Separation of CO2 from SO2 with Frozen n-Pentane as a Technique for the Precision Analysis of 18O in Sulfates

Mizutani, Yoshihiko; Oana, Shinya

doi:10.5702/massspec1953.21.255

Cited by 22 publications

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“…The combustion was forcibly completed by circulating oxygen with a glass fan and by passing the evolved gas through a column filled with copper oxide at 750°C. The CO 2 was finally trapped with liquid nitrogen and further purified against SO 2 by an /?-pentane frozen technique developed by Mizutani and Oana (1973). Carbon dioxide thus purified was subjected to mass-spectrometric analysis.…”

Section: Methodsmentioning

confidence: 99%

Deep Sea Carbonate Nodules from the Middle America Trench Area off Mexico, Deep Sea Drilling Project Leg 66

Wada¹,

Niitsuma²,

Nagasawa³

et al. 1982

Initial Reports of the Deep Sea Drilling Project

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We collected 20 carbonate nodules from the inner trench slope deposits of the Middle America Trench area off Mexico. Carbonate nodules are found only within the methane-rich layer beneath the mixed layer of methane and hydrogen sulfide. They have been investigated by microscopic, scanning electron microscopic (SEM), X-ray diffraction, and stable isotopic analytical methods. Calcite, magnesian calcite, dolomite, and rhodochrosite were recognized as carbonate minerals. Each carbonate nodule is usually represented by single species of carbonate minerals. Carbonate nodules are subdivided into micrite nodules and recrystallized nodules according to textural features. The carbonate crystallites in each micrite nodule are equidimensional. Their sizes range from several to 30 µm, as revealed by SEM micrographs.The chemical composition of calcite is changed from pure calcite to high magnesian calcite, as shown by the shift of the (104) reflection in X-ray diffraction patterns. Fe substitution for Ca in dolomite was also observed.Carbon isotopic composition shows an unusually wide range-from -42.9 to + 13.5% O -in PDB scale, whereas oxygen isotopic compositions of almost all the carbonate nodules are constantly enriched in 18 O from + 3.4 to + 7.60% 0 in PDB scale. These wide variations in carbon isotopic composition indicate several sources for the carbon in carbonate nodules. Carbon with a negative δ 13 C value was derived from biochemical oxidation of methane with a negative δ 13 C value. On the other hand, carbon with positive δ 13 C value was probably formed during methane production in an anoxic condition.

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Section: Methodsmentioning

confidence: 99%

Deep Sea Carbonate Nodules from the Middle America Trench Area off Mexico, Deep Sea Drilling Project Leg 66

Wada¹,

Niitsuma²,

Nagasawa³

et al. 1982

Initial Reports of the Deep Sea Drilling Project

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“…The SO produced was cryogenically puri ed using a vacuum preparation line [42]. The isotopic analyses were carried out using the Delta Advantage V mass spectrometer in the Laboratory of Isotope Geology and Geoecology, Department of Applied Geology and Geochemistry, Institute of Geological Unauthenticated Download Date | 5/11/18 12:24 PM Sciences, University of Wrocław.…”

Section: Decomposition Of Polysul Desmentioning

confidence: 99%

Variability of sulfur speciation in sediments from Sulejów,Turawa and Siemianówka dam reservoirs (Poland)

et al. 2015

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Abstract:A study on sulfur circulation in sediments was carried out in dam reservoirs (Sulejów, Siemianówka, Turawa) with di erent hydrological and age characteristics as well as with a di erent level of sediment accumulation and organic matter content. Di erences in the isotopic composition of SO − in the water column and small variations in the concentration of this ion were observed in the Turawa reservoir. The investigations did not show vertical variation in the watercolumn concentrations and isotopic composition. This is due to the small depths of the reservoir and mixing of water. A part of sulfate sulfur from the water column is reduced by incorporating it into cell structures, while a part of it is deposited in the sediment. The study revealed a small exchange of SO − between the water column and the sediment. Depending on the season of the year and the sediment sampling site, biogeochemical transformations of sulfur species are observed. A signi cant variation in the biogeochemical processes was found between the Siemianówka and Sulejów reservoirs, both in the concentrations and in the isotopic composition of particular sulfur species. This primarily results from the di erent characteristics of either of these reservoirs ( ows, sedimentation, and material discharge to the lake). The main source of sulfur supplied to the sediments in the Siemianówka reservoir is organic sulfur contained in organic matter deposited at the bottom. In the sediment, organic sulfur is bacterially oxidized and xed as SO − .This is manifested in a substantial enrichment of sulfate in S. The presence of polysul des was found in both reservoirs, but a distinct depletion of δ S(S − ) in the light sulfur isotope was observed in the Siemianówka reservoir. In a part of the Sulejów reservoir, polysul des are oxidized to SO − ,probably at the sediment/water interface.

