X荧光分析仪定性结合微波消解-电感耦合等离子体发射光谱法定量测定铝灰中钾、钙、镁、铁  

Qualitative analysis of potassium,calcium,magnesium and iron in aluminum ash by X-ray fluorescence analyzer with microwave digestion and quantitative analysis by inductively coupled plasma atomic emission spectrometry

作　　者：刘飞飞 赵辽辽 袁立勇 高崇鹏 燕亚娥 Liu Feifei;Zhao Liaoliao;Yuan Liyong;Gao Chongpeng;Yan Ya’e(Shaanxi Coal Group Yulin Chemical Co.,Ltd.,Yulin 719000,China)

机构地区：[1]陕煤集团榆林化学有限责任公司,榆林719000

出　　处：《分析仪器》2023年第2期47-51,共5页Analytical Instrumentation

摘　　要：铝灰是铝冶炼行业产生的主要危险废弃物。目前尚没有针对铝灰的微量金属元素进行分析的标准方法。本实验采用压片-X射线荧光分析仪对铝灰样品进行定性及半定量分析,确定测定铝灰所含金属元素的种类。再通过微波消解-电感耦合等离子体发射光谱法对其中的钾、钙、镁、铁元素进行定量分析。实验表明:0.1000g铝灰在3mL硫酸和6mL磷酸的酸体系下,功率800W消解60min达到完全消解,钾、钙、镁、铁元素在0.00、1.00、3.00、5.00、10.00、20.00μg/mL浓度范围内,相关系数大于0.9997;加标回收率在97.20%~101.19%之间;检出限在0.00007%~0.00019%之间,重复性RSD分别为1.64%、2.22%、4.81%、1.89%(n=6)。表明此方法简单且可靠,适用于铝灰中钾、钙、镁、铁微量金属元素的测定。Aluminum ash is the main hazardous waste produced in the aluminum smelting industry.The results show that 0.1000g aluminum ash can be completely digested in the acid system of 3mL sulfuric acid and 6mL phosphoric acid at 800W power for 60 minutes.The concentration of potassium,calcium,magnesium and iron is within the range of 0.00,1.00,3.00,5.00,10.00 and 20.00ug/mL,and the correlation coefficient is greater than 0.9997.The recovery rate is 97.20%—101.19%.The detection limit is 0.0007%—0.0019%,and the repeatability RSD is 1.64%,2.22%,4.81%and 1.89%,respectively(n=6).This method is simple and reliable,and is suitable for the determination of potassium,calcium,magnesium and iron in aluminum ash.

关 键 词：铝灰 X荧光 微波消解 电感耦合等离子体发射光谱法 金属元素 

分 类 号：X833[环境科学与工程—环境工程] O657.31[理学—分析化学]