改装元素分析—稳定同位素比值质谱联用仪测定固体样品硫同位素

Modification of Elemental Analysis-Stable Isotope Ratio Mass Spectrometer Combined Instrument for Determination of Sulfur Isotopes in Solid Samples

  • 摘要: 本文对元素分析—稳定同位素比值质谱联用仪(EA-IRMS)进行改装,并利用其测定不同形态硫同位素标准物质和样品。结果表明,在色谱柱后加装SO2气体捕集管,可捕集氧化还原产生的SO2气体,并重复调用作为参考气使用,无需外部引入高纯SO2气体,减小了其对仪器管路腐蚀和实验室环境危害;硫酸钡进样量约400 μg时,捕集管中的SO2气体可提供至少20次峰中心聚焦;改装后的EA-IRMS系统测试硫同位素标准物质(IAEA-SO-5、 IAEA-S-2、IAEA-S-3、EMA-P1),当硫元素进样量为20 μg时,δ34S值测试精度达到0.2‰(n=3),4种国际标准物质测量值与真实值相关系数良好(R2=1),表明硫的不同化合物δ34S值可以相互校准,也表明EA-IRMS改装后可以满足硫同位素测试精度的要求。

     

    Abstract: In this paper, the elemental analysis-stable isotope ratio mass spectrometer (EA-IRMS) is modified to testing different forms of sulfur isotope standard material and sample. A SO2 gas trap tube is installed after chromatographic column to trap the SO2 gas generated by redox reaction and the captured SO2 can be used as reference gas several times, there is no need to introduce high-purity SO2 gas externally, which reduces the damage to the instrument pipeline corrosion and laboratory environment. When the amount of barium sulfate is about 400 μg, SO2 gas in the trap tube can provide at least 20 peak center focus. Modified EA-IRMS system testing sulfur isotope standard material (IAEA-SO-5, IAEA-S-2, IAEA-S-3, EMA-P1), when the sulfur element injection volume is 20 μg, the δ34S value test accuracy achieve 0.2‰(n=3), 4 kinds of international standard material measured value and true value have a good correlation coefficient (R2=1), it indicates that the δ34S value of different compounds of sulfur can be mutual calibration, and the modified EA-IRMS can meet the accuracy requirement of the sulfur isotope test.

     

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