高效液相色谱法同时检测某水溶性聚合物中三种单体含量  

Simultaneous Determination of Three Residual Monomers in Water-soluble Polymer by HPLC

作　　者：刘华沙 李菁菁 刘思伽 孙强[1] LIU Huasha;LI Jingjing;LIU Sijia;SUN Qiang(COSL Oilfield Chemicals Institute,Tianjin 300459,P R of China)

机构地区：[1]中海油田服务股份有限公司,天津300459

出　　处：《油田化学》2025年第1期154-158,共5页Oilfield Chemistry

基　　金：中海油田服务股份有限公司“油田化学品核心控制指标体系研究”(项目编号YHB22YF004)。

摘　　要：针对水溶性聚合物残余单体的检测方法针对性太强的问题,建立了一种同时测定某水溶性聚合物中三种单体(顺式丁烯二酸、反式丁烯二酸和衣康酸)质量分数的高效液相色谱(HPLC)分析方法。实验条件经优化后确定为:前处理过程为采用乙腈对该水溶性聚合物进行萃取30 min,再以0.1%磷酸水溶液-乙腈(85∶15)进行等度洗脱,使用安捷伦Zorbax Eclipse XDB C18色谱柱(250×4.6 mm,5μm),柱流速为0.8 m L/min,柱温为45℃,检测波长为210 nm。实验发现:该水溶性聚合物中3种残余单体分离度良好(分离度大于3),线性关系良好(R^(2)大于0.999),稳定性良好(RSD小于1%);顺式丁烯二酸、反式丁烯二酸和衣康酸的最小检测限分别为0.32、0.34、0.63 mg/kg;顺式丁烯二酸、反式丁烯二酸和衣康酸的最小限定限分别为1.21、1.26、2.02 mg/kg;3种单体的加标回收率均在98%~101%之间。某钻井液用增黏剂样品中上述3种单体的质量分数的依次为2.261%、0.284%、2.775%。该方法可以准确控制水溶性聚合物的合成过程,实现对其进行精准质量控制。色谱检测时间小于10 min,高效准确,可实现对该水溶性聚合物的质量控制。As for the problem that the detection method of residual monomer of water-soluble polymer was too targeted,a method for simultaneous determination of maleic acid,fumaric acid and itaconic acid in water-soluble polymer used in drilling fluid by HPLC was established.The experimental conditions were obtained as follows:the water-soluble polymer was extracted with acetonitrile for 30 min,and the mobile phase contained 0.1%phosphoric acid and acetonitrile at volume ratio 85∶15.Agilent Zorbax Eclipse XDB C18 column(250×4.6 mm,5μm)was used,and the flow rate of column was 0.8 mL/min,the column temperature was 45℃,and the detection wavelength was 210 nm.Under the above experimental conditions,the detection results had good separation characteristics(the separation degree was greater than 3),good linear relationship(the R^(2)value was greater than 0.999)and good stability(the RSD was less than 1%).The minimum detection limit of maleic acid,fumaric acid and itaconic acid were 0.32,0.34 and 0.63 mg/kg.the quantitation of maleic acid,fumaric acid and itaconic acid were 1.21,1.26 and 2.02 mg/kg.The recoveries of the three residual monomers were 98%—101%.The mass fractions of the three residual monomers in a sample of the viscosifier were 2.261%,0.284%and 2.775%.The time of chromatographic detection was less than 10 min,and it could meet the quality control of the water-soluble polymer.The method could accurately control the synthesis process of water-soluble polymers and achieve accurate quality control.

关 键 词：水溶性聚合物 高效液相色谱法 残余单体 质量分数 定量 

分 类 号：TE254.1[石油与天然气工程—油气井工程]