Determination of thallium in manganese ore by inductively coupled plasma atomic emission spectrometry afterion exchange separation
XIE Xiao-yan1, WU Wen-qi1, LI Fen1, LIAO Hong-mei2 , LIU Yuan-yuan1
1. Liuzhou Entry-Exit Inspection and Quarantine Bureau, Liuzhou 545006, China; 2. The Technology Center of Guangxi Entry-Exit Inspection and Quarantine Bureau, Nanning 530022, China
Abstract:The manganese ore was dissolved with hydrochloric acid, nitric acid, hydrofluoric acid and perchloric acid. The pH of sample solution was adjusted to 1.7-2.0 with sodium hydroxide solution. The Tl(Ⅰ) in solution was oxidized to Tl(Ⅲ) with bromine water. After D401 ion exchange resin column and elution with 0.015 mol/L of nitric acid, the Tl(Ⅲ) on column was reduced to Tl(Ⅰ) with 2 mL of 3 g/L sulfurous acid solution. Then, the Tl(Ⅰ) was eluted with 0.015 mol/L nitric acid solution. The Tl 190.857 nm was selected as the analytical line. The content of thallium in solution after separation was determined by inductively coupled plasma atomic emission spectrometry. The detection limit of method was 1 ng/mL, and the lower determination limit was 0.8 μg/g. The interference test results showed that tolerant amount of co-existing ions for 0.1 μg/mL of thallium was listed as following (in μg/mL): iron (50); manganese (2); aluminum, cadmium, chromium, nickel, lead and zinc (10). The general manganese ore samples were separated and determined according to the experimental method. The iron, manganese, aluminum, cadmium, chromium, nickel, lead and zinc did not interfere with the determination of thallium. The thallium in manganese ore sample was determined according to the experimental method. The relative standard deviations (RSD, n=8) of determination results were between 1.6% and 11%, and the recoveries of standard addition were between 90% and 108%.
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