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High-Pressure Structural Study of Dolomite and Ankerite

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High-Pressure Structural Study of Dolomite and Ankerite American Mineralogist, Volume 77, pages412-421, 1992 High-pressure structural study of dolomite and ankerite NlNcv L. Ross Deparrment of Geological Sciences,University CollegeLondon, Gower Street,London WCIE 68T, U.K. Rrcn.q.noJ. Rrnnnn Mineral PhysicsInstitute and Department of Earth and SpaceSciences, State University of New York, StonyBrook, New York 11794,U.S.A. Ansrucr Structural parametershave been refined using X-ray intensity data for a stoichiometric dolomite singlecrystal at room pressureand at 1.50,2.90,3.70, and 4.69 GPa; and for a single crystal of a ferroan dolomite with approximately 70 molo/oCaFe(COr)' at room pressureand at 1.90,2.97, and 4.0 GPa. The principal structuralchange with increasing pressureis compression of the CaOu and (Mg,Fe)Ouoctahedra. The CO, group remains essentiallyinvariant throughout the pressurerange studied. The effect of the polyhedral compression is reflected in the anisotropic compression of the unit-cell parameters. In both dolomite and ankerite, c is approximately three times as compressibleas a. In addition to displaying similar axial compressibilities,dolomite and ankerite display similar bond compressibilitiesand bulk moduli. The isothermal bulk modulus of dolomite determined from cell volume compressiondata, assumingthe pressurederivative is 4, is 94 GPa,and that of ankerite is 9l GPa. The polyhedralbulk moduli of CaO. and (Mg,Fe)Ou are also similar, with CaOu being slightly more compressiblethan (Mg,Fe)Ou'The latter has a greater compressibility than generally observed in other oxides and silicates. The distortion of the octahedra, though already small, decreasesslightly with pressure.No phasechange was observedin either compound throughout the pressurerange studied. INtnonucrroN Rotational disordering of the CO, group in calcite has (Dove Powell, Relatively little is known about the structural behavior also been studied at high temperatures and only of carbonate minerals at conditions of high pressureand 1989; Redfern et al., 1989). Of these carbonates, high pressures. temperature. Most petrologic interest in calcium magne- calcite has been studied in any detail at phase at room sium iron carbonates has been in the properties of the Calcite undergoesa displacive transition monoclinic phases at near-surfaceconditions. However, metamor- temperatureand approximately1.5 GPa to a poly- phic and igneouscarbonates have also generatedconsid- phase,CaCO.-II, which itself transforms to another (Merrill and erable interest, and in some casesthe carbonateshave morph, CaCOr-I[, at approximately 2.2 GPa polymorphs ap- provided important constraints on petrogenesis.There Bassett,1975). Both high-pressure are within stability field of has been considerabledebate concerning the possiblerole parently metastableand exist the of carbonatesin the upper mantle (e.g.,Irving and Wyllie, aragonrte. refine- 1973). Experimental phase equilibria studies demon- In this study we report the results of structure X-ray intensity strate that dolomite is stable over a wide range of pres- ments for dolomite and ankerite using pressure cell. suresand temperatures.Irving and Wyllie (1975) show data obtained at high in a diamond-anvil for phasetransition was the stability field of dolomite solid solution extending to Unlike calcite, no evidence any in dolomite or to 4.00 GPa in approximately 1300"C at 3.0 GPa, near the upper limit observedto 4.69 GPa contrasting of pressurein their piston-cylinder experiments.The oc- ankerite. Possible factors leading to these pressure with currenceof dolomite and ferroan dolomite as major con- structural responsesto are discussed,along high-tem- stituents in many carbonatites and the speculatedexis- a comparison between the higft-pressureand tenceofthese phasesin mantle carbonatedperidotite raise perature behavior of dolomite. questions chemical behavior of concerning the crystal ExpnnrprrNTAr- METHoD carbonateminerals at lower crust and upper mantle con- ditions. Specimendescription High-temperature crystal structures have been refined The dolomite crystal usedin this study was taken from for three rhombohedral carbonates:calcite (up to 800 "C), a clear cleavagerhomb of Eugui dolomite. Eugui dolo- magnesite (up to 500 "C), and dolomite (up to 600 "C) mite was selectedfor this study becauseof its high-quality (Markgraf and Reeder,1985; Reeder and Markgral 1986). single crystals and becauseit was used in earlier studies, 0003-004x/92l0304-04I 2s02.00 412 ROSS AND REEDER: HIGH P DOLOMITE AND ANKERITE STRUCTURES 413 including the single-crystaldeformation work of Barber TABLE1, Data measurementand refinementinformation for do- et al. (1981),the refinementsof thermally disordereddo- lomite at several oressures lomite by Reeder and Wenk (1983), and Reeder and Pressure No. ind. obs. Markgrafs (1986) high-temperaturestudy. Eugui dolo- (GPa) (>2o) R R" GOF mite is fully ordered and the composition is nearly ideal, 0.00 108 0.027 0.014 