注采液中纳米级聚合物微球的检测方法*

Detection Method of Nanoscale Polymer Microspheres in Oilfield Injection and Production Fluids

薛芳芳 马 波 初立国 程 辰 刘保彻 梁晓静

XUE Fangfang MA Bo CHU Liguo CHENG Chen LIU Baoche LIANG Xiaojing

油田注采液中纳米级聚合物微球的检测对纳米级聚合物微球堵水调剖机理研究具有重要意义，但目前关于这方面的报道尚属空白。为了实现油田注采液复杂体系中纳米级聚合物微球含量的快速、高效、准确检测，采用高效液相色谱法，通过选择合适的检测器、色谱柱和流动相条件，实现了油田注采液中纳米级聚合物微球和其它干扰物的先分离后检测，建立了一种简便、快速、准确测定油田注采液中纳米级聚合物微球浓度的方法：选用双羟基亲水色谱柱，250 mg/L NaH2PO4水溶液为流动相，绘制纳米级聚合物微球浓度~纳米级聚合物微球色谱峰面积（保留时间1.1 min处）的标准曲线，将得到的保留时间1.1 min处色谱峰面积带入标准曲线即可得到纳米级聚合物微球的浓度。该检测方法的线性范围是10~ 2000 mg/L，最小检出量为5 mg/L。该方法具有非常好的日内、日间精密度（RSD<5%）和加标回收率（>90%），可用于实际油田注采出液中纳米级聚合物微球的快速、准确检测。图4表1参13

The detection of nanoscale polymer microspheres in oilfield injection-production fluids is of great significance to the study of water shutoff and profile control mechanism of nanoscale polymer microspheres. However，there is still no report on this aspect. In this paper，a convenient，rapid，and accurate method for the determination of polymer microspheres in oil field injection and production fluids was developed by using high performance liquid chromatography with carefully selecting appropriate detectors，chromatographic columns and mobile phase conditions. Using a double hydroxyl hydrophilic column and 250 mg/L NaH2PO4 aqueous solution as mobile phase，the standard curve of concentration of nanoscale polymer microspheres-peak area of nanoscale polymer microspheres chromatography（retention time at 1.1 min）was drawn. The concentration of nanoscale polymer microspheres could be obtained by substituting the peak area of chromatographic peak at the retention time of 1.1 min into the standard curve. The linear range of the established detection method was 10—2000 mg/L，and the minimum detection quantity was 5 mg/L. The method had very good intraday and daytime precision（RSD<5%）and labeled recovery（>90%），which could be used for the rapid and accurate detection of nanoscle polymer microspheres in the injection and production fluids of actual oil fields.

10.19346/j.cnki.1000-4092.2020.01.029