微波消解-电感耦合等离子体原子发射光谱法测定烧结除尘灰中9种元素

Determination of nine elements in sintering dedusting ash by inductively coupled plasma atomic emission spectrometry after microwave digestion

中国工业生产过程中,每年产生近亿吨的烧结除尘灰,而准确测定烧结除尘灰中元素含量,可大大提高烧结除尘灰的回收利用率。针对烧结除尘灰中铁、碳元素含量较高的问题,实验采用盐酸-硝酸-氢氟酸以微波消解的方式溶解烧结除尘灰样品,高效溶解样品可消除碳元素干扰;采用基体匹配法配制标准系列溶液,选用谱线拟合校正(FACT)与自动匹配法相结合方式可有效校正基体铁元素的干扰。最终选择K 766.491nm、Na 588.995nm、Ca 317.933nm、Mg 285.213nm、Al 308.215nm、Zn 206.200nm、Pb 283.305nm、Cu 324.754nm、P 177.434m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)测定烧结除尘灰中钾、钠、钙、镁、铝、锌、铅、铜、磷的方法。结果表明,在仪器最优工作状态下,各元素校准曲线线性相关系数均大于0.9990,各元素定量限为0.0006%~0.0032%。方法应用于2个烧结除尘灰样品中9种元素的测定,结果的相对标准偏差(RSD,n=6)均小于5.0%。分别使用实验方法与其他化学方法测定相同烧结除尘灰样品中钾、钠、钙、镁、铝、锌、铅、铜、磷,测定结果基本一致。

Nearly 100 million tons of sintering dedusting ash are produced in the process of industrial production in China every year.The accurate determination of elemental contents in sintering dedusting ash can greatly improve its recovery and reuse rate.Since the content of iron and carbon in sintering dedusting ash was relatively high,the sample was dissolved in hydrochloric acid-nitric acid-hydrofluoric acid by microwave digestion.The efficient dissolution of sample could eliminate the interference of carbon.The standard series solution was prepared by matrix matching method.Fast Automated Curve-Fitting(FACT)and automatic matching method were combined to effectively correct the interference caused by matrix iron.K 766.491nm,Na 588.995nm,Ca 317.933nm,Mg 285.213nm,Al 308.215nm,Zn 206.200nm,Pb 283.305nm,Cu 324.754nm and P 177.434nm were selected as the analytical lines.The determination method of potassium,sodium,calcium,magnesium,aluminum,zinc,lead,copper and phosphorus in sintering dedusting ash by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The results showed that the linear correlation coefficients of calibration curves were all greater than 0.9990 under the optimal working conditions of instrument.The limits of quantification for elements were between 0.0006%and 0.0032%.The proposed method was applied for the determination of nine elements in two sintering dedusting ash samples.The relative standard deviations(RSD,n=6)of determination results were all less than 5.0%.The contents of potassium,sodium,calcium,magnesium,aluminum,zinc,lead,copper and phosphorus in one sintering dedusting ash sample were determined according to the experimental method and by other chemical methods.The found results were basically consistent.