A modified procedure for gas-source isotope ratio mass spectrometry: the long-integration dual-inlet (LIDI) methodology and implications for clumped isotope measurements
Zhou Liping, et al.
High-precision stable isotope measurements in gas-source isotope ratio mass spectrometry are generally carried out by repeated comparison of the composition of an unknown sample with that of a working gas (WG) through a dual-inlet (DI). Due to the established DI protocols, however, most of the sample gas is wasted rather than measured, which is a major problem when sample size is limited. Here we propose a new methodology allowing the measurement of a much larger portion of the available sample. We tested a new measurement protocol, the long-integration dual-inlet (LIDI) method, which consists of a single measurement of the sample for 200 to 60065seconds followed by a single measurement of the WG. The isotope ratios of the sample are calculated by comparison of the beam ratios of the WG and sample at equivalent intensities of the major ion beam. Three isotopically very different CO2 samples were analyzed. The LIDI measurements of large samples (50 to 1006508mol of CO2) measured at quasi-constant beam sizes, and of small samples (1.5 to 26508mol of CO2) measured in micro-volume mode, generated results that are indistinguishable from the standard DI measurements for carbon, oxygen and clumped isotope compositions. The external precision of Δ47 using the LIDI protocol (-±0.007‰) is similar to that of the state of the art DI measurements. For traditional and clumped isotope measurements of CO2, the LIDI protocol allows the measurement of a much larger portion of the sample gas rather than only ~20% of it. In addition, the sample can be measured at higher signal intensity and for longer time, allowing the measurement of smaller samples while preserving precision. We suggest that other gases commonly used for stable isotope measurements with gas-source mass spectrometry would also benefit from this new protocol.
Hu B, Radke J, Schlüter H J, et al. A modified procedure for gas‐source isotope ratio mass spectrometry: the long‐integration dual‐inlet (LIDI) methodology and implications for clumped isotope measurements[J]. Rapid Communications in Mass Spectrometry, 2014, 28(13): 1413-1425.
刘雪萍, 周力平, 马丹. 鄂霍次克海叶绿素浓度反演及其与海冰的关系[J]. 第十八届中国环境遥感应用技术论坛论文集, 2014.
Rapid sample preparation of dissolved inorganic carbon in natural waters using a headspace-extraction approach for radiocarbon analysis by accelerator mass spectrometry
Zhou Liping, et al.
We have established a high-throughput headspace-extraction method for the preparation of dissolved inorganic carbon (DIC) from water samples for radiocarbon (14 C) analysis by accelerator mass spectrometry (AMS). Readily available septum-sealed screw cap vials were used for sample processing. Headspace-equilibrated gases with sample CO 2 were transferred using a syringe and cryogenically purified on a vacuum line for graphitization and 14 C-AMS measurements in the Keck Carbon Cycle AMS facility at the University of California, Irvine (KCCAMS/UCI). Systematic investigations have shown that the extraction process does not introduce contaminants that could bias the 14 C measurements and that the 14 C results for standards are consistent with their consensus values. Large numbers of duplicate measurements have established a precision of 1.7‰ for modern samples with an average background of 43,400 radiocarbon year for graphite target samples > 0.3 mg carbon. Seawater samples collected from Newport Beach, California, and processed using the headspace-extraction method yielded 14 C results in excellent agreement with published values obtained with conventional DIC stripping (≤ 2σ). The simplicity of our headspace-extraction approach allows its easy adaptation/implementation to any isotope lab, as we demonstrate here by a series of tests carried out at Peking University, China (PKU). With this innovative method, just 30 mL seawater per sample is needed. Coupled with the sealed tube zinc reduction method, 15 water samples can be prepared and graphitized in 1 day.
Gao P, Xu X, Zhou L, et al. Rapid sample preparation of dissolved inorganic carbon in natural waters using a headspace‐extraction approach for radiocarbon analysis by accelerator mass spectrometry[J]. Limnology and Oceanography: Methods, 2014, 12(4): 174-190.