高级检索

    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

    • 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。

       

      Abstract: 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.

       

    /

    返回文章
    返回