Methacrylate-based monolithic column was prepared in fused-silica capillary (80 ′ 0.32 mm i.d.) by in situ polymerizetion reaction using glycidyl methacrylate as monomer;ethylene dimethacrylate as crosslinker;1-propa...Methacrylate-based monolithic column was prepared in fused-silica capillary (80 ′ 0.32 mm i.d.) by in situ polymerizetion reaction using glycidyl methacrylate as monomer;ethylene dimethacrylate as crosslinker;1-propanol, 1,4-butanediol, and water as porogenic solvents. The monolith matrix was modified with trimethylamine to create strong anion exchanger via ring opening reaction of epoxy groups. The morphology of the monolithic column was studied by using Scanning Electron Microscope (SEM). This column had good mechanical stability and permeability. The effects of various mobile phases for separation of inorganic anions were investigated. Iodate, bromate, nitrite, bromide, and nitrate were separated within 11 min using100 mMpotassium chloride as mobile phase and detected at 210 nm. This method showed good precision of retention time, acceptable linearity and good sensitivity. Under the optimum condition, the RSD of the retention time was in the range of 1.09%-1.75% (n = 6). The calibration curve showed linear relationships between the peak area and the concentration. The limits of detection (LOD) and the limits of quantitation (LOQ) were between 0.08-0.18 mM and 0.26-0.61 mM, respectively. This method was applied to the determination of inorganic anions in tap water and ground water samples.展开更多
目的:建立一种同时检测天然矿泉水中4种无机阴离子含量的方法。方法:待测样品经0.45μm水系过滤膜过滤后,采用Metrosep A Supp 5 Guard/4.0保护柱以及Metrosep A Supp 5阴离子分离柱分离,8 mmol·L^(-1)碳酸氢钠水溶液作为淋洗液进...目的:建立一种同时检测天然矿泉水中4种无机阴离子含量的方法。方法:待测样品经0.45μm水系过滤膜过滤后,采用Metrosep A Supp 5 Guard/4.0保护柱以及Metrosep A Supp 5阴离子分离柱分离,8 mmol·L^(-1)碳酸氢钠水溶液作为淋洗液进行等度淋洗,流速为1.0 mL·min^(-1),电导检测器进行检测。结果:4种无机阴离子在一定浓度范围内线性关系较好,相关系数均在0.9960以上,检出限在0.0001~0.0100 mg·L^(-1),定量限在0.0004~0.0400 mg·L^(-1);相对标准偏差在0.59%~8.16%,加标回收率在80.00%~112.50%。结论:该方法具有灵敏度高、分离度好、准确度强等优势,适用于天然矿泉水中F^(-)、Cl^(-)、NO_(3)^(-)和SO_(4)^(2-)的快速定量检测。展开更多
文摘Methacrylate-based monolithic column was prepared in fused-silica capillary (80 ′ 0.32 mm i.d.) by in situ polymerizetion reaction using glycidyl methacrylate as monomer;ethylene dimethacrylate as crosslinker;1-propanol, 1,4-butanediol, and water as porogenic solvents. The monolith matrix was modified with trimethylamine to create strong anion exchanger via ring opening reaction of epoxy groups. The morphology of the monolithic column was studied by using Scanning Electron Microscope (SEM). This column had good mechanical stability and permeability. The effects of various mobile phases for separation of inorganic anions were investigated. Iodate, bromate, nitrite, bromide, and nitrate were separated within 11 min using100 mMpotassium chloride as mobile phase and detected at 210 nm. This method showed good precision of retention time, acceptable linearity and good sensitivity. Under the optimum condition, the RSD of the retention time was in the range of 1.09%-1.75% (n = 6). The calibration curve showed linear relationships between the peak area and the concentration. The limits of detection (LOD) and the limits of quantitation (LOQ) were between 0.08-0.18 mM and 0.26-0.61 mM, respectively. This method was applied to the determination of inorganic anions in tap water and ground water samples.