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Manganese Uptake During Calcite Precipitation from Seawater: Conditions Leading to the Formation of a Pseudokutnahorite

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Manganese Uptake During Calcite Precipitation from Seawater: Conditions Leading to the Formation of a Pseudokutnahorite Gewhimica et Cosmoehimic~ Acta Vol.52, pp. 1859-1868 0016-7037/88/$3.00 + .OO Copyright Q 1988 Pcrgamon Press plc.printed in U.S.A. Manganese uptake during calcite precipitation from seawater: Conditions leading to the formation of a pseudokutnahorite ALFONSOMUCCI Department of Geological Sciences, McGill University, 3450 University Street, Montreal, Quebec, Canada, H3A 2A7 (Received September 17, 1987; cicceptedin revisedform April 6, 1988) Abstract-Manganoan magnesian calcite overgrowths were precipitated from artificial seawater at 25°C on inure calcite seeds using a constant disequilibrium technique. The coinposition of the overgrowths, and more specifically their Mn, Mg, Na and Sr content, was determined as a function of the precipitation rate and Mn*+ concentration in the parent solution. X-ray di!Traction patterns indicate that the overgrowths produced were one-phase multicomponent solid solutions, and contained up to 40 mole% MnCO,. The amount of Mn coprecipitated with calcite decreased with increasing precipitation rate. Thus, overgrowths are not in exchange equilibrium with the solutions from which they precipitated. A kinetic model is proposed which adequately describes the composition of the overgrowths in terms of the relative precipitation rate of an 8- 10 mole% magnesian calcite and a “pseudokutnahorite” from seawater. The possible existence of a pseudokutnahorite in marine sediments and its implications are discussed. The concentration of Mg in the overgrowths decreased with increasing MnCOp content, but their Mg:Ca ratio remained nearly constant. Strontium and Na incorporation was strongly dependent on the number of available non- lattices sites. INTRODUCTION positions lying below the solvus observed at high temperature were obviously metastable, but found them to reinain un- IT HAS BEEN SUGGESTED(EMERSON et al., 1980; SAYLES, changed in contact with their supematant liquid for at least 1981, 1985; BOYLE, 1983; DE LANGE, 1986) that the for- six months. Furthermore, DE CAPITANI and PETERS (198 1) mation of an authigenic mixed Mn-Mg-Ca carbonate phase suggested that it was probably impossible to demix metastable may explain the observed supersaturation of deep-sea car- (Ca, Mn)C03 solid solutions under laboratory conditions bonate-rich sediment pore waters with respect to calcite in because the process was too slow either due to high activation the reduced manganese zone. If this is true, it may have a energies or low diffusion rates. As is often observed, theoretical significant influence on the accumulation of calcite and the modeling of solid solutions fails short of predicting their actual diagenesis of carbonate-rich deep-sea sediments. behavior in natural systems because of kinetic restrictions. In marine sediments, MnC03 has been found to occur in Estimates of the distribution coefficient of Mn( II) in calcite solid solution with calcite up to 50 mole percent (LYNN and have been derived from field and laboratory measurements. BONATTI, 1965; CALVERTand PRICE,1970; PEDERSENand Observed and selected values range between approximately PRICE,1982). BOYLE (1983) has observed that the Mn/Ca 2.5 and 20 (BODINE et al., 1965; MICHARD, 1968; ICHIKUNI, ratio of foraminifera tests increases significantly below the 1973; KUMAGAI, 1978; PINGITORE, 1978; TEN HAVE and manganese redox boundary. He argued that the increases are HELJNEN,1985 ) , but these studies give little indication of the due to the formation of manganese carbonate overgrowths compositional range over which the solid solution can form. and that manganese carbonate coatings may be a significant Furthermore, L~RENS (198 1) and PINC~ITOREet al. (1988) sink of manganese in deep-sea sediments. Likewise, MICHARD found that the distribution coefficient of Mn(II) in calcite (197 1) and THOMSONer al. (1986) noted the importance of varies with the precipitation rate. They observed that the dis- Mn( II) adsorption on calcium carbonate surfaces to the dif- tribution coefficient decreases with increasing precipitation fusive flux of Mn( II) from anoxic sediments and it has been rate. The value determined by L~RENS (198 1) at the slowest suggested that the process may be responsible for the scarcity precipitation rate (i.e. close to calcite saturation) is approx- of manganese nodules in calcareous sediments (PIPER and imately 50. Unfortunately, most of these studies were con- WILLIAMSON,1977; BOYLE, 1983 ) . The formation of mixed ducted in solutions whose compositions differ significantly Mn-Ca carbonates has also been inferred or demonstrated from seawater and may not be applicable directly to a seawater (MANHEIM, 1961; SUES& 1979; ELDERFIELDet al., 1981; system. In fact, FRANKLINand MORSE (1983) obbrved that FRANKLINand MORSE, 1983) to explain the apparent non- the adsorption behavior of Mn( II) on calcite in dilute solu- equilibrium behavior of rhodochrosite in marine sediments. tions and in seawater is clearly