石英砂固体分散剂制样的裂解气相色谱法测定涤/毛纤维混纺比列

Analysis of Polyester /Wool Blended Fibers by Pyrolysis Gas Chromatography Using Quartz Sand as Dispersant for Solid Sample Preparation

基于纵型微型炉裂解器的裂解气相色谱法（Py-GC）建立了涤/毛纤维混纺比例的测定方法。以石英砂为固体质量分散剂,将样品加入其中碾磨成粉末后称量进样,在550℃的裂解温度下得到相应的裂解色谱图,依据各自特征裂解谱图与释放气体分析曲线可识别涤纶与羊毛纤维;选择涤/毛二元混纺纤维裂解谱图上涤纶的特征裂解产物——联苯为定量峰,计算混纺纤维中涤纶的质量百分含量,进而推算出羊毛纤维的含量。样品和石英砂的最佳配比为0.02 g∶4 g,涤纶质量在0.0256~0.2048 mg范围内联苯的线性良好,相关系数R2=0.9952。对不同涤/毛混纺比例的实际样品进行了测定,相对标准偏差RSD〈3%（n=3）;本法与国标法所得结果的偏差小于5%。结果表明,本方法简便、准确,适合涤/毛二元混纺纤维混纺比例的质控分析。

A pyrolysis gas chromatographic （Py-GC） method using a vertical microfurnace pyrolyzer was applied for analysis of polyester and wool fibers as well as polyester/wool blending ratio. The samples dispersed with the quartz sand were milled into a homogeneous powder and then injected by weighing carefully. The pyrograms of the samples were obtained at the pyrolysis temperature of 550℃. Polyester and wool fiber could be identified by their evolved gas analysis （EGA） curves and pyrograms. Diphenyl, one of the characteristic peaks thermally decomposed from polyester, was selected as the peak to quantitatively determine the blending ratio. The optimum ratio of samples and quartz sand was 0.02 g ： 4 g. At the mass range from 0. 0256 to 0. 2048 mg of polyester contained in samples, the achieved calibration curves exhibited good linearity with the correlation coefficient （R2） 0. 9952. Real samples with different polyester/wool blending ratios were measured and the relative standard deviation （RSD） of polyester mass ratio in blended fibers was less then 3%. The deviation of result was less then 5% compared with those obtained by the method of National Standards. The result shows that Py-GC method is simple, fast and accurate, suitable for the analysis of polyesters and wool fibers and their blending ratio. The proposed method can be used for quality control of blend levels in polyester/wool yarns.