Severalmonths'observation
of both susceptibility and AMS of specimens also showedthat
sideriteat room temperatureis relatively stable,which is in
contrastto the observationof Ellwood et al. [ 1986]. Remanences
slowly increasedwith prolongedtime due to acquisitionof
thermalviscousremanence(VRM) component.
Another group of siderite-bearingcubic specimenswere
incrementally heatedup to 600øCat intervalsof 100øCwith an
appliedsteadyfield of 100 •tT (referredto as the field-rising-
temperature, FRT experiment).The field was turnedoff in both
theheatingandthe coolingprocesses to preventfromacquisition
of partial thermal remanence.As shown in Figure 12b,
 PAN ET AL.' ROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE 789

3.1. Direct Mineral Analyses

1.10 Both transmittedand reflectedlight microscopyobservations
revealedthat magnetite,maghemite,and hematitewere createdin
1.08 the oxidationproducts.The thermalgravity analysis(TGA) (by
heating at 10øC/min, similar to that in •:(T) measurements)
demonstratesa 36% weight loss between 400ø and 600øC,
1.06 • +
+
indicatingthe decompositionof siderite and the loss of carbon
oxide. A notable endothermic valley around 400øC and a
1.04 prominent exothermic peak around 584øC on the differential
thermalanalysis(DTA) curve suggests a decompositionreaction
0 0 ß ß + ß ß
[] ß ++ and an oxidationreaction,respectively.
1.02 + + ß •
XRD analyses indicate that unheated siderite is well
crystallized,the main peak (d=2.794) at 20=31.99 degree. A
1.00 spinelmagnetitephasewas identifiedin productsafter the 490øC
run and found to be dominantin productsafter the 510øC run.
, I i I I , I I I , I , I , I Spinel maghemitecoexistingwith rhombohedralhematite was
0.98
100 200 300 400 500 600 700 800 identified after 580øC run. Hematite fraction was calculated to be

Temperature about30% after 640øCrun and 80% after 690øCrun, respectively

(Figure13).
Becausemagnetite and maghemite have not only the same
q
spinel structurebut also similar magneticproperties,they are
2.00 - always difficult to distinguishusing traditional rock magnetic
ß
methodsand eventhe XRD method[Solheid,1998]. Thanksto the
ß ß []
differencein hyperfinefields betweenmagnetiteand maghemite,
1.60 - ß ß and an inner absorptionpeak in the spectrumof magnetite,
Mbssbauereffect spectroscopyis very useful in distinguishing
¸ []
¸ thesetwo magneticphases.In addition,it can be usedto detecta
1.20 - weakly magneticiron mineral such as hematite,which is often
¸
maskedmagneticallyby evena low concentration (few percent)of
ß

magnetite[Solheid,1998]. In this study,oxidationproductsused

0.80 Prolate
in rock magneticexperimentswere analysedthroughM6ssbauer
q=0.69 spectroscopy. Detailed resultswill be reportedlater in a separate
Oblate ß ¸ []
¸
o• paper.An admixtureof the quadruplesplittingdoubletof siderite
0.40 - with the magnetically split componentsof magnetite can be
ß ¸o ¸
detectedin samplesafter the 410øC run. It can be estimatedfrom
,•.• ß .
ß the area of subspectrathat 4%, 39% and 62% of magnetiteare
0.00 , I , I , I , ? , [ , I , I , I formed after the 410øC, 490øC, and 510øC runs, respectively.
0 100 200 300 400 500 600 700 800 After a treatmentat 530øC the spectraconsistof two sextetswith
Temperature
Figure 7. Variations of anisotropy degree (P) and shape
parameter(q) of siderite-bearing
specimens
afterheating.
1.0--

0.8-

magnitudesof both susceptibilities

and remanencesincreasein the
runs over 250øC and reach maximum values around 490øC, an E
increasethat was hundredstimes higher than that of unheated
specimens,followed by a distinctdecreaseat higherthan 490øC
0.6-
runs.It is revealedthat all prior declinationsand inclinationsof 0.4
remanenceswere changedto the directionof externalappliedfield
without exceptionafter thermal treatmentsin 350øC to 600øC
runs,regardlessof theirpreviousdirectionsof remanences. 0.2

