Determination of Cr， Mn， Si and P in high chromium alloy cast iron by microwave digestion-inductively coupled plasma optical emission spectrometry
BAI Huanhuan, LI Jian, LUO Ce, LIU Ting
BaoTi Group Co., Ltd., Baoji 721014, China
摘要：建立微波消解-电感耦合等离子体发射光谱法测定高铬合金铸铁中的铬、锰、硅、磷4种元素的分析方法。以盐酸-硝酸-氟酸(体积比为6∶2∶1)混合酸为溶剂，采用程序升温微波消解法分解样品。电感耦合等离子体发射光谱仪工作条件：激发功率为1 300 W，等离子气流量为12 L/min，雾化气流量为0.7 L/min，辅助气流量为1.0 L/min。标准曲线外标法定量。铬、锰、硅、磷的质量浓度分别在150～200、0.02～10.0、0.05～10.0、0.07～0.5 mg/L范围内与光谱强度具有良好的线性关系，相关系数均不小于0.999 7。锰、硅、磷元素的检出限分别为0.002%、0.005%、0.007%。样品加标回收率为97.7%～104.5%，测定结果的相对标准偏差均为0.29%～1.31%(n=7)。该方法快速、准确，满足高铬合金铸铁中铬、锰、硅、磷的检测要求。
Abstract：A method for the determination of Cr, Mn, Si and P in high chromium alloy cast iron by microwave digestion-inductively coupled plasma optical emission spectrometry was established. The sample was decomposed by temperature programmed microwave digestion with HCl-HNO-HF(volume ratio was 6∶2∶1) as solvent. Working 3 conditions of inductively coupled plasma emission spectrometer: The excitation power was 1 300 W, the plasma gas flow was 12 L/min, the atomization gas flow was 0.7 L/min, and the auxiliary air flow was 1.0 L/min. The external standard method of standard curve was used for quantitative analysis. The mass concentrations of Cr, Mn, Si and P had a good linear relationship with spectral intensity in the range of 150-200, 0.02-10.0, 0.05-10.0 and 0.07-0.5 mg/L, respectively, and the correlation coef ficients were all not less than 0.999 7. The detection limits of Mn, Si and P were 0.002%, 0.005% and 0.007%, respectively. The recoveries of spiked samples were 97.7%-104.5%, and the relative standard deviations of the determination results were 0.29%-1.31%(n=7). The method is rapid and accurate, and it meets the testing requirements of Cr, Mn, Si and P in high chromium alloy cast iron.
Keywords：microwave digestion; ICP-OES; high chromium alloy cast iron
BAI Huanhuan，LI Jian，LUO Ce，et al. Determination of Cr，Mn，Si and P in high chromium alloy cast iron by microwave digestion-inductively coupled plasma optical emission spectrometry[J]. Chemical Analysis and Meterage，2022，31(7)：43.