A procedure was developed for the determination of residual monomers in polycarboxylate superplasticizer by reversed-phase high performance liquid chromatography. Seven kinds of residual monomers were quantitatively determined on a SinoChrom ODS-BP (C18) column and UV detector at 205 nm. The mobile phases which were used to determine micromolecular monomers were composed of acetonitrile and phosphate buffer solution (0.05 mol L−1, pH = 3) in the ratio of 8:92 (v/v). While the mobile phases for long side-chain monomers testing were composed of acetonitrile and phosphate buffer solution (0.05 mol L−1, pH = 6.5) in the ratio of 40:60 (v/v). The linear response ranged from 4.0 × 10−6–2.0 × 10−3 mol L−1. The detection limit was 0.12 × 10−5–0.8 × 10−5 mol L−1. Determination of real samples showed that relative standard deviation of high conversion rate samples was 3.1–8.7% and standard addition recovery ratio was 91.5–102.8%. While the relative standard deviation of low conversion rate samples was less than or close to 1% and the standard addition recovery ratio was 96.3–103.1%.
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机译:建立了一种通过反相高效液相色谱法测定聚羧酸类高效减水剂中残留单体的方法。在SinoChrom ODS-BP(C18)色谱柱和205 nm紫外检测器上定量测定了7种残留单体。用于测定微分子单体的流动相由乙腈和磷酸盐缓冲溶液(0.05 mol L sup-1,pH = 3)组成,比例为8:92(v / v)。用于长侧链单体测试的流动相由乙腈和磷酸盐缓冲溶液(0.05 mol L -1 sup>,pH = 6.5)组成,比例为40:60(v / v)。线性响应范围为4.0×10 -6 sup> –2.0×10 -3 sup> mol L -1 sup>。检出限为0.12×10 -5 sup> -0.8×10 -5 sup> mol L -1 sup>。实际样品的测定表明,高转化率样品的相对标准偏差为3.1–8.7%,标准添加回收率为91.5–102.8%。低转化率样品的相对标准偏差小于或接近1%,标准加样回收率为96.3-103.1%。
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