色谱

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高效液相色谱法测定聚合物水处理剂中残留的单体

符军放1,刘克清1,丁玉1,王蕾1,黄瑞娟2,马政生2   

  1. 1.Technology Development Center of Oilfield Chemicals Department, China Oilfield Services Ltd., Yanjiao 065201, China; 2.School of Chemical Engineering, Northwest University, Xi’an 710069, China
  • 收稿日期:2008-05-04 修回日期:2008-08-04 出版日期:2008-11-30 发布日期:1983-06-25
  • 通讯作者: 符军放
  • 基金资助:

Determination of residual monomers in polymer water treatment chemicals using high performance liquid chromatography

FU Junfang1, LIU Keqing1, DING Yu1, WANG Lei1, HUANG Ruijuan2, MA Zhengsheng2   

  1. 1.Technology Development Center of Oilfield Chemicals Department, China Oilfield Services Ltd., Yanjiao 065201, China; 2.School of Chemical Engineering, Northwest University, Xi’an 710069, China
  • Received:2008-05-04 Revised:2008-08-04 Online:2008-11-30 Published:1983-06-25
  • Contact: FU Junfang

摘要: 建立了采用高效液相色谱测定聚环氧琥珀酸钠盐(PESA)、丙烯酸/马来酸酐二元共聚物(AA/MA)、聚丙烯酸盐(PAA)、水解聚马来酸钠盐(HPMA)、马来酸酐/丙烯酸/丙烯酸甲酯三元共聚物(MA/AA/MAc)5类聚合物水处理剂中残留单体的方法。以Agilent ZORBAX 300SB-C18柱(5 μm,150 mm×4.6 mm)为分析柱,柱温为30 ℃,流动相为0.01 mol/L KH2PO4溶液(用5%H3PO4调节pH为2.3)-甲醇(体积比为95∶5)进行等度洗脱,检测波长为210 nm,流速为0.6 mL/min,样品用流动相稀释过滤后直接进样分析,10 min内马来酸、富马酸及丙烯酸残留单体获得分离和定量。上述3种残留单体的检出限分别为0.5,0.5和0.2 mg/L,回收率为98.9%~103.7%,相对标准偏差为1.09%~1.69%,相关系数为0.9996~0.9999。实验结果表明,该法简便快速、灵敏可靠,适用于5类聚合物水处理剂中残留单体的测定。

关键词: 丙烯酸, 残留单体, 富马酸, 高效液相色谱, 聚合物水处理剂 , 马来酸

Abstract: A method was developed for the determination of residual monomers in polymer water treatment chemicals (sodium of polyepoxysuccinic acid (PESA), acrylic acid/maleic anhydride copolymer (AA/MA), polyacrylic acid (PAA), sodium of hydrolyzed polymaleic acid (HPMA), and maleic anhydride/acrylic acid/methyl acrylate copolymer(MA/AA/MAc) using high performance liquid chromatography. The separation was performed on a ZORBAX 300SB-C18 column (5 μm, 150 mm×4.6 mm). The mobile phase was 0.01 mol/L KH2PO4 (pH 2.3, adjusted by 5%H3PO4)-methanol (95∶5, v/v) with a flow rate of 0.6 mL/min. The detection wavelength was set at 210 nm and the column temperature was 30 ℃. The sample was diluted by the mobile phase and filtrated for analysis. The residual monomers of maleic acid, fumaric acid and acrylic acid were completely separated and determined in 10 min, and the limits of detection were 0.5, 0.5, and 0.2 mg/L, respectively. The average recoveries were 98.9%-103.7% with the relative standard deviations of 1.09%-1.69%. The correlation coefficients for the linear equations were 0.9996-0.9999. These results demonstrate that the proposed method is simple, sensitive and reliable for the determination of the residual monomers in five polymer water treatment chemicals.

Key words: acrylic acid, fumaric acid, maleic acid, polymer water treatment chemicals , residual monomers, high performance liquid chromatography (HPLC)