Komatsu Daisuke D, Ishimura Toyoho, Nakagawa Fumiko, Tsunogai Urumu
Earth and Planetary System Sciences, Faculty of Science, Hokkaido University, N10 W8, Sapporo 060-0810, Japan.
Rapid Commun Mass Spectrom. 2008 May;22(10):1587-96. doi: 10.1002/rcm.3493.
We developed a rapid, sensitive, and automated analytical system to determine the delta15N, delta18O, and Delta17O values of nitrous oxide (N2O) simultaneously in nanomolar quantities for a single batch of samples by continuous-flow isotope-ratio mass spectrometry (CF-IRMS) without any cumbersome and time-consuming pretreatments. The analytical system consisted of a vacuum line to extract and purify N2O, a gas chromatograph for further purification of N2O, an optional thermal furnace to decompose N2O to O2, and a CF-IRMS system. We also used pneumatic valves and pneumatic actuators in the system so that we could operate it automatically with timing software on a personal computer. The analytical precision was better than 0.12 per thousand for delta15N with >4 nmol N2O injections, 0.25 per thousand for delta18O with >4 nmol N2O injections, and 0.20 per thousand for Delta17O with >20 nmol N2O injections for a single measurement. We were also easily able to improve the precision (standard errors) to better than 0.05 per thousand for delta15N, 0.10 per thousand for delta18O, and 0.10 per thousand for Delta17O through multiple analyses with more than four repetitions with 190 nmol samples using the automated analytical system. Using the system, the delta15N, delta18O, and Delta17O values of N2O can be quantified not only for atmospheric samples, but also for other gas or liquid samples with low N2O content, such as soil gas or natural water. Here, we showed the first ever Delta17O measurements of soil N2O.
我们开发了一种快速、灵敏且自动化的分析系统,通过连续流同位素比率质谱法(CF - IRMS),无需任何繁琐耗时的预处理,就能同时测定一批纳摩尔量样品中氧化亚氮(N₂O)的δ¹⁵N、δ¹⁸O和Δ¹⁷O值。该分析系统由用于提取和纯化N₂O的真空管路、用于进一步纯化N₂O的气相色谱仪、用于将N₂O分解为O₂的可选热炉以及CF - IRMS系统组成。我们还在系统中使用了气动阀和气动执行器,以便能够通过个人计算机上的定时软件自动操作该系统。对于单次测量,当注入的N₂O大于4 nmol时,δ¹⁵N的分析精度优于0.12‰;当注入的N₂O大于4 nmol时,δ¹⁸O的分析精度优于0.25‰;当注入的N₂O大于20 nmol时,Δ¹⁷O的分析精度优于0.20‰。通过使用该自动化分析系统,对190 nmol样品进行四次以上重复的多次分析,我们还能够轻松地将精度(标准误差)提高到δ¹⁵N优于0.05‰、δ¹⁸O优于0.10‰、Δ¹⁷O优于0.10‰。使用该系统,不仅可以对大气样品中的N₂O的δ¹⁵N、δ¹⁸O和Δ¹⁷O值进行定量,还可以对其他N₂O含量低的气体或液体样品,如土壤气体或天然水中的这些值进行定量。在此,我们展示了首次对土壤N₂O的Δ¹⁷O测量。