衍生化高效液相色谱法测定烯烃-酸酐共聚物中的酸酐值
Determination of anhydride value in olefin-anhydride copolymers by derivatization high-performance liquid chromatography
This thesis focuses on olefin-anhydride copolymers as the research subject,utilizing 1-dimethylaminonaphthalene-5-sulfonylhydrazide as the derivatizing reagent,and anhydrous DMF as the solvent.A high-performance liquid chromatography method is established to determine the anhydride value in olefin-anhydride copolymers.After the derivatized copolymer samples experience a reflux reaction at 90℃ for 60 minutes,the reaction solution is diluted with methanol to obtain the reacted material.XDB-C18 chromatographic column (5 μm×4.6 mm×250 mm) is employed,methanol and ultrapure water at a ratio of 1∶1 under isocratic elution is served as the mobile phase with a flow rate of 1.0 mL/min,and the detection wavelength is set at 230 nm.The diluted sample solution is measured to record the peak area of 1-dimethylaminonaphthalene-5-sulfonylhydrazide.The remaining amount of 1-dimethylaminonaphthalene-5-sulfonylhydrazide after derivatization reaction is calculated by substituting into the peak area-concentration standard curve,which is then used to calculate reversely the actual content of the anhydride value in the anhydride-containing copolymer.The results show that within the range of 7.0-42.0 mg/L,the standard curve of 1-dimethylaminonaphthalene-5-sulfonylhydrazide exhibits a good linear relationship with a correlation coefficient greater than 0.999.The recovery rates of the derivatized anhydride copolymer samples at three different spiked levels are between 98.41% and 102.36%,with an RSD of 0.42% (n=6).This method is compared with the chemical titration method,and it is found that this method solves the problem encountered by the chemical titration method,where trace amounts of carboxyl functional groups that may have hydrolyzed in the sample cannot be deducted,leading to a measured value higher than actual one.This method is simple,rapid,sensitive,and has good repeatability,suitable for the determination of anhydride values in olefin-anhydride copolymers.
酸酐值 / 衍生化 / 高效液相色谱法 / 1-二甲氨基萘-5-磺酰肼 / 烯烃-酸酐共聚物
anhydride value / derivatization / high performance liquid chromatography / 1-dimethylaminonaphthalene-5- sulfonylhydrazide / olefin-anhydride copolymers
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