微波消解电感耦合等离子体质谱法测定云母钛珠光颜料中的砷  

Determination of arsenic in mica titanium pearlescent pigment by ICP-MS with microwave digestion

作　　者：马娜[1] 张灵火 郭心玮 李玉芳 白金峰[1] 陈海杰[1] MA Na;ZHANG Linghuo;GUO Xinwei;LI Yufang;BAI Jinfeng;CHEN Haijie(Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang 065000,China)

机构地区：[1]中国地质科学院地球物理地球化学勘查研究所,河北廊坊065000

出　　处：《化学分析计量》2023年第11期12-15,共4页Chemical Analysis And Meterage

基　　金：国家重点研发计划(2021YFC2903001);中国地质调查局中国地质科学院基本科研业务费项目(AS2020J18)。

摘　　要：采用硝酸+氢氟酸混酸微波密闭消解云母钛珠光颜料样品,以动能歧视-电感耦合等离子体质谱(KEDICP-MS)法测定砷元素的含量。使用氦气作为碰撞气,利用其与干扰分子间的碰撞裂解作用可显著降低测定时的质谱干扰,选择铑作为内标可有效校正非质谱干扰。通过考察不同氦气流量对砷元素灵敏度和背景等效浓度的影响,优化了碰撞气流量,选择氦流量为3.0 mL/min为最佳检测条件,在此条件下砷元素的质量浓度在0~50 ng/mL范围内与其对应的离子强度校正值线性关系良好,相关系数r>0.999,检出限为0.14 ng/mL。样品测定值的相对标准偏差为4.84%(n=6),两水平加标回收试验砷的回收率为98.3%~102.4%。该方法简便、快捷,为企业对云母钛珠光颜料进行质量控制提供了一种可靠的检测方法。An inductively coupled plasma mass spectrometry with kinetic energy discrimination system(KED-ICPMS) method was developed for the determination of arsenic in mica titanium pearlescent pigment samples digested by nitric acid and hydrofluoric acid mixed with microwave.By using helium as the collision gas,its collisional cleavage with the interfering molecules could significantly reduce the mass spectral interferences during the determination,and rhodium as the internal standard could effectively correct the non-mass spectral interferences.The collision gas flow rate was optimized by considering the effects of different He flow rates on As sensitivity and background equivalent concentration(BEC) and the best gas flow rate for He was 3.0 m L/min.The mass concentration of As had a good linear relationship with its corresponding ionic strength correction value.The linearity of the standard curve for As was performed with the correlation coefficient(r)0.999 in the range of 0-50 ng/mL and the detection limit of 0.14 ng/mL.The relative standard deviation of the sample detection results was 4.84%(n=6),and the recoveries of As in two samples with high and low level addition ranged from 98.3% to 102.4%.This method is simple and rapid,which provides a reliable detection method for quality control of mica titanium pearlescent pigments.

关 键 词：微波消解 电感耦合等离子体质谱法 云母钛珠光颜料 砷 

分 类 号：O657.3[理学—分析化学]