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“…To separate CO 2 from SO 2 (Eq. 1), the remaining gas was processed with an open n-pentane bath immersed in liquid nitrogen (from here on referred to as "pentane trap") that was similar in configuration to that of Mizutani and Oana (1973), but with dimensions given by Kusakabe (2005). It should be noted that n-pentane is a highly flammable liquid that exerts high vapor pressure at ambient temperature.…”

Section: Materials and Proceduresmentioning

confidence: 99%

“…Therefore, this trap should never be used near an open flame. The details of the separation procedure have been described elsewhere (Oana and Ishikawa 1966;Mizutani and Oana 1973;Kusakabe 2005). In principle, the two gases are separated near the melting point of n-pentane (-130.8°C), at which point CO 2 exerts measurable vapor pressure, while SO 2 does not.…”

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confidence: 99%

Determination of radiocarbon in marine sediment porewater dissolved organic carbon by thermal sulfate reduction

Johnson

Komada

2011

Limnology & Ocean Methods

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Fractional abundances of 14 C and 13 C in dissolved organic carbon (DOC) in sediment porewaters may hold important clues about organic carbon cycling in sediments. Yet there is a dearth of isotopic signatures for porewater DOC because of the difficulty associated with oxidizing DOC in seawater. At present, marine DOC can be processed for analyses of 14 C and 13 C with high precision and minimal contamination by ultraviolet (UV) oxidation, but this method is resource intensive and could be difficult to implement. To resolve this, a thermal sulfate reduction (TSR) method, previously developed to determine 13 C in seawater DOC (Fry et al. 1996), was modified and tested for 14 C and 13 C determination in porewater DOC. CO 2 yields from six test materials ranged between 90% and 108%. d Application of TSR to archived porewater DOC samples from a sediment incubation experiment revealed notable changes in isotopic values that were not readily discerned in the DOC concentration data alone. The total uncertainty in the 14 C values after blank correction was ± 0.005 to 0.02 fraction modern (Fm) for sample sizes ranging between 143 and 560 µg C. For systems where precision on the order of ± 0.02 Fm is acceptable, TSR could be a viable alternative to UV oxidation for processing small, concentrated marine DOC samples. *Corresponding author: E-mail: tkomada@sfsu.edu AcknowledgmentsWe thank Ann McNichol for encouraging us to pursue this method and for sharing the protocol that she and Bill Martin developed. Sheila Griffin and Ellen Druffel generated the UV oxidation data, ran our AMS samples, and provided many helpful discussions. Xiaomei Xu provided assistance in radiocarbon data interpretation. Sabrina Crispo ran the TOC-V and assisted in the laboratory and in the field. We thank the captain and crew of R/V Point Sur, J. Polly, R. Paul, D. Burdige, M. Jinuntuya, and A. Pitts for the work conducted in the Santa Monica Basin. Three anonymous reviewers provided comments that helped improve the quality of this manuscript. This work was supported by NSF-OCE0726819 (TK) and James C Kelley Scholarship (LJ).Acknowledgment is made to the Donors of the American Chemical Society Petroleum Research Fund for partial support of this research (ACS-PRF #46120-GB2 to TK). DOI 10.4319/lom.2011.9.485 Limnol. Oceanogr.: Methods 9, 2011, 485-498 © 2011, by the American Society of Limnology and Oceanography, Inc. LIMNOLOGY and OCEANOGRAPHY: METHODSues for marine porewater DOC have been reported in only a handful of studies (Bauer et al. 1995; Alperin et al. 2000).Several different methods have been developed to oxidize DOC to CO 2 for subsequent determination of 14 C and 13 C. As summarized by Bauer (2002), these can be broadly categorized into three types: (1) UV oxidation (Armstrong et al. 1966;Williams 1968; Williams et al. 1969; Williams and Gordon 1970;Druffel et al. 1989; Bauer et al. 1998;Beaupré et al. 2007), (2) sealed-tube dry combustion (Fry et al. 1993; Fry et al. 1996), and (3) flow-through high-temperature oxidation (Bauer ...

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Separation of CO2 from SO2 with Frozen n-Pentane as a Technique for the Precision Analysis of 18O in Sulfates

Cited by 22 publications

References 0 publications

Deep Sea Carbonate Nodules from the Middle America Trench Area off Mexico, Deep Sea Drilling Project Leg 66

Deep Sea Carbonate Nodules from the Middle America Trench Area off Mexico, Deep Sea Drilling Project Leg 66

Variability of sulfur speciation in sediments from Sulejów,Turawa and Siemianówka dam reservoirs (Poland)

Determination of radiocarbon in marine sediment porewater dissolved organic carbon by thermal sulfate reduction

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