反相高效液相色谱法测定聚羧酸类减水剂合成原料
RPHPLC Determination of Raw Materials of Synthetic Polycarboxylic Water Reducing Agent
摘 要
提出了反相高效液相色谱法同时测定聚羧酸类减水剂“大单体”原料中甲基丙烯酸(MA)、聚乙二醇单甲醚(MPEG)和聚乙二醇单甲醚甲基丙烯酸酯(MPEG-MA)的含量。以ZORBAX 300SB-C18柱为分离柱,以不同体积比的甲醇和0.1%三氟乙酸(体积比,pH 2.0)的混合溶液为流动相进行梯度洗脱,用紫外检测器于波长218 nm检测MA,在蒸发光检测器载气流量和漂移管温度分别为1.2 L·min-1和80 ℃时检测MPEG和MPEG-MA。结果表明:样品中3个大单体原料的残留量存在较大差异。
甲基丙烯酸
聚乙二醇单甲醚
聚乙二醇单甲醚甲基丙烯酸酯
聚羧酸类减水剂
RPHPLC
MA
MPEG
MPEG-MA
Polycarboxylic water reducing agent
Abstract
A method of RPHPLC was proposed for the simultaneous determination of “macromonomers”, raw materials of synthetic polycarboxylic water reducing agent, including methacrylic acid (MA), poly (ethylene glycol) monomethyl ether (MPEG) and methoxy (polyethyleneglycol) methacrylate (MPEG-MA). ZORBAS 300SB-C18 column was used as stationary phase for separation, and mixtures of methanol and (φ) 0.1% trifluoroacetic acid of pH 2.0 in different ratios were used as mobile phase in the gradient elution. The content of MA was determined by UV-detection at the wavelength of 218 nm; and the contents of MPEG and MPEG-MA were determined by evaporation light detector with the temperature of drift tube at 80 ℃ and flow rate of carrier gas at 1.2 L·min-1, respectively. It was found that the residual amounts of 3 macromonomers were quite different.
中图分类号 O652.63
所属栏目 工作简报
基金项目 陕西省科技厅基金项目(SJ08E.08)
收稿日期 2011/10/14
修改稿日期
网络出版日期
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备注孟祖超(1978-),男,陕西兴平人,讲师,博士研究生,主要从事油田化学品的分析及应用研究。
引用该论文: MENG Zu-chao,FU Jun-fang,LIU Xiang,ZHANG Hao. RPHPLC Determination of Raw Materials of Synthetic Polycarboxylic Water Reducing Agent[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(7): 773～776
孟祖超,符军放,刘祥,张浩. 反相高效液相色谱法测定聚羧酸类减水剂合成原料[J]. 理化检验－化学分册, 2012, 48(7): 773～776
被引情况:
【1】谢丽娜,姚晨之,严方, "聚羧酸系减水剂的大单体组分的分离分析",理化检验－化学分册 52, 284-287(2016)
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参考文献
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【9】ANDERSEN T, MOLANDER P, TRONES R, et al. Separation of polyethylene glycol oligomers using inverse temperature programming in packed capillary liquid chromatography［J］. J Chromatogr A, 2001,918:221-226.
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【2】刘丽霞,杨长辉,吴芳,等.掺聚羧酸减水剂的高强混凝土塑性收缩与抗裂性能研究［J］.混凝土, 2009(10):80-82.
【3】PLANK J, SACHSENHAUSER B. Impact of molecular structure on zeta potential and adsorbed conformation of α-allyl-ω-methoxypolyethylene glycol-maleic anhydride superplasticizers［J］. J Adv Concr Technol, 2006,4(2):233-239.
【4】SHIN J Y, HONG J S, SUH J K, et al. Effects of polycarboxylate-type superplasticizer on fluidity and hydration behavior of cement paste［J］. Korean J Chem Eng, 2008,25(6):1553-1561.
【5】孙振平,赵磊.聚羧酸系减水剂的合成研究［J］.建筑材料学报, 2009,12(2):127-131.
【6】RISSLER K. Improved separation of polyethylene glycols widely differing in molecular weight range by reversed-phase high performance liquid chromatography and evaporative light scattering detection［J］. Chromatographia, 1999,49:615-620.
【7】BARMAN B N, CHAMPION D H, SJOBERG S L. Identification and quantification of polyethylene glycol types in polyethylene glycol methyl ether and polyethylene glycol vinyl ether［J］. J Chromatogr A, 2009,1216:6816-6823.
【8】符军放,刘克清,丁玉.高效液相色谱法测定聚合物水处理剂中残留的单体［J］.色谱, 2008,26(6):772-774.
【9】ANDERSEN T, MOLANDER P, TRONES R, et al. Separation of polyethylene glycol oligomers using inverse temperature programming in packed capillary liquid chromatography［J］. J Chromatogr A, 2001,918:221-226.
【10】LI X F, FRED M, BART D, et al. Evaporative light scattering detector: toward a general molecular weight cutoff characterization of nanofiltration membranes［J］. Anal Chem, 2009,81:1801-1809.
【11】魏泱,丁明玉.蒸发光散射检测技术［J］.色谱, 2000,18(5):394-401.
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