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    高效液相色谱法快速测定沥青基耐根穿刺防水卷材中聚合物类阻根剂的含量

    Rapid Determination of Polymeric Root Retardants in Asphalt-Based Waterproof Sheets of Resistance to Root Penetration by HPLC

    • 摘要: 针对采用团体标准T/CBMF 49-2019&T/CWA 301-2019测定沥青基耐根穿刺防水卷材中聚合物类阻根剂含量分析时间长(约12 h)、检出率低等问题,提出了题示方法。取1 g样品,加入25 mL甲基叔丁基醚,在室温下超声溶解30 min后加入25 mL乙醇,超声萃取15 min,用0.45 μm疏水聚四氟乙烯(PTFE)滤头过滤,用高效液相色谱法(HPLC)测定滤液中游离4-氯-2-甲基苯氧基丙酸(MCPP酸)质量分数(w)。另取1 g样品,加入甲基叔丁基醚25 mL,在室温下超声溶解30 min,加入含0.1 mol·L-1氢氧化钠的乙醇溶液25 mL,继续超声15 min,取出后于40℃水浴中皂化水解1 h,用0.45 μm疏水PTFE滤头过滤,用HPLC测定滤液中总MCPP酸质量分数(w)。在HPLC分析时,流动相采用0.5%(体积分数)磷酸溶液-乙腈体系,以(w-w)/0.6计算聚合物类阻根剂的含量。结果表明:方法的分析时间可缩短至约3 h,MCPP酸标准曲线的线性范围为5~100 mg·L-1,检出限(3S/N)为0.03‰。方法用于来自不同厂家的不同类型样品的分析,测定值和产品标签值基本一致,测定值的相对标准偏差(n=6)均小于2.0%,加标回收率为95.1%~108%。

       

      Abstract: To solve the problems of long analysis time (about 12 h) and low detection rate when determining polymeric root retardants in asphalt-based waterproof sheets of resistance to root penetration with the group standard T/CBMF 49-2019&T/CWA 301-2019, the method as mentioned by the article was proposed. The sample of 1 g was mixed with methyl tert-butyl ether of 25 mL, and dissolved by ultrasound for 30 min at room temperature. Ethanol of 25 mL was added to the above solution for extraction by ultrasound for 15 min, the mixed solution was filtered with 0.45 μm hydrophobic PTFE filter, and mass fraction of free MCPP acid (wfree) in the filtrate was determined by HPLC. Another sample of 1 g was taken and dissolved with methyl tert-butyl ether by ultrasound for 30 min at room temperature, and 25 mL of ethanol solution containing 0.1 mol·L-1 NaOH was added to the above solution for extraction by ultrasound for 15 min. The solution obtained was taken out, saponified and hydrolyzed in water bath at 40 ℃ for 1 h. After filtering with 0.45 μm hydrophobic PTFE filter, mass fraction of total MCPP acid (wtotal) in the filtrate was determined by HPLC. In HPLC analysis, the system composed of 0.5% (φ) phosphoric acid solution and acetonitrile was used as the mobile phase, and the content of polymeric root retardant was calculated by (wtotal-wfree)/0.6. As found by results, the analysis time of the method could be shortened to about 3 h, and linear range of standard curve of MCPP acid was found in the range of 5-100 mg·L-1, with detection limit (3S/N) of 0.03‰. The proposed method was applied to the analysis of different types of samples from different manufacturers. The determined values were basically the same as the labeling values, and RSDs (n=6) of the determined values were less than 2.0%, with results of test for the spiked recovery in the range of 95.1%-108%.

       

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