有机元素分析仪测定聚丙烯腈基预氧化纤维中氧元素

Determination of oxygen elements in polyacrylonitrile based preoxidized fibers by organic element analyzer

建立有机元素分析仪测定聚丙烯腈基预氧化纤维中的氧元素含量的方法。考察了样品舟、裂解温度以及称样量等对氧元素测试结果的影响,优化后的测定条件:样品舟为4 mm×4 mm×11 mm的锡舟,裂解温度为1 150 ℃,称样质量为(3±0.2) mg。氧元素的质量(x)在0.058~0.271 mg范围内与其响应峰面积(y)具有良好的线性关系,线性回归方程为y=269 329x+2 289,相关系数为r=0.999 9。对样品进行五次平行测定结果的相对标准偏差为5.1%~5.2%,加标回收率为95%~106%。该方法具有取样量少、简单快捷等优点,适用于聚丙烯腈基预氧化纤维中氧元素的测定。

A method for the determination of oxygen content in polyacrylonitrile based preoxidized fibers by organic element analyzer was established.The influence of sample boat,pyrolysis temperature and sample weight on the oxygen element test results was investigated.The optimized measurement conditions were as follows:the sample boat was a tin boat with a size of 4 mm ×4 mm ×11 mm,the pyrolysis temperature was 1 150 ℃,and the sample weight was (3±0.2) mg.The mass of oxygen had good linear relationship with the peak area in the range of 0.058–0.271 mg,the linear regression equation was y=269 329x+2 289,and the correlation coefficient was r=0.999 9.The relative standard deviation of the five parallel determinations of the samples were 5.1%–5.2%,and the recovery rates of standard addition were 95%–106%.The method has the advantages of less sampling amount,simplicity and quickness,etc.,and it is suitable for the determination of oxygen element content in polyacrylonitrile–based preoxidized fibers.