针对PAN基碳纤维中金属杂质元素(Ca、Mg、Na、K、Fe)的测定方法进行研究,样品经过灰化处理,用盐酸、硝酸、氢氟酸对灰化后的样品进行溶解,同时采用ICP-OES内标法,以Y作为内标元素,可以校正基体效应干扰、有效控制非光谱干扰对分析结果引起的偏差,提高了测试方法的准确度和精密度。通过考察干扰元素、检出限、精密度及加标回收实验,确定了最佳实验条件,实验发现,Ca、Mg、Na、K和Fe等5种元素的谱线强度与其浓度在1～100mg/L范围内均具有良好的线性关系,方法检出限分别为0.72、0.96、1.44、0.96和1.56mg/kg,精密度分别为0.45%、1.22%、0.53%、0.82%和1.33%,测试PAN基碳纤维的加标回收率分别为97.3%～105%、81.3%～88.3%、99.3%～107.3%、90.2%～101.2%和90.3%～109.3%。结果表明,相同条件下,此方法优于常规的标准曲线法,即外标法。

The determination method of metal impurity elements (Ca,Mg,Na,K,Fe) in PAN based carbon fiber(CF) was studied.After ashing,the ashing sample was dissolved by hydrochloric acid,nitric acid and hydrofluoric acid.At the same time,ICP-OES internal standard method with y as internal standard element can correct matrix effect interference and effectively control the deviation caused by non spectral interference.The accuracy and precision of the test method were improved.The optimum experimental conditions were determined by investigating interference elements,detection limit,precision and standard addition recovery test.The results showed that there was good linear relationship between the spectral line intensity of Ca,Mg,Na,K,Fe and their concentrations in the range of 1～100mg/L.The detection limits of the method were 0.72,0.96,1.44,0.96 and 1.56mg/kg,respectively.The recoveries were 97.3%～105%,81.3%～88.3%,99.3%～107.3%,90.2%～101.2%,90.3%～109.3%,respectively.The results shown that under the same conditions,this method was superior to the conventional standard curve method,namely external standard method.