Determination of inorganic chlorine stable isotopes by continuous flow isotope ratio mass spectrometry

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 mumol 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 +/-0.04parts per thousand (+/-STDV). The external precision using seawater standard is better than +/-0.07parts 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. Copyright (C) 2004 John Wiley Sons, Ltd.