3. Interpretation and Discussion 0.0 ' I ' I ' I

0 200 400 600 8OO

To further verify the mineral transformationproducts of
siderite oxidation as revealed by the indirect rock magnetic Temperature (øC)
methodsand to provide a betterunderstanding of the association Figure 8. Representative thermal dependence of the
betweenmagneticpropertiesand mineral alteration,we carried magnetizationinducedin the powder siderite specimen.The
out combined conventionaldirect mineral analyses on the intensityof appliedfield was 0.48 T. A heating/cooling rate of
productsusedin rock magneticanalyses. 10øC was used.
790 PAN ET AL ßROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE

10000

lOOO

(• RT
• 300øC
lOO [-] 400oC
• 490øC
• 550øC
ß 580oC

,,• 680oC

.Ol

0 200 400 600 800 1000

Applied Field (mT)

Figure9. Progressive
acquisition
of IRM fora representative
specimen
afterheating
totheindicated
temperatures.
RT standsfor the room temperature.

hyperfinefieldsof 49 T and45 T corresponding to iron atomsat the decomposition

of sideritewas almostcompleteandwQstite
A site and B site of Fe304 [Singhviet al., 1986]. A sextetof andmagnetitepredominated. BaginandRybak[1970]foundthat
maghemitewith a hyperfine field of 50 T can be observedafter heatingsideritein air above 300øC might result in the formation
heating at 550øC. Spectra after the 580øC run consistof two of magnetiteand maghemite.Decompositionof sideriteproceeds
sextetswith hyperfine fields causedby maghemiteand of simultaneouslywith dissociationinto maghemiteand magnetite,
hematite.After that,the magnetitespectrum
disappeared
andthe and hematite as the end product after complete oxidation.
amountof maghemitedecreased,and the quantityof hematite Nevertheless,
thepresence of "unstable" spinelphases suchas
increased,reachingapproximately34% and 77% approximately magnetite/maghemite
or otherintermediatecompositions
between
after the samples had been treated at 640øC and 690øC, maghemiteand hematite has not been detectedby some others
respectively.Althoughthepreciseamountsmay be affectedby the [e.g.,Hus,1990].Ozdernir
andBanerjee[1984]studied
thehigh-
presenceof impuritiessuchas Mg or Mn, it is nevertheless
clear temperaturestability of acicular maghemitebetween20øC and
that magnetite,maghemiteand hematite are producedduring 600øC. They found synthetic monodomainmaghemiteto be
siderite oxidation in air atmosphere,an observationthat is stablewith respectto hematiteat temperatureas high as 500øC
completely consistentwith the conclusionsof XRD and other and that the true Curie point of pure maghemitewas close to
methods. 645øC.
Clearly, the resultsof microscopy,XRD, and M6ssbauereffect It is shown in this study that both of the spinel structure
spectroscopyagree well with the previously describedmineral magneticphasesare intermediateproductsand do have relative
magneticparameters.This showsthat magnetiteand maghemite stability in some temperatureranges. Magnetite may form by
are formed when siderite is oxidized in air. decompositionfrom sideritedirectly, or be producedfrom the
oxidation reaction between wustite and carbon oxide gas.
3.2. General Discussion However, wustite was not identified in our experiments.
The decomposition of siderite in air is a complex Magnetite was transformedto maghemiteand hematitegenerally
physicochemical processbecauseit involvesthe decomposition of after 540øC runs in stepwisethermaltreatments.Maghemitewas
theCO32'complexandrearrangement of thecrystalstructure.An not completely transformedto hematite in stepwisethermal
excellentwork on the thermaldecomposition of sideritein special treatmenteven after 690øC;the productwas a two-phasemixture
atmospheres was carriedout by Gallagherand Warne [1981] and of maghemiteand hematite. Hematite was the end product at
Gallagher et al. [1981] using thermogravimetry,evolved gas highertemperatures. The reactionsin the sideriteoxidationmight
analysisand M6ssbauereffect methods.They foundthat siderite be expressedas follows:
oxidationin flowing oxygenis so rapid that only hematitecan be 3FeCO3-->Fe304+ 2CO2+ CO
detectedas the by-product.In vacuum,muchof the decomposed 4Fe304+02 -->3¾Fe203 + 30tFe203
wustite (FeO) from siderite is retained, but when heating at Decomposition of siderite depends critically on heating
atmosphericpressurein a flowing inert gas, magnetite is the temperature,time, crystallinity,porosity,and the availability of
predominantproduct.After thermal decomposition in a vacuum, 02. The temperaturevariationof magneticpropertiesdiscussed in
metallic iron andmagnetitewere formedwhen sideritewas heated section two can be explained well through the mineral
to 385øC and 410øC. At higher temperatures, 450øC and 600øC, transformationprocesses.
 PAN ET AL.: ROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE 791

