24. Horstad, I., Larter, S. R. & Mills, N. in The Geochemistry of Reservoirs (eds Cubitt, J. M. & England, W. A.) 159–183 (Geological Society Special Publication No. 86, London, 1995). Acknowledgements We thank Saga Petroleum ASA, Norsk Hydro, PEMEX and the Mexican Petroleum Institute for support and permission to publish. Correspondence and requests for materials should be addressed to R. d. P. (e-mail: rolando.di-primio@hydro.com). letters to nature 176 NATURE | VOL 406 | 13 JULY 2000 | www.nature.com ................................................................. Anomalous 17 O compositions in massive sulphate deposits on the Earth Huiming Bao*, Mark H. Thiemens*, James Farquhar*, Douglas A. Campbell*, Charles Chi-Woo Lee*, Klaus Heine & David B. Loope * Department of Chemistry and Biochemistry, University of California San Diego, Mail Code 0356, La Jolla, California 92093, USA Institute of Geography, University of Regensburg, 93053 Regensburg, Germany Department of Geosciences, University of Nebraska Lincoln, Lincoln, Nebraska 68588-0340, USA .................................. ......................... ......................... ......................... ......................... ........ The variation of 18 O that results from nearly all physical, biological and chemical processes on the Earth is approximately twice as large as the variation of 17 O. This so-called ‘mass- dependent’ fractionation is well documented in terrestrial minerals 1,2 . Evidence for ‘mass-independent’ fractionation (D 17 O= 17 O - 0.52 18 O), where deviation from this tight rela- tionship occurs, has so far been found only in meteoritic material and a few terrestrial atmospheric substances 3 . In the rock record it is thought that oxygen isotopes have followed a mass-dependent relationship for at least the past 3.7 billion years (ref. 4), and no exception to this has been encountered for terrestrial solids 5 . Here, however, we report oxygen-isotope values of two massive sulphate mineral deposits, which formed in surface environments on the Earth but show large isotopic anomalies (D 17 O up to 4.6‰). These massive sulphate deposits are gypcretes from the central Namib Desert and the sulphate- bearing Miocene volcanic ash-beds in North America. The source of this isotope anomaly might be related to sulphur oxidation reactions in the atmosphere and therefore enable tracing of such oxidation. These findings also support the possibility of a chemical origin of variable isotope anomalies on other planets, such as Mars 6 . We have analysed sulphates from laboratory experiments and natural sources (Fig. 1). The 18 O and 17 O of seawater sulphate, evaporites, sulphate from microbial sulphate reduction experi- ments, and sulphates formed from mineral-sulphide oxidation in air or soils, all fall on the mass-dependent terrestrial fractionation line, given by the relationship 17 O = 0.52 18 O. The deviation from this relationship, defined as D 17 O= 17 O - 0.52 18 O, is approxi- mately zero ( -0.04 0.05‰, n = 36). The central Namib Desert gypcretes and the Miocene volcanic ash-falls in the western United States, however, possess sulphate 18 O and 17 O values that deviate from the terrestrial fractionation line. The sulphate D 17 O of Namib gypcretes ranges from 0.20‰ to 0.51‰ (Table 1), well outside the experimental error of 0.05‰. Gypsum and other water-soluble sulphate minerals from Miocene volcanic ash deposits in Nebraska and South Dakota have strikingly large D 17 O values, up to 4.59‰, in contrast to the zero or slightly positive D 17 O found in adjacent soil and fluvial horizons (Table 2). Sulphate minerals with D 17 O 0‰ are expected because thermodynamic and kinetic (including biological) processes such as evaporation, mineral-sulphide oxidation (by Fe 3+ or air O 2 ), and sulphate reduction generate mass-dependent compositions (Fig. 1). Therefore, sulphate minerals with positive D 17 O values, such as those found in the central Namib Desert gypcretes and the Miocene volcanic ash-falls in the western United States require a different process. The only documented terrestrial reservoirs with positive D 17 O are from the atmosphere. Oxidants such as O 3 and H 2 O 2 are known to have positive D 17 O values that range from 1 to more than 25‰ (refs 7–10). Others, like OH and NO x , remain to be measured. Tropospheric O 3 and H 2 O 2 in rainwater may transfer their positive D 17 O values to the product sulphate by in situ oxidation of surface minerals (for example, sulphides). Our measurement of the sulphate produced by marcasite (FeS 2 ) oxidation in the air yielded D 17 O 0‰, indicating that the in situ pathway is not the major source of positive D 17 O. A more likely source is the wet and dry atmospheric deposition of sulphate produced by atmospheric oxidation of reduced gaseous sulphur compounds. The anomaly can come from atmospheric oxidants such as O 3 ,H 2 O 2 or OH radicals as a result of aqueous or gas-phase S(IV) oxidation. A similar explanation was invoked to interpret positive D 17 O values (0.20‰ to 1.80‰) observed in aerosol and rainwater sulphate 11,12 . Although the mechanisms of these atmospheric processes are still subjects of intensive study, the connection between our D 17 O- positive sulphate minerals and atmospheric oxidation processes is unequivocal, as shown by the close association with a high flux of atmospheric reduced sulphur compounds in our two reported cases. Gypcrete soils in the central Namib Desert occur extensively near the coast and gradually thin off and disappear at about 50–70 km from the coast, constituting one of the most extensive gypsum accumulations in Africa. On the basis of 34 S, meteorological, hydrological, and geological information, Eckardt and Spiro 13 suggest that sulphate in the Namib Desert originates mostly from biologically produced marine sulphur (that is, not derived from sea salt), particularly the oxidation of marine dimethyl sulphide (DMS). This conclusion is also supported by the lack of correlation between gypcrete accumulation and bedrock in this location and the positive correlation between gypcrete accumulation and the proximity to the ocean, a source of DMS. The Benguela Current, Table 1 Isotopic compositions and occurrences of the Namib gypcretes Sample 18 O 17 O D 17 O Depth below surface (cm) ............................................................................................................................................................................. GOR13-2 12.4 6.8 0.34 5 GOR13-3 8.3 4.6 0.33 16 GOR13-5 10.5 5.9 0.42 36 GOR13-6 11.6 6.4 0.35 52 GOR14-6 12.2 6.6 0.29 40 GBB16-6 11.8 6.4 0.26 45 GBB17-5 9.8 5.3 0.20 16 GBB17-6 9.5 5.2 0.26 46 GBB17-8 11.3 6.1 0.26 66 AUS6-5 9.9 5.6 0.40 10 SWA6-1 12.6 7.0 0.40 1 SWA6-2 12.0 6.6 0.31 9 (crack) SWA6-3 11.4 6.3 0.34 5 SWA6-4 13.2 7.3 0.40 24 SWA6-6 13.0 7.1 0.37 50 SWA6GYP 11.1 6.2 0.38 52 SWA6-7 10.1 5.8 0.51 70 SWA9-10 11.3 6.1 0.23 46 ............................................................................................................................................................................. Samples from the same soil profile are grouped together. Soil profiles are listed with decreasing distance from the ocean. Isotopic compositions are given in SMOW. 18 O = [(R sample /R standard ) - 1] × 1,000‰, where R is the number ratio 18 O/ 16 O. © 2000 Macmillan Magazines Ltd