电感耦合等离子体发射光谱法快速测定白云石、石灰石中高含量氧化钙  

Rapid determination of high content of calcium oxide in dolomite,limestone by inductively coupled plasma emission spectrometry

作　　者：赵建峰 侯淘 ZHAO Jianfeng;HOU Tao(Hebi product quality inspection and Testing Center,Hebi 458030,China;Hebi branch of Henan Special Equipment Safety Testing Institute,Hebi 458030,China)

机构地区：[1]鹤壁市产品质量检验检测中心,河南鹤壁458030 [2]河南省特种设备安全检测研究院鹤壁分院,河南鹤壁458030

出　　处：《化学分析计量》2024年第5期24-28,共5页Chemical Analysis And Meterage

基　　金：河南省市场监督管理局科技项目(2021sj38)。

摘　　要：建立电感耦合等离子体发射光谱法测定白云石、石灰石中高含量氧化钙。样品经10 mL盐酸溶液(1∶1)、1.5 mL浓硝酸溶解后,设定测试功率为1 150 W,分析谱线波长为373.6 nm,氩气流量为0.7 L/min,辅助气流量为0.5L/min,氩气压力为0.2 MPa,观测高度为13 mm,泵转速为50 r/min,采用等离子体原子发射光谱法进行测定。钙的质量浓度在0~10.0μg/L范围内与信号强度线性良好,相关系数为0.999 9,方法检出限为3.2μg/L。采用所建方法分别测定白云石和石灰石标准样品,测定结果的相对标准偏差分别为0.28%~0.31%、0.19%~0.25%(n=6),测定平均值与标准值的相对误差分别为0.20%~0.48%、0.18%~0.22%。分别用所建方法与GB/T 3286.1—2012方法测定白云石、石灰石样品,测定结果的相对误差分别为0.26%~0.29%、0.34%~0.48%。该方法满足白云石、石灰石中高含量氧化钙的测定要求。A method for the determination of high content of calcium oxide in dolomite,limestone by inductively coupled plasma emission spectrometry was established.Samples were dissolved in 10 mL hydrochloric acid solution(1∶1)and 1.5 mL concentrated nitric acid,which were detected by inductively coupled plasma emission spectrometry,with the conditions of test power of 1150 W,analytical spectral line wavelength of 373.6 nm,argon flow of 0.7 L/min,auxiliary gas flow of 0.5 L/min,argon pressure of 0.2 MPa,observation height of 13 mm,and pump speed of 50 r/min.The mass concentration of calcium had a linear relationship with the signal strength in the range of 0-10.0μg/L,with the linear correlation coefficient of 0.9999,and the detection limit was 3.2μg/L.The standard samples of dolomite and limestone were determined by this method,and the relative standard deviations of the determination results were 0.28%-0.31%and 0.19%-0.25%(n=6),respectively.The relative errors between the average value and the standard value were 0.20%-0.48%and 0.18%-0.22%,respectively.The dolomite and limestone samples were determined by the established method and GB/T 3286.1-2012 method,the relative errors of the determination results were 0.26%-0.29%and 0.34%-0.48%,respectively.The method can meet the requirement for the determination of high content calcium oxide in dolomite and limestone.

关 键 词：电感耦合等离子体原子发射光谱法 快速测定 白云石 石灰石 高含量氧化钙 

分 类 号：O657.31[理学—分析化学]