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A method using solvent extraction following a preconcentration of iodine by evaporation was developed for separation of iodine in waters associated with coalbed methane (CBM) for the determination of 129I using accelerator mass spectrometry, for exploration of CBM resources. The 129I/127I ratios in water samples collected in a CBM field have been determined using the developed method to be (1.6–2.4) × 10–11, which are 2–3 orders of magnitudes lower than that of environmental samples in Xi'an, but 2 orders of magnitude higher than the procedure blank of (1.5–2.1) × 10–13, confirming no measurable crossover contamination during sample analysis and slightly input of modern water in the CBM water. [ABSTRACT FROM AUTHOR]