摘要
聚酯纤维在氢氧化钾-乙醇溶液中解聚,解聚液用水定容后采用在线衍生高效液相色谱法(HPLC)分析苯二甲酸,建立了快速测定聚酯纤维中对苯二甲酸(TPA)与间苯二甲酸(IPA)含量的方法。结果表明:聚酯纤维在65℃氢氧化钾-乙醇溶液中振荡处理35min后完全解聚;在190~360nm检测波长范围内,TPA和IPA的最大吸收波长分别为196、212nm,次吸收波长分别为241、220nm,流动相为乙腈-水(0.1%甲酸,V_(乙腈)∶V_(水)=15∶85)时的保留时间分别为6.038、7.776min;TPA和IPA的检出限分别为0.50、1.58mg/L,加标回收率高,相对标准偏差小。该方法样品前处理简单,分析快捷,结果可靠。
Polyester fibers were depolymerized in potassium hydroxide-ethanol solution,and the depolymerized solution was determined by constant volume with water.The benzene dicarboxylic acid was analyzed by online derivatization high performance liquid chromatography(HPLC),and a rapid method was established for the determination of terephthalic acid(TPA)and isophthalic acid(IPA)content in polyester fibers.The results showed that polyester fibers were completely depolymerized by shaking treatment in potassium hydroxide-ethanol solution at 65℃for 35min;within the detection wavelength range of 190~360nm,TPA and IPA had maximum absorption wavelengths at 196nm and 212nm,respectively,with secondary absorption wavelengths at 241nm and 220nm,respectively.The retention time was 6.038min and 7.776min,respectively when the mobile phase was acetonitrile-water(0.1%formic acid,V_(acetonitrile)∶V_(water)=15∶85);the limit of detection of TPA and IPA were 0.50 mg/L and 1.58mg/L,respectively,and the spiked recoveries were high with the small relative standard deviations.The method exhibits rapid analysis and reliable results with simple pretreatment.
作者
郎巧文
陈海相
李冲
王大伟
冯敏
LANG Qiaowen;CHEN Haixiang;LI Chong;WANG Dawei;FENG Min(National Engineering Lab for Textile Fiber Materials and Processing Technology,Zhejiang Sci-Tech University,Hangzhou 310018,China)
出处
《浙江理工大学学报（自然科学版）》
2024年第6期795-800,共6页
Journal of Zhejiang Sci-Tech University(Natural Sciences)
基金
浙江省文物保护科技项目(2022001)。
关键词
聚酯纤维
对苯二甲酸
间苯二甲酸
在线衍生
高效液相色谱
快速测定
polyester fibers
terephthalic acid
isophthalic acid
online derivatization
high performance liquid chromatography(HPLC)
rapid determination
