Pressurised Extraction Using Dilute Ammonia: A Simple Method for Determination of Iodine in Soil, Sediment and Biological Samples by Inductively Coupled Plasma‐Mass Spectrometry

Abstract

A simple sample treatment method for the accurate and precise determination of iodine in soil, sediment and biological samples by inductively coupled plasma‐mass spectrometry (ICP‐MS) is described. Iodine in samples was extracted in screw top PTFE‐lined stainless steel bombs using a 10% v/v ammonia solution at 185 C for 18 hours (overnight), after which the extract was introduced into the ICP‐MS for direct measurement. 126Te was employed as the internal standard to compensate for matrix effects and instrument drift. The limit of detection (LOD, three times the standard deviation of the procedural blank solution, expressed as the concentration in the sample solution) was 0.003 ng ml‐‐1. The limit of quantitation (LOQ, ten times the standard deviation of the procedural blank solution, expressed as the concentration in the solid samples, dilution factor DF = 100) was 0.01 μg g‐‐1 (dry mass). The accuracy and precision of the method were demonstrated by analysing different Chinese geological certified reference materials (soils, stream sediments and a hair sample). The measured concentrations were in a good agreement with the certified values indicating that bias in the method was not significant. The precision (n = 10) for different concentrations ranged from 1.82% to 4.32% RSD. Comparison of the ammonia extraction procedure with a “sintering” method indicated that there was no significant difference in results obtained with the two methods for geological soil and stream sediment samples. However, for biological samples, such as hair, kelp, tea etc., the results obtained by the sintering method were far below those of the ammonia extraction method. The ammonia extraction has advantages, as it is simpler than the “sintering” method, and has a lower procedural blank, better detection limits and reproducibility. Due to the simplicity of the method, a high rate of sample throughput is possible.