after 530 øC after 580'C

0.75 SiRM=0.396Am
2 0 ---[SiRM=0.166Am
2 •
Hs:
0.1T '1 Hs:
0.11T •J.
0.25 O,
0 .0 0 ......... 0i • •

-0,
-0.25-- a
- ...f.

-1000 -750 -500 -250 0 250 500 750 1000 -1000 -750 -500 -250 0 250 500 750 1000

H(mT) H(mT)

.... - - -Z- -7.-

n 7c
.... /.JI after640'C=•' /
SIRM=0-0408Am2
Hsl: 0.11T ---=/' I -] Hs:>2.7T ,,/ I ,./

0'50-1
Hs2:>2'7T
1 Hcr1=O.O33T

0'251
Hcr2=0'49T/t I•-0'25t /
ø'øøT-
"I c ' I d
-1000 -750 -500 -250 0 250 500 750 1000 -1000 -750 -500 -250 0 250 500 750 1000

H(mT) H(mT)

' after
700øC
0.75--SlRM=0.03Am
2• •' [-00
- Hs:>2.7T

I o.
:::i -' 000 -750
I
-500 -250 0 250 500 750 1000
o, - ........
-1000 -750 -500 -250 0 250 500 750 1000

H (mT) H (mT)

Figure10. Progressive
acquisition
of IRM anda reverse
fieldremovalof SIRM for a specimen
afterheating
to
different
hightemperatures
asindicated.
Hsstandsforthefieldstrength
atwhich90%SIRMwasacquired; Heris
theremanence
coercivity.

3.3. Interpretationfor AMS Exchange

because magnetite and maghemite have higher magnetic
It is well knownthatthe iron-bearing carbonates
(siderite),susceptibilityand lower anisotropyand hematite has lower
tourmaline,cordierite,
goethite,andsingle-domain
magnetite
have susceptibility but higheranisotropy.The grainsize of the initial
inversemagneticfabrics,while hematite,pyrrhotiteand siderite affected the oxidation rate and thus the rate of AMS
multidomain magnetite(orrelatedcubicironoxides)
havenormal exchange.
magnetic fabrics[Rochette
et al., 1992].Thecompaction
effectin Ellwood et al.'s [1986, 1989] samplesexperienceda near
thelaboratory
duringthepreparation
of specimens leadsthebasal completeexchangebetweenmaximum and minimum principal
planesof mostrhombohedralsideritegrainsto be in accordwith axes when heating/oxidationcaused a change of siderite to
the bedding planes.Therefore mostKma x axesare parallelto maghemite/magnetite. The work of Hirt and Gehring [199l]
crystalline
c-axes(andperpendicular to thecompaction planes) showed that the low- temperaturemagnetic fabric remained
andcontribute to the initialinverse
fabricsof siderite-bearing
inverseuntil 480øC.Thereforethey attributedthe AMS exchange
cubicspecimens.Magnetitewascreatedon thesurfaceandin the observedto berthierinedecomposition.
Accordingto our results,
cracksof sideritegrainsabove 350øC as we observedin thin however, the contribution to AMS exchange from siderite
sections.
Magnetitesusceptibilities
graduallysubmerged,
and oxidationin their Northamptonironstonecannot be excluded,
substituted
for, the susceptibilities
of unoxidizedsiderite.It is the althoughmostlysideriteis stillpresentandcontrolsthe anisotropy
distribution
anisotropy
contributed
by theprevailingdistributionat low-temperature.In fact, when 0.5% (weight) of magnetite
of magnetite
in beddingplanesthatchangedthe initial inverse and/ormaghemiteoccurredin sideritespecimens,the contribution
fabrics
to normalfabrics
afterthe350ø-490øC runs.Althoughthe of sideritesusceptibility
at roomtemperature canbe overwhelmed
transformation
betweenmagnetite/maghemite tohematitekeptthe [Tarling and Hrouda, 1993]. This also explainswhy the AMS
magnetic fabrics
normal,it caused swingsin declination
of Kmax exchanges in our experiments occurredat lowertemperatures
than
axesin thebeddingplanes at thehigh-temperature
stage.Thisis the temperatures for peak susceptibilityoccurrence.
792 PAN ET AL.: ROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE

