Analysis of low-level 129I in brine using accelerator mass spectrometry

Abstract

An improved solvent extraction procedure for iodine separation from brine samples has been applied at Xi’an Accelerator Mass Spectrometry (AMS) center. Oil in the brine sample has to be removed to avoid appearance of the third phase during solvent extraction and to improve the chemical yield of iodine. The small amount of oil remained in the water phase was first removed by phase separation through settling down sufficiently based on their immiscibility, and then by filtration through a cellulose filter, on which oil was absorbed and removed. After oil removed, extraction recovery of iodine could achieve more than 90 %. The sodium bisulfite as an effective reductant should be added before acidification to avoid loss of iodine by formation of I2 in sample via reaction of iodate and iodide at pH 1–2, and then pH was adjusted to 1–2 to reduce the iodate to iodide followed by oxidation of iodide to I2 and solvent extraction to separate all inorganic iodine. As a pre-nuclear era sample, 129I/127I ratio in brine is normally more than two orders of magnitude lower than that in present surface environmental samples, so prevention of cross-contamination and memory effect in apparatus during processing procedure are very critical for obtaining reliable results, and monitoring the procedure blank is very important for analytical quality of 129I. The 129I/127I isotopic ratio in the brine samples and procedure blank of iodine reagents were measured to be (1.9–2.7) × 10−13 and 2.08 × 10−13, respectively, 3–4 orders of magnitudes lower than that in environmental samples in Xi’an, and the result of procedure blank is in the same level as the previous experiments in past 3 years, indicating contamination is not observed in our method.