ICP-OES法同时测定煅炉甘石中氧化锌及13种金属元素杂质的含量
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篇名: ICP-OES法同时测定煅炉甘石中氧化锌及13种金属元素杂质的含量
TITLE:
摘要: 目的:建立同时测定煅炉甘石中氧化锌及13种金属元素杂质含量的方法。方法:经硝酸、氢氟酸微波消解后,采用电感耦合等离子体发射光谱法测定。发射功率为1 300 W,载气流量为15 L/min,辅助气流量为0.1 L/min,蠕动泵速为0.8 L/min,雾化气流量为0.8 L/min,雾化器压力为315 kPa,以轴向观察方式在不同波长下检测。结果:铝、砷、钡、钙、镉、钴、铬、铜、铁、汞、镁、锰、铅、锌检测质量浓度线性范围为0.001~4.000 μg/mL(r为0.999 2~0.999 8);定量限为0.000 7~0.044 0 μg/mL,检测限为0.000 2~0.013 2 μg/mL;中间精密度、稳定性、重复性试验的RSD均小于4%;加样回收率为86.1%~116.9%(RSD为0.9%~3.6%);耐用性试验的RSD均小于5%。结论:该方法操作简便、准确,精密度、稳定性、重复性、耐用性好,可用于煅炉甘石中氧化锌及13种金属元素杂质含量的同时测定。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of zinc oxide and 13 metallic element impurities in calcined calamine. METHODS: After microwave digestion of nitric acid and hydrofluoric acid, inductively coupled plasma atomic emission spectrometry (ICP-OES) was used to determine the content of various metallic element in calamine with emssive power of 1 300 W, carrier gas current flow of 15 L/min, auxiliary gas current flow 0.1 L/min, peristaltic pump flow of 0.8 L/min, atomizing air current flow of 0.8 L/min, atomizer pressure of 315 kPa and axial observation at different wavelengths. RESULTS: The linear range of Al, As, Ba, Ca, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Pb, Zn in calamine were 0.001-4.000 μg/mL (r were 0.999 2-0.999 8). The quantitation limit ranged 0.000 7-0.044 0 μg/mL, detection limits ranged 0.000 2-0.013 2 μg/mL. RSDs of intermediate precision, stability and repeatability tests were all lower than 4%. The recoveries were 86.1%-116.9% (RSDs were 0.9%-3.6%). RSDs of durability tests were all lower than 5%. CONCLUSIONS: The method is simple, accurate, precise, stable, reproducible and durable, and it is can be used for simultaneous determination of zinc oxide and 13 metallic element impurities in calcined calamine.
期刊: 2018年第29卷第16期
作者: 谢凯,杨洋,薛汝增,徐单单,郑公铭,王如意,李志平
AUTHORS: XIE Kai,YANG Yang,XUE Ruzeng,XU Dandan,ZHENG Gongming,WANG Ruyi,LI Zhiping
关键字: 电感耦合等离子体发射光谱法;煅炉甘石;氧化锌;金属元素杂质
KEYWORDS: Inductively coupled plasma atomic emission spectrometry; Calcined calamine; Zinc oxide; Metallic element impurity
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