different. They demonstrated Recently, in a theoretical study of the system CaC03- that this distinction was most likely due to the presence of MnCOs-H20, MIDDELBURGet al. (1987) indicated that the magnesium ions in seawater. carbonates should form solid solutions over a very limited In view of the discrepancies which exist in the literature compositional range. However, GOLDSMITH and GRAF and the questionable applicability of previous laboratory (1957) and FUBINI and STONE(1983) were successful in pre- studies to a seawater system, the factors governing Mn (II) cipitating a complete series of well-crystallized solid solutions incorporation in calcite must be clarified before we can draw between calcite and rhodochrosite at room temperature. any conclusions concerning the influence of Mn( II) on the GOLDSMITHand GRAF ( 1957 ) noted that at least those com- solubility behavior of calcite in seawater. In this paper I pre- 1859 1860 A, Mucci sent and discuss the results of a laboratory study on the in- determined by MUCCI (1983) in S = 35 seawater at 25°C (4.39 corporation of Mn( II) in magnesian calcite overgrowths pre- X IO-’ mole* kg-’ SW) was used to calculate the saturation state of cipitated from seawater at 25°C. the solution with respect to calcite, aa defined by: MATERIALS AND METHODS where K,* is the equilibrium stoichiometric solubility of calcite in All the calcite overgrowth precipitations were carried out using seawater. Baker “Instra-analyzed flux reagent” grade calcium carbonate as a Saturation calculations using pH measurements done on both scales seed material. This material was washed in deionized distilled water and the appropriate constants agreed in most cases to within a few and size separated (3-7 pm) by settling. The CaCQ was freeze percent or better. Results presented in this paper were calculated dried, X-rayed (>99% calcite) and its surface area (0.52 m2 g-i) was from pH measurements based on the NBS scale, as they may be determined by the Kr-BET method of DE KANELand MORSE(1979). more consistent when used with the stoichiometric solubility constant Aged artificial seawater was used for all the experiments. The ar- of calcite determined by MIJCCI(1983). tificial seawater of salinity 35 was prepared to include all major ele- The SrZf and Mn2+ concentrations ofthe solutions were measured ments of natural seawater including F- according to the method of before and after the reaction by flame atomic absorption spectro- KESTER ef al. (i967), mod&d to fit the analysis Of MILLER0(1974). photometry (AAS) using aqueous standards in a seawater matrix for Mn(II) was added to the artificial seawater solution prior to each ~libmtion. Precision of the AAS analysis is estimated to be better experiment in the form of a concentrated (2000 ppm) Mn(II) so than 3% for Mn2+ and 5% for Sr”. lution. This concentrated solution was prepared by dissolution of MnClz .4HrO in artificial seawater. Four sets of experiments were conducted, corresponding to the following initial Mn( II) concentra- Overgrowthcomposition tions in the precipitating solution; 1,5, 10 and 25 ppm. The manganese, magnesium, strontium and sodium content of Precipitation reactions were carried out in an open system in so- most of the overgrowths was determined following the acid digestion lutions of close to constant composition over a wide range of precip of a known amount of reacted solid by AAS. The mole fraction of nation rates iO-*.5to 104,5 mole m-* hr- i. Constancy of composition MnCOs, MgCOp and SrCOs and the Na content of the overgrowth was maintamed during the length of the precipitation by the use of were calculated from the results of the AAS analyses, the amount of a chemo-stat technique through the simultaneous injection of two carbonate precipitated and the amount of material dissolved for titrants in equal amounts by a dual syringe pump. The mixture of analysis (MUCCI and MORSE,1983). No correction was introduced the two &rants reproduced the exact composition of the precipitating to compensate for the presence of residual solution salts as the over- solution plus an excess in calcium, manganese(II), strontium and growths were rinsed with distilled water equilibrated with calcite after carbonate alkalinity to compensate for the manganoan magnesian being filtered out of the parent solution (Mucc~, 1986). calcite p~ipi~tion. The temperature of the p~ipi~ting solution Some of the reacted solids were also examined by X-my apron was held constant at 25 (kO.05 )“C by circulating water through a spectrometry to determine their mineralogy and identify other car- jacketed 400 ml glass reaction vessel from a constant temperature bonate mineral phases which might have precipitated along with the bath. The PcoZ of the solution was kept nearly constant at -3000 manganoan magnesian calcite. Powder packs were prepared and ir- ppm or lO-2.5 atm. by bubbling a C02/Nz gas mixture of known radiated using a Siemens model D-500 X-ray dilBactometer. The composition. A detailed description of the chemo-stat, its working Cu-I& wavelength radiation was used as a source and the diffraction concept and titrant compositions have been presented previously spectra were recorded using a proportional counter detector.
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