微波消解-电感耦合等离子体原子发射光谱法测定冷轧乳化液废水中铁锌铜镍铅镉  

Determination of iron, zinc, copper, nickel, lead and cadmium in cold rolling emulsion wastewater by inductively coupled plasma atomic emission spectrometry with microwave digestion

作　　者：董礼男 张继明 赵希文 朱春要 DONG Linan;ZHANG Jiming;ZHAO Xiwen;ZHU Chunyao(Institute of Research of Iron&Steel,Shagang,Jiangsu Province,Zhangjiagang 215625,China)

机构地区：[1]江苏省(沙钢)钢铁研究院,江苏张家港215625

出　　处：《冶金分析》2022年第10期51-56,共6页Metallurgical Analysis

摘　　要：轧钢生产过程中产生的含轧制油、乳化剂及少量重金属的一类废水,常被称为冷轧乳化液废水。这类液体废物中含有的重金属元素若处理不当,会对环境造成严重的污染,因此准确测定冷轧乳化液废水中重金属含量对其后续处理方案的选择具有指导作用。采用硝酸、盐酸、过氧化氢酸溶体系并使用微波消解法消解样品,可有效消解有机物质且不会造成待测元素的损失。选择Fe 259.940 nm、Zn 209.994 nm、Cu 324.754 nm、Ni 231.604 nm、Pb 220.353 nm、Cd 226.502 nm作为分析谱线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定冷轧乳化液废水中铁、锌、铜、镍、铅、镉的方法。讨论了样品前处理方式、消解酸及其用量,研究了共存元素对铁、锌、铜、镍、铅、镉测定的影响。结果表明:在仪器的最优工作条件下,各元素校准曲线的线性相关系数均不小于0.999 6;铁、锌、铜、镍、铅、镉的检出限分别为0.004 9、0.002 1、0.002 0、0.001 2、0.001 4和0.001 0 mg/L。对冷轧乳化液废水中铁、锌、铜、镍、铅、镉含量进行测定,各元素测定结果的相对标准偏差(RSD,n=7)为0.32%~2.8%,加标回收率为96%~104%。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%.

关 键 词：电感耦合等离子体原子发射光谱法(ICP-AES) 冷轧乳化液 废水 铁 锌 铜 镍 铅 镉 微波消解法 

分 类 号：O657.31[理学—分析化学] TF033[理学—化学]