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《Metallurgical Analysis》 2009-04
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Determination of antimony and bismuth in caustic calcined magnesite by microwave digestion-hydride generation atomic fluorescence spectrometry

ZENG Ze,XIE Yan ,HU Xiao-jing , LU Qi(Liaoning Exit-Entry Inspection and Quarantine Bureau,Dalian 116001,China)  
The determination of antimony and bismuth in caustic calcined magnesite by microwave digestion-hydride generation atomic fluorescence spectrometry was studied and the optimum experimental conditions were discussed. Samples were thoroughly dissolved in the mixed solution of hydrochloric acid and nitric acid (9+1) to ensure the high valency of antimony and bismuth. Volume fraction of the acid was controlled at 20 % to prevent antimony and bismuth from hydrolization. Ascorbic acid was employed to reduce antimony. Thiourea was added to eliminate interference of impurities( especially that of transitional heavy metals). The detection limit was 0.04 mg/kg for Sb and 0.003 mg/kg for Bi. In range of 1-32 ng/mL, good linearity was shown between the content of antimony or bismuth with fluorescence intensity . Through 12 times of repeated tests, relative standard deviation was 7.1% for 0.2 mg/kg antimony and 2.3 % for 0.02 mg/kg bismuth. This method was applicable to the determination of antimony and bismuth in caustic calcined magnesite with the recovery of 98 %-103 % for Sb and 100 %-113 % for Bi.
【CateGory Index】: TG115.3
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