Quantification of Cl, Br and I in Geological Materials by NH4F Digestion: Comparison with Rapid Acid Digestion

Abstract

The lack of analytical techniques for halogens in geological materials is mainly due to the loss of analytes during sample preparation. This study describes a rapid bulk rock digestion method (NH4F digestion) for determination of the abundances of Cl, Br and I in geological materials by SF‐ICP‐MS. During high temperature (200–240 °C) digestion, NH3 released from the decomposition of molten NH4F can effectively prevent the loss of halogens released from geological samples. Chlorine, Br and I were not lost during NH4F digestion at 220 °C for 0.25–6 h. The limits of quantitation for NH4F digestion were 2.8, 0.018 and 0.003 μg g‐1 Cl, Br and I, respectively. Most results for halogens in geological reference materials by NH4F digestion were in agreement with their certified values, confirming that the high‐performance rapid bulk rock NH4F digestion has sufficient digestion capability to extract Cl, Br and I from rocks, sediments and soils. In comparison, results obtained following acid digestion showed that HNO3 + HF digestion could effectively extract Br and I from soil and sediment samples, and that HNO3 acid digestion is only suitable to use for the determination of Br and I in soil samples.