Determination of cadmium and lead in phosphate ore and phosphate fertilizer by solid phase extraction-inductively coupled plasma atomic emission spectrometry
LU Ke1, ZHENG Xiang-ming2, WU Xue-ying2, GONG Qi*1, WANG Kun-qi1, LI Min1
1.College of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China; 2.China Certification & Inspection Guangxi Co., Ltd., Fangchenggang 538001, China
Abstract：The direct determination of Cd and Pb in phosphate ore and phosphate fertilizer by inductively coupled plasma atomic emission spectrometry (ICP-AES) is usually interfered by coexisting elements such as P and Ca. When the mass concentration of P and Ca in testing solution was 10 times higher than that of Cd and Pb, the relative errors of direct determination results of Cd and Pb exceeded 5%. However, the contents of Cd and Pb in phosphate ores and phosphate fertilizers were much higher than this value. It was found that the Cd (Ⅱ) and Pb(Ⅱ) in sample solution could be quantitatively extracted by strongly basic anion exchange fiber (SBAEF) in medium at pH≈2 containing 0.01 g/mL ascorbic acid and 0.20 mol/L KI. Meanwhile, Ca2+, PO43－ and other cations were not extracted. The extracted Cd(Ⅱ) and Pb(Ⅱ) by SBAEF could be quantitatively eluted using 0.07 mol/L EDTA solution, and then determined by ICP-AES. The interference of coexisting elements such as P and Ca could be eliminated. The mass concentration of Cd and Pb in range of 1.00×10-3-2.00 μg/mL and 2.00×10-2-40.0 μg/mL was linear to the emission intensity. The linear correlation coefficient (R2) was 0.999 294 and 0.999 984, respectively. The low limit of determination of Cd and Pb in this method was 6.00×10-2 μg/g and 2.00×10-1 μg/g, respectively.The content of Cd and Pb in simulated sample was analyzed according to the experimental method. The found results were consistent with the theoretical values.The proposed method was applied to the determination of Cd and Pb in actual samples of phosphate ore and phosphate fertilizer. The relative standard deviations (RSD, n=5) were less than 4.4%. The proposed method was also applicable for the determination of Cd and Pb in phosphate ores and phosphate fertilizers by flame atomic absorption spectrometry (FAAS).
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