Single analysis of human hair for determining halogens and sulfur after sample preparation based on combustion reaction.

A single analysis of hair for determining halogens (chlorine, bromine, fluorine, and iodine) and sulfur by ion chromatography with suppressed conductivity and mass spectrometry detection (IC-MS) was proposed. Inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS) were also used to compare the results. For this purpose, 300 mg of human hair were digested by microwave-induced combustion (MIC) using 20 bar of oxygen pressure. The analytes were absorbed in 100 mmol L NHOH. Trueness of the proposed method was evaluated by analysis of a CRM of human hair; by recovery tests, using standard solution at two levels (50% and 100%), and by comparison of results with those obtained by ICP OES (Cl and S) and ICP-MS (Br and I). Suitable recoveries (ranging from 92 to 105%) were obtained, and the results from CRM analysis did not differ significantly from those described in the certificate. Moreover, results obtained by IC-MS did not present significant differences (p > 0.05) from those obtained by ICP OES and by ICP-MS. Precision was evaluated in terms of repeatability and intermediate precision, and the relative standard deviations were always lower than 8%. The proposed method presented good accuracy and it is a reliable strategy for human hair analysis. Final digests obtained using the MIC method were fully compatible with all proposed determination techniques. Compared to others reported in the literature, the proposed method presents several advantages, especially given that it is possible to determine halogens and sulfur in a single analysis. Graphical abstract.