Shouakar-Stash Orfan, Drimmie Robert J, Frape Shaun K
Department of Earth Sciences, University of Waterloo, 200 University Ave. W., Waterloo, Ontario, Canada N2L 3G1.
Rapid Commun Mass Spectrom. 2005;19(2):121-7. doi: 10.1002/rcm.1762.
Chlorine stable isotope analyses of inorganic samples were conducted using continuous flow isotope ratio mass spectrometry (CF-IRMS) coupled with gas chromatography (GC). Inorganic chloride was precipitated in the form of silver chloride (AgCl) by using silver nitrate in a standard methodology. Chlorine stable isotope analysis was carried out on methyl chloride (CH3Cl) after converting AgCl into CH3Cl by reacting it with methyl iodide (CH3I). The reaction between AgCl and CH3I took place in 20 mL size vials. Addition of CH3I was performed in a glove bag under helium flow. An Agilent 6890 gas chromatograph equipped with a CTC Analytics CombiPAL autosampler and a DB-5MS 60 m column was used to separate CH3Cl from CH3I. This new technique uses samples as small as 0.2 mg of AgCl (1.4 micromol of Cl-). The chlorine stable isotope analysis using continuous flow technology showed excellent precision and accuracy. The internal precision using pure CH3Cl gas is better than +/-0.04 per thousand (+/-STDV). The external precision using seawater standard is better than +/-0.07 per thousand (+/-STDV) for n=12. Moreover, the sample analysis time is much shorter and many more samples can be analyzed in one day than by using the conventional off-line techniques.
使用与气相色谱(GC)联用的连续流同位素比率质谱仪(CF-IRMS)对无机样品进行氯稳定同位素分析。采用标准方法,用硝酸银将无机氯化物以氯化银(AgCl)的形式沉淀出来。通过使AgCl与甲基碘(CH3I)反应将其转化为CH3Cl后,对CH3Cl进行氯稳定同位素分析。AgCl与CH3I之间的反应在20 mL的小瓶中进行。在氦气流下于手套箱中加入CH3I。使用配备CTC Analytics CombiPAL自动进样器和DB-5MS 60 m色谱柱的安捷伦6890气相色谱仪将CH3Cl与CH3I分离。这项新技术使用的样品量低至0.2 mg的AgCl(1.4 μmol的Cl-)。采用连续流技术进行的氯稳定同位素分析显示出极高的精密度和准确度。使用纯CH3Cl气体的内部精密度优于±0.04‰(±标准偏差)。对于n = 12,使用海水标准的外部精密度优于±0.07‰(±标准偏差)。此外,样品分析时间更短,与使用传统离线技术相比,一天内可分析的样品更多。