Minimization of Volatile Nitrogen Oxides Interference in the Determination of Arsenic by Hydride Generation Atomic Absorption Spectrometry

摘要

In this study emphasis was given to minimize the interference of volatile nitrogen oxides from digestion procedures with nitric acid on the determination of arsenic by hydride generation atomic absorption spectrometry (HG AAS). Sulfamic acid (SA) is proposed to minimize this interference by employing three procedures for the digestion of hair in closed systems: conventional and microwave (MW) heating in polytetrafluorethylene (PTFE) vessels and by MW heating in glass vials. Hair samples were digested with H_2SO_4 + HNO_3 or HNO_3 + H_2O_2 mixtures. Concentrated hydrochloric acid was added for the digestion for the procedure in glass vials. The accuracy of the procedures with PTFE vessels was verified by the spike recoveries of organic (p-aminobenzenearsonic acid and dimethyl arsinic acid, from 92 to 101%) and inorganic (sodium arsenate, from 98 to 102%) arsenic compounds. For the procedure in glass vials the recevery was from 86 to 97% for organic As and from 97 to 102% for inorganic As. The results obtaiond for a certified hair reference material using the three digestion procedures were well within the 95% confidence interval of the certificate when SA was added to the solutions. However, when SA was not added, recoveries were low and non-reproducible signals and high background levels were observed. Urea, benzoic acid and hydroxylamine hydrochloride were also studied (maximum As recovery of 90% using hydroxylamine hydrochloride) but the best results were obtained with use of SA.