Determination of iron,zinc,copper,nickel,lead and cadmium in cold rolling emulsion wastewater by inductively coupled plasma atomic emission spectrometry with microwave digestion
DONG Linan, ZHANG Jiming, ZHAO Xiwen, ZHU Chunyao
Institute of Research of Iron & Steel, Shagang, Jiangsu Province, Zhangjiagang 215625, China
Abstract：Cold rolling emulsion wastewater containing rolling oil, emulsifier and heavy metal elements is produced in steel rolling process. It will cause serious pollution to the environment if the heavy mental elements in such wastewater are improperly treated. Therefore, the accurate determination of heavy metal elements in cold rolling emulsion wastewater is important to guide the selection of subsequent treatment schemes. The sample was treated by microwave digestion with nitric acid, hydrochloric acid and hydrogen peroxide. The organic matters could be effectively digested without the loss of testing elements. Fe 259.940 nm, Zn 209.994 nm, Cu 324.754 nm, Ni 231.604 nm, Pb 220.353 nm and Cd 226.502 nm were selected as the analytical lines. The method for the determination of Fe,Zn,Cu,Ni,Pb and Cd in cold rolling emulsion wastewater by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The sample pretreatment method, digestion acids and dosages were discussed. The influence of coexisting elements on the determination of Fe, Zn, Cu, Ni, Pb and Cd was studied. The results showed that under the optimized working condition of instrument, the linear correlation coefficients of calibration curves for elements were all not less than 0.999 6. The limits of detection were 0.004 9, 0.002 1, 0.002 0, 0.001 2, 0.001 4 and 0.001 0 mg/L for Fe,Zn,Cu,Ni,Pb and Cd, respectively. The contents of Fe,Zn,Cu,Ni,Pb and Cd in cold rolling emulsion wastewater were determined. The relative standard deviations (RSD, n=7) were between 0.32% and 2.8%, and the recoveries were between 96% and 104%.
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