1.91 Ca, oo,Mgo n'Feo o,oMnooo, (CO.), (Reederand Wenk, 1.50 108 0.035 0.029 3.69 1983).In addition, examinationin the transmissionelec- 2.90 108 0.032 0.026 3.33 2.39 tron microscope 3.70 108 0.032 0.020 has shown that Eugui dolomite is ho- 4.69 85 0.034 o.o22 2.68 mogeneouswith relatively low dislocation densities(Bar- Note:R : >lle | - | F"llDI F.I andF* : p tt{| F"| - | F.l)'D wl F"l"l''" ber et al., l98l; Reederand Wenk, 1983).The crystal GOF: Estimatedstandard deviation of unitweight observation usedin this study has approximatedimensions of 150 x 62 x Jg pm. The crystal was selectedafter examination with the polarizing microscope, which showed that the crystal was clear, free of inclusions, and appearedto be a following the procedureof King and Finger (1979). Initial single crystal. Further examination on the diffractometer unit-cell refinementswere made without constraints (i.e., verified that the crystal is untwinned and has sharp, well- as triclinic) to test for deviations from hexagonaldimen- defined diffraction peak profiles. sionality. At all pressuresc and D were within 2 esd of The ankerite crystal used in this study, AMNH 8059, each other, a and B were within 2 esd of 90o,and ,y was was taken from the same sample used by Reeder and within 2 esdof 120".Final cell parameterswere calculated Dollase (1989) in their study of the dolomite-ankerite with hexagonalconstraints (Ralph and Finger, 1982). solid solution series.The composition reported by those An automated Picker four-circle diffractometer oper- authors, on the basis of microprobe results, is ating with filtered MoKa radiation (I : 0.7107 A; was CaonnrMg rrrFeo uruMno,oro (CO r) r. X-ray refinements of the used for all diffraction-intensity measurements.Full sets site occupanciesof the crystal chosen in this study agree of intensitydata for dolomite were obtainedat 0.0, 1.50, with Reederand Dollase's(1989) site refinements:the A 2.90,3.70, and 4.69 GPa. Intensitydata for ankeritewere site is filled with Ca and the B site is filled with 730lo obtainedat 0.0, 1.90,2.97, and 4.00 GPa. All accessible Fe (+ Mn) and 27o/oMg. Several ankerite crystals were reflections, including crystallographically equivalent re- examined with the polarizing microscopeand on the dif- flections, to sin d/tr < 0.7 were obtained by the @-scan fractometer. Each crystal examined either contained in- techniquewith 0.025" stepsand counting times of 4.0 s clusions,was twinned, or both. We chosean inclusion- per step. Corrections were made for 1,, effects and ab- free crystal with approximate dimensions 75 x 50 x 50 sorption by the components of the diamond-anvil cell. pm. Examination of the crystal on the diffractometer Absorption corrections for the crystal were made with showedthat the crystalis twinned with twin law t I120). program Absorb (Burnham, 1966),yielding minimum and The parent to twin volume ratio determined from refine- maximum transmission factors of 90 and 930/ofor dolo- ments (seebelow) is 1.0:0.27. mite and 88 and 9lolofor ankerite. A reflection was con- sidered unobservedwhen 1 I 2 o,. Absorption-corrected High-pressure data measurements data were symmetry averagedprior to each refinement, The procedure for studying single crystalsat high pres- resulting in approximately I l0 (dolomite) or 90 (anker- sure is describedin detail by Hazen and Finger (1932). ite) independent observationsat each pressure. In brief, eachcrystal was mounted in a triangular Merrill- Bassett-typediamond-anvil cell with an INCONEL 750X Structure refinements gasket with a hole diameter of 350 pm. The crystal and Refinements were carried out with the least-squares a l5-pm chip of ruby pressurecalibrant were affixed to program RFINE6, a development version of RFINE4 one diamond face with a thin smear of the alcohol-in- (Fingerand Prince, 1975),which incorporatesan option soluble fraction of vaseline, and a 4: I mixture of non- for refining the fraction of a twin given the parent-twin dried methanol to ethanol was the hydrostatic pressure- law. The twin fraction of the ankerite crystal used in this transmitting medium. The pressure was calculated by study, determined from intensity data measuredin air [to measuring the shift of the R, fluorescenceline of ruby sin(d)/I : 0.7 and including three asymmetric unitsl, is relative to the room pressure reading before and after 27o/o.In the refinementswith data obtained at high pres- eachexperiment. The uncertainty is the pressurereadings sure, the twin fraction was therefore set equal to 27o/o. is +0.05 GPa. For dolomite and ankerite, a weight of l/(o2r)was assigned Unit-cell parametersof dolomite were obtained at 0.47, to eachreflection, where o. is basedon counting statistics. 1.50,2.34,2.90,3.70,4.20, and 4.69 GPaas well as ar The refinements were initiated with the atomic coordi- room pressurewith the crystal mounted in the diamond- natesof Reederand Markgraf (1986)for Eugui dolomite anvil cell. Similarly, unit-cell parametersof ankerite were and those of Reederand Dollase ( I 989) for ankerite sam- measuredat 0, 0.97, 1.90,2.56, 2.97, 3.40, and 4.00 ple AMNH 8059.
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