1 1 i,

-3Am2 x10-3Am 2
0.8 0.8-

0.6 0.6

0.4 0.4

0.2 0.2

0 I
0
' I-'
200
I
400
T--•'•=•l
600 800
o 0 200 400 600
b I
8oo

Temperature (øC) Temperature (øC)

1 1

7.9xl 0 -4Am2

0.8 0.8

0.6 0.6

0.4

0.2

o i ' i ' i ' i I

0 200 400 600 800 0 200 400 600 8oo

Temperature (øC) Temperature (øC)

Figure 11. Thermaldemagnetization of three-axes of differentcoercivityIRM components for a specimen
after
heatingto (a) 580øC,(b) 610øC,(c) 640øC,and(d) 720øC.Solidcircles,rhombuses andsquaresrepresentthe soft
component (<0.05 T), mediumcomponent (0.05-0.5 T) andhardcomponent (0.5-2.7 T), respectively.

3.4. Nature of Remagnetization andOzdemir,

1997andreferences
therein].
Although
noattempt
As previously described, magnetization acquired in FRT is madehereto separatethe effectsof CRM, spontaneous
IRM,
experimentswas parallel to the appliedfield and its intensitywas and thermal VRM, it is believed that the mechanismof remanence
enhancedhundredsof times higher around the 490øC runs. We acquisitiondescribedhere is complex, becauseit involves a
can consider the secondarymagnetization to consist of three multiphase rhombohedral [siderite]- spinel [magnetite/
components:a thermal VRM, an initial IRM and chemical maghemite]-rhombohedral[hematite] intergrowth.The stresses
remanentmagnetization(CRM). Remagnetizationoccurreddue to resultingfrom differentcrystallinestructuretransitions
might
somecrystalgrowth,alterationandphasetransitionduringsiderite causetheunusualincreasein CVRM over600øC(Figure12b)and
oxidation.It is the case that CRM (including both the growth the unusuallyhigh coercivity,980 mT, of the remanence
of the
CRM and the two-phaseCRM) is continuouslyaugmentedby oxidizedproducts,
asshownin Figure1Of.
VRM duringheating,so the remagnetizationcan be referredto as Theproblem
of exchange
coupling
across
themaghemite
to
chemical-viscousremanent magnetization(CVRM) as defined hematite
phaseboundaryremains controversial.
Oneinteresting
earlierby OzdemirandDunlop[1989].The peakintensity of studycouldbe thetestof a self-reversal
occursduringthe
CVRM around490øC is evidently attributedto the formationof a transformation
frommaghemite to hematite.
Negative
super-
large amountof magnetitein specimens.Reductionin intensity exchange
coupling of themaghemiteandhematite
regionsat the
above 490øC is caused oy magnetic transformation from inversion
temperature seems
toexistwhenmaghemite,produced
magnetite to maghemite and hematite, consistent with the by dehydrating
lepidocrocite,
invertstowards
hematite
[Hedley,
variationsin susceptibilities. 1968;McClelland,
1987;McClellandand Goss,1993]or during
In nature, many types of oxidation and alteration processes room-temperature
oxidationof siderite[Ellwoodet al., 1986].On
change the crystal structure of an initial magnetic phase. thecontrary,
Ozdemir
andDunlop[1988]heated
single-domain
Knowledge of the configurationof the crystallographicphase maghemite from300øCto 604øC,keptthesamples for 3 hoursin
boundaryor boundariesduring alterationis vital to understand a 50 pT field,andstill observed
remanent
directions
parallelto
phasecoupling,but this knowledgeis usuallylacking.No doubt, the appliedfield. Althougha field similarto that usedby
the oxidation processof siderite providesus with an unusual McClellandandGoss[1993]wasapplied in ourexperiments,
no
opportunity to further investigate the crystallizationremanent selfreversalphenomenonwasobserved.
Magnetization directions
magnetizationbetweendifferentstructureandphases[seeDunlop acquiredin theFRT experiments
wereparallelto theappliedfield,
 PAN ET AL.' ROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE 793

