摘要
采用Delta V Advantage质谱仪与Gas Bench Ⅱ在线制样装置,分别用12mL和3.7mL的样品瓶,对不同质量(5~50eg)的碳酸盐标准样品(IAEA-CO-1)进行碳氧同位素组成测定。测试结果表明,当取样量小于40μg,且用12mL样品瓶进行酸化测试时,δ^13C和r^18O测量结果的内部标准偏差一半以上大于0.1‰,不能满足测试要求。当改用3.7mL样品瓶,样品取样量在15~50μg时,δ^13C的内部标准偏差为0.01‰~0.07‰,δ^18O的内部标准偏差为0.01‰~0.08‰,满足测试要求。所以,当样品量较少时,Gas BenchⅡ在线制样装置可以通过改用3.7mL样品瓶,实现对低至15μg微量碳酸盐样品的碳氧同位素精确测最。同时,碳酸盐样品的质量与峰面积具有很好的线性关系(R^2〉0.9932),表明该方法也可用于样品中碳酸盐含量的测定。
An analytical method for measuring carbon and oxygen isotopic compositions of trace amount carbonate (〉15μg) was established by Delta V Advantage isotope Ratio MS coupled with GasBench Ⅱ. Different trace amount (5-50μg) carbonate standard samples (IAEA-CO-1) were measured by GasBench Ⅱ with 12 mL and 3.7 mL vials. When the weight of samples was less than 40μg and it was acidified in 12 mL vials, most standard deviations of the δ^13C and δ^18O were more than 0.1‰, which couldn't satisfied high-precision measurements. When the weight of samples was grea ter than 15 μg and it was acidified in 3.7 mL vials, standard deviations for the δ^13C and δ^18O were 0. 01‰-0. 07‰ and 0.01‰-0. 08‰ respectively, which satisfied high-precision measurements. Therefore, small 3.7 mL vials were used to increase the concentration of carbon dioxide in headspace, carbonate samples even less as 15μg can be analyzed routinely by a GasBench Ⅱ continuous-flow IRMS. Meanwhile, the linear relationship between sample's weight and peak's area was strong (R^2〉0. 993 2) and it can be used to determine the carbon content of carbonate samples.
出处
《同位素》
CAS
2015年第1期41-47,共7页
Journal of Isotopes
基金
国家青年基金"河口地区硫酸盐还原过程随盐度梯度的变化规律及其控制因素"(41006072)