Other
Scientific paper
Jul 1993
adsabs.harvard.edu/cgi-bin/nph-data_query?bibcode=1993metic..28r.380k&link_type=abstract
Meteoritics, vol. 28, no. 3, volume 28, page 380
Other
1
Cape York, Forest Vale, H Chondrites, Isotopic Anomalies, Jilin, Nitrogen
Scientific paper
Several research groups have studied contamination problems and molecular interferences in nitrogen isotope measurements, but some problems still require clarification. Protocols adopted for nitrogen isotope measurements generally consider questions such as CO interference, removal of hydrocarbons, and N2O and NO conversion [1]. In the analysis of nanogram amounts of N, contamination, exchange reactions, and interferences are more visible than in large N samples. During nitrogen measurements we observed several potential problems and developed an improved protocol to achieve high-quality isotopic data: 1. Nitrogen loss and isotopic exchange were observed on the extraction system wall. The wall has active surfaces produced by vapor deposition (previous samples) that absorb many molecules, including nitrogen. This absorbed nitrogen releases or exchanges nitrogen with sample N in the following extraction steps. Therefore the losses need to be calibrated and the extent of isotopic exchange determined at the nanogram level. A continuous adsorption during sample extraction of the gas phase onto zeolite at liquid nitrogen temperature reduces nitrogen loss and amount of exchange. 2. We also found nitrogen isotopic memory effect by CuO. During sample gas cleaning by CuO, nitrogen exchanges with residual nitrogen in the CuO, and losses to CuO by solubility and/or uptake of nitrogen during oxygen uptake. This effect is clearly visible after analysis of large amounts of nitrogen. In such cases the CuO blank showed traces of previously measured isotopic signatures. Therefore, the isotopic signature of the CuO blank must be assessed before proceeding. 3. NO interference was recognized. In measurements of N in bulk H chondrites, the steps above 900 degrees C show anomalous contribution to the mass 30 peak, which decreases rapidly with time in the mass spectrometer. Using the ratio mass 30 to mass 31 and the corresponding physical properties of the interfering compound, we identified the NO molecule. NO is produced during heating of the meteorites, and this molecule interacts with metal surfaces (e.g., valves and system metal). It is then released slowly from a metal surface and added to sample nitrogen during N transfer to the inlet volume of the mass spectrometer. Similar effects were reported last year [2], in addition to a rapid change of the measured 29/28 ratio. Hashizume and Sugiura concluded that curious phenomena indicate nonequilibria between two components, and thus the silicates in ordinary chondrites would not contain trapped nitrogen, which is in contradiction with their data. To eliminate the NO effect on mass 30, we made two modifications in the protocol. One is a final cleaning step of the gas phase using a glass finger at liquid nitrogen temperature; the other is the closing of the inlet valve after admitting the sample gas to the mass spectrometer. This protocol eliminates NO interference when the mass spectrometer is not contaminated by NO. 4. There are also nitrogen calibration issues. Last year nitrogen data for metal separates and bulk samples of some H chondrites were reported to reveal large isotopic variations (delta ^15N value from -44 to 119) [3]. Because Kung and Clayton [4] did not observe such variations, we measured nitrogen in Jilin (H5) and found a bulk average delta ^15N = 17 per mil. We also measured a metal separate from Forest Vale and observed a maximum value delta ^15N = 15 per mil. We were unable to confirm the value reported by [3]. We performed a series of calibrations against air nitrogen and NBS-steel standards to determine nitrogen loss and exchange, and against an internal meteorite standard (Cape York). Our analytical procedures are well reproduced. The NBS- steel and Cape York iron are therefore suitable as interlaboratory calibration standards for removal of experimental artifacts. References: [1] Boyd S. R. et al. (1988) J. Phys. E: Sci. Instrum., 21, 876- 885. [2] Hashizume K. and Sugiura N. (1992) GCA, 56, 1625-1631. [3] Hashizume K. and Sugiura N. (1992) Meteoritics, 27, 232. [4] Kung C. and Clayton R. N. (1978) EPSL, 38, 421-435.
Kim Jinyoung Serena
Marti Kurt
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