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 |
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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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