k/kmax J/Jmax SUS/SUSmax J/J max

I I I I I I I I I I I
1.0 1.0 1.0 1.0

0.8
ß 0.8 0.8 0.8

0.6 0.6 0.6 - 0.6

_

0.4 0.4 -0.4

0.2 0.2 0.2

_

a
0.0 -0.0 0.0 b-o.o
• • • • •ß I I . I I
5 6 7 8 9 10 11 12 0 100 200 300 400 500 600 700

Time (hour) Temperature (øC)

Figure12. Representative
curves
of remagnetization
in siderite
oxidation.
Susceptibilities
(withoutconnecting
line)andremanent
magnetization
(withline)of specimensafterheating
weremeasuredat theroomtemperature.
(a)FCTexperiments
heating
at250øCina fieldof50pT;(b)FRTexperiments heating
ina fieldof 100pT.

consistentwith OzdemirandDunlopg [1988]results.Therefore, 2. In the absenceof strong ferrimagneticminerals, the

contraryto McCIeIIand's[1987]conclusion,
we concludethatthe crystallineanisotropyof paramagnetic
sideriteleadsto inverse
self-reversalis not necessarilya common phenomenonin the magneticfabrics,thatis, the maximumprincipalaxisKma x normal
transformation of maghemiteto hematite. to the beddingplanesin siderite-bearing specimens.However,
normalmagneticfabricsusuallycreatedduringthermaltreatments
4. Conclusions
can be attributed to mineralogical transformations from
1. Temperature-dependent variationsof magneticsuscepti- paramagnetic siderite to ferromagnetic minerals such as
bilities are very useful in identifyingthe presenceof the magnetite,maghemite,andhematite.
paramagnetic mineral siderite,as well as being capableof 3. Mineral magneticparametersare reliable and sensitivefor
detecting associatedthermalalteration
products. of identifyingthe magneticphasescausedby sideriteoxidation.Both
Susceptibility
sideritevariesaccordingto theCurie-Weisslaw below250øC. magnetiteand maghemiteare identified in the products.The

mh

H •mH H H (e)
mh mh

• Sd
'• U Sd U (C)

M• Sd )

