超级微波消解-电感耦合等离子体原子发射光谱法测定硼铁中铬、锰、镍、铜、铝、钛元素的含量  

Determination of Chromium,Manganese,Nickel,Copper,Aluminum and Titanium Elements in Ferroboron by Inductively Coupled Plasma Atomic Emission Spectrometry with Super Microwave Digestion

作　　者：付罗岭 孙建民 胡潇 曹俊飞 李鹰 李剑 FU Luoling;SUN Jianmin;HU Xiao;CAO Junfei;LI Ying;LI Jian(Hangzhou Puyu Technology Development Co.,Ltd.,Hangzhou 311300,China)

机构地区：[1]杭州谱育科技发展有限公司,杭州311300

出　　处：《理化检验（化学分册）》2024年第1期73-78,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出了超级微波消解-电感耦合等离子体原子发射光谱法测定硼铁中铬、锰、镍、铜、铝、钛元素含量的方法。以3 mL硝酸、1 mL盐酸、2 mL氢氟酸、1 mL硫酸、1 mL高氯酸为消解酸体系,采用超级微波消解仪对0.1 g硼铁样品进行处理。在升温压力4 MPa条件下,于最高消解温度270℃保持40 min,样品可以完全消解。结果表明:以基质匹配法定量,6种待测元素工作曲线的线性范围均为0.1~2.0 mg·L^(-1),检出限为8.5×10^(-5)%~2.22×10^(-4)%;按照标准加入法对实际样品进行回收试验,回收率为90.0%~110%,测定值的相对标准偏差(n=11)均小于3.0%;方法用于硼铁标准样品分析,测定值与标准值具有较好的一致性。A method for the determination of chromium,manganese,nickel,copper,aluminum and titanium elements in ferroboron by inductively coupled plasma atomic emission spectrometry with super microwave digestion was proposed.The digestion acid system composed of 3 mL of nitric acid,1 mL of hydrochloric acid,2 mL of hydrofluoric acid,1 mL of sulfuric acid and 1 mL perchloric acid was used to treat 0.1 g of ferroboron sample by super microwave digestion instrument,and the sample could be completely digested at the highest digestion temperature of 270℃for holding 40 min under the heating pressure of 4 MPa.It was shown that the linear ranges of the working curves for 6 analytic elements were 0.1-2.0 mg·L^(-1),with detection limits in the range of 8.5×10^(-5)%-2.22×10^(-4)%.Test for recovery was made on the actual sample by standard addition method,giving results in the range of 90.0%-110%,and RSDs(n=11)of the determined values were less than 3.0%.The method was used to analyze the ferroboron standard samples,and the determined values were in good agreement with the standard values.

关 键 词：超级微波消解 电感耦合等离子体原子发射光谱法 硼铁 元素 

分 类 号：O657.31[理学—分析化学]