近红外光谱法检测氨纶中残存DMAC溶剂含量

Determination of residual DMAC solvent content in spandex via near-infrared spectroscopy

以丙酮为溶剂,将氨纶中的残存溶剂N,N'-二甲基乙酰胺(DMAC)进行超声萃取,采用近红外光谱技术,结合偏最小二乘法,建立DMAC定量校正模型,测定氨纶中残存DMAC溶剂含量。结果表明:采用交叉验证得到了DMAC质量分数的线性范围为0~1.79%,1.79%~9.44%,模型的相关系数(R^2)分别为0.999 96,0.999 64,校正集的交叉验证均方根误差分别为0.004 11,0.041 34,预测集的均方根误差分别为0.003 95,0.032 30,方法的加标回收率为86.58%~100.87%,相对标准偏差为0.25%~0.95%。

The residual solvent N,N ＇- dimethylacetamide （DMAC）, in spandex was ultrasonic extracted with acetone solvent. A quantitative calibration model was established to deterimine the residual DMAC solvent content by the combination of near-in- frared spectroscopy and partial least squares. The results showed that the linear ranges of the assay were determined as 0 - 1.79% and 1.79% -9.44% in term of DMAC mass fraction, the correlation coefficient （ R2 ）as 0.999 96 and 0.999 64, the root mean square error of calibration set as 0. 004 II and 0.041 34, the root mean square error of prediction set as 0.003 95 and 0.032 30 by outcross validation; and the addition standard recovery of the method was 86.58% - 100.87% and the relative standard deviation was 0.25% -0.95%.