20.00
S• Sd••Sd
I
•dj• Ssd•d
Sd(a) ' I
40.00
' I
60.00
' I
80.00

2 Theta [degree]

Figure13. X-raydiffraction
of a specimen
heatedafterdifferent
temperatures'
(a) unheated,
(b) 490øC,(c) 510øC,
(d) 580øC,and(e) 690øC.Sd,M, mhandH referto siderite,
magnetite,
maghemite andhematite,
respectively.
794 PAN ET AL.: ROCK MAGNETIC BEHAVIOR DURING HEATING SIDERITE

maghemitephasewas relatively stableand did not completely Hrouda, F., A techniquefor the measurementof thermal changesof
invertto hematiteat temperatures as high as 690øC.Hematite,the magnetic susceptibilityof weakly magnetic rocks by the CS-2
terminalphase,is abundantin the productswith somemaghemite apparatusand KLY-2 Kappabridge,Geophys.J. Int., 118, 604-612,
1994.
mixture. Wustite is probablyoxidized so quickly that it was Hrouda,F., and V. Jelinek,Resolutionof ferrimagneticandparamagnetic
unidentifiedin our experiments.Rock magneticpropertiesof the anisotropiesin rocks, using combined low-field and high-field
siderite oxidation productsdemonstratenicely the constituent measurements, Geophys.J. Int., 103, 75-84, 1990.
mineraltransformationprocesses. Hus, J.J.,The magneticpropertiesof sideriteconcretionsandthe CRM of
4. No self-reversal behavior is observed during the theiroxidationproducts,Phys.Earth Planet.Inter., 63, 41-57, 1990.
Jacobs,L.S., Metamagnetism of siderite(FeCO3),d. Appl. Phys.,34, 1106-
transformationfrom maghemiteto hematite in the thermal- 1107, 1963.
treatmentof crystallinesiderite. Jover, O., P. Rochette, J.-P. Lorand, M. Maeder, and J.-L. Bouchez,
5. Evidently,thermalalterationof sideritein an externalfield Magnetic mineralogy of some granites from the French massif
can producea very strongCVRM with a directionparallelto the Central,Phys.Earth Planet. Inter., 55, 79-92, 1989.
Li, X.L., and H.H. Yin, Compositionsof Sideritedepositsin China, in:
appliedfield. The acquisitionmechanismof the CVRM during Symposiumof SideriteDeposits(in Chinese),SciencePress,Beijing,
sideriteoxidationis believedto be very complex.If one hopesto pp.81-97, 1983.
enhanceSheprimaryAMS or separatethe characteristic remanent Lowrie, W., Identificationof ferromagneticminerals in a rock by
magnetizationthroughthermal treatmentsof lake and marine coerc•vityandunblockingtemperature properties,Geophys.
Res.Lett.,
17, 159-162, 199C.
sediments(in which authigenic siderite is common as either
McClelland, E., Self-;eversalof chemical remanent magnetization:A
detritusgrainsor matrix),greatcautionshouldbe taken. paleomagneticexample. Geophys.J. R. Astron. Soc., 90, 615-625,
1987.
Acknowledgements. We would like to thank Steve Lund, Brooks McClelland, E. and C. Goss, Self reversal of chemical remanent
Ellwood, and Bernie Housen for their commentswhich improvedthis magnetizationon the transformationof maghemiteto haematite,
manuscript.Thisworkis financiallysupportedin Chinaby theMinistryof Geophys.J. Int., 112,517-532, 1993.
Scienceand Technology(MOST) and National DistinguishedYouth Nagy, D.L., Erlangen,Dezsi I., Budapest,U. Gonser,and Saarbrucken,
Programof NSFC (49425405),and in the United Statesby the Earth M6ssbauer studies of FeCO3 (siderite), News Jahrb. Mineral.
SciencesDivisionof the NationalScienceFoundation(NSF). The IRM is Monatsh., 3, 101-114, 1975.
fundedby theInstruments andFacilitiesProgram,EarthSciences
Division, Ozdemir,
O. andS.K.Banerjee, Hightemperature stability
of maghemite
u.S. NSF, W. M. KeckFoundation, andtheUniversityof Minnesota,Twin (¾Fe203),Geophys.Res.Lett., 11, 161- 164, 1984.
Cities. This is IRM contribution 9905. Ozdemir,O., andD. J. Dunlop,Crystallization
remanent
magnetization
duringthe transformation
of maghemiteto hematite.J GeophysRes,
93, 6530-6544, 1988.
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