提出了超级微波消解-电感耦合等离子体原子发射光谱法(ICP-AES)同时测定特种工程塑料如芳香聚砜(PSF)、聚醚醚酮(PEEK)、聚苯硫醚(PPS)中铝、砷、钙、镉、汞、钡、钴、铬、铜、铁、钾、镁、锰、钠、镍、磷、铅、硅、锡、硒、锑、钛、钒、锌等24种元素含量的方法。取0.100 g样品,依次加入5.0 mL硝酸、0.5 mL高氯酸和1.0 mL氢氟酸,使用超级微波消解仪,预加压力4 MPa,按温度程序(最终温度280 ℃,保持50 min)消解样品,冷却后取出消解液,用水定容至50 mL,采用ICP-AES测定其中24种元素的含量。结果表明:24种元素的质量浓度均在0.020~1.000 mg·L^-1内与其对应的信号强度呈线性关系,检出限(3s)为0.130~5.92 mg·kg^-1。按照标准加入法进行回收试验,回收率为90.7%~110%,测定值的相对标准偏差(n=6)均小于4.0%。

A method for simultaneous determination of 24 elements (Al, As, Ca, Cd, Hg, Ba, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, Pb, Si, Sn, Se, Sb, Ti, V, Zn) in special engineering plastics, such as aromatic polysulfone (PSF), polyether ether ketone (PEEK) and polyphenylene sulfide (PPS) by inductively coupled plasma atomic emission spectrometry (ICP-AES) with super microwave digestion was proposed. The sample (0.100 g) was taken,and 5.0 mL of nitric acid, 0.5 mL of perchloric acid and 1.0 mL of hydrofluoric acid were added. The above mixture was digested in a super microwave digestion instrument with pre-added pressure of 4 MPa on the temperature program (keeping for 50 min at 280 ℃ of final temperature). After cooling, the digestion solution was taken out, and made its volume up to 50 mL with water, in which 24 elements were determined by ICP-AES. As shown by the results, linear relationships between values of the corresponding signal intensity and mass concentration of the 24 elements were found in the range of 0.020-1.000 mg·L^-1, with detection limits (3s) in the range of 0.130-5.92 mg·kg^-1. Test for recovery was made by the standard addition method, giving results in the range of 90.7%-110%, with RSDs (n=6) of the determined values less than 4.0%.