高效液相色谱法同时测定化工废水中乙醇酸、乙醛酸和草酸的含量
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摘要
水样经0.22μm亲水针筒式过滤器过滤,根据需要进行稀释后,在Acclaim MixedMode WAX-1色谱柱(4.6mm×150mm,5μm)上进行分离,以90mmol·L~(-1)磷酸盐缓冲溶液[pH 6.0,溶剂为10%(体积分数)乙腈溶液]为流动相进行等度洗脱,在波长210nm处进行紫外检测。结果表明:乙醇酸、乙醛酸和草酸的质量浓度分别在3.51～2 500,4.20～8 000,18.0～800mg·L~(-1)内与对应的峰面积呈现线性关系,检出限(3S/N)分别为1.00,1.24,4.82mg·L~(-1),测定下限(10S/N)分别为3.32,4.15,16.1mg·L~(-1)。对实际样品进行加标回收试验,乙醇酸、乙醛酸和草酸的回收率分别在98.2%～101%,99.6%～103%,99.2%～101%之间,测定值的相对标准偏差(n=6)分别为0.77%,0.65%,1.1%。
The water sample was filtered through a 0.22μm hydrophilic syringe filter,diluted as needed,and separated on an Acclaim Mixed-Mode WAX-1 column(4.6 mm×150 mm,5μm),with 90 mmol·L~(-1) phosphate buffer solution[pH 6.0,10%(volume fraction) acetonitrile solution as solvent]as mobile phase for elution.UV detection was performed at the wavelength of 210 nm.The results showed that linear relationships were obtained between peak area and mass concentration of glycolic acid,glyoxylic acid and oxalic acid in the ranges of 3.51-2 500,4.20-8 000 and 18.0-800 mg·L~(-1),respectively.The detection limits(3 S/N) were 1.00,1.24,4.82 mg·L~(-1),and the lower limits of determination(10 S/N) were 3.32,4.15,16.1 mg·L~(-1).Tests for recovery was made by standrard addition method to the actual samples,giving values of recovery of glycolic acid,glyoxylic acid and oxalic acid between 98.2%-101%,99.6%-103%and 99.2%-101%,respectively.The relative standard deviation of the measured values(n=6) were 0.77%,0.65% and 1.1%,respectively.
The water sample was filtered through a 0.22μm hydrophilic syringe filter,diluted as needed,and separated on an Acclaim Mixed-Mode WAX-1 column(4.6 mm×150 mm,5μm),with 90 mmol·L~(-1) phosphate buffer solution[pH 6.0,10%(volume fraction) acetonitrile solution as solvent]as mobile phase for elution.UV detection was performed at the wavelength of 210 nm.The results showed that linear relationships were obtained between peak area and mass concentration of glycolic acid,glyoxylic acid and oxalic acid in the ranges of 3.51-2 500,4.20-8 000 and 18.0-800 mg·L~(-1),respectively.The detection limits(3 S/N) were 1.00,1.24,4.82 mg·L~(-1),and the lower limits of determination(10 S/N) were 3.32,4.15,16.1 mg·L~(-1).Tests for recovery was made by standrard addition method to the actual samples,giving values of recovery of glycolic acid,glyoxylic acid and oxalic acid between 98.2%-101%,99.6%-103%and 99.2%-101%,respectively.The relative standard deviation of the measured values(n=6) were 0.77%,0.65% and 1.1%,respectively.
引文
[1] 李涛.乙醛酸的生产及市场应用[J].乙醛醋酸化工,2008(8):9-14.
[2] 刘士松.电解法由草酸制备乙醛酸的研究[J].煤炭与化工,2006,29(12):32-33.
[3] 田玫,张恒彬,曹学静,等.草酸电还原制取乙醛酸的研究[J].分子科学学报,2002,18(1):19-24.
[4] 潘沅.草酸电化学还原生产乙醛酸的进展[J].辽宁化工,1999(2):84-86.
[5] 王爱菊,张新胜,徐苹,等.微分脉冲极谱法测定草酸[J].理化检验-化学分册,2009,45(6):738-739.
[6] 宋振华.高锰酸钾滴定法测定乙醛酸的含量[J].化工技术与开发,1999(4):50-51.
[7] 杜治平,喻幼卿,任慧,等.电位滴定用于乙醛酸的分析[J].化学世界,2002,43(4):181-184.
[8] 马祯,张新胜,李云飞,等.乙醛酸的微分脉冲极谱法定量分析[J].分析试验室,2007,26(2):30-32.
[9] 王玉萍,彭盘英,周耀明.紫外吸光光度法同时测定乙醛酸和乙二醛[J].理化检验-化学分册,2005,41(3):199-202.
[10] 关瑾,王慧泽,任丽艳,等.乙醛酸和草酸的毛细管区带电泳分析[J].色谱,2012,30(1):107-110.
[11] 王存进,杜晓磊.离子色谱法测定乙醛酸中的顺丁烯二酸和乙二酸[J].化学分析计量,2013,22(2):94-96.
[12] 杨秀平,张凤云,翟梅枝,等.气相色谱法测定乙醛酸含量[J].应用化工,2003,32(5):52-53.
[13] 刘树彬,陆敏,张星辰,等.乙醛酸和草酸的高效液相色谱分析[J].应用化工,2007,36(10):1027-1029.
[14] 卢立泓,陶建伟,陆庆宁,等.反相高效液相色谱测定在乙醇酸和草酸存在下的乙醛酸含量[J].理化检验-化学分册,2006,42(8):644-645.
[15] 林灵超.HPLC法测定乙醛酸水溶液中的草酸[J].应用化工,2013,42(4):756-757.
[2] 刘士松.电解法由草酸制备乙醛酸的研究[J].煤炭与化工,2006,29(12):32-33.
[3] 田玫,张恒彬,曹学静,等.草酸电还原制取乙醛酸的研究[J].分子科学学报,2002,18(1):19-24.
[4] 潘沅.草酸电化学还原生产乙醛酸的进展[J].辽宁化工,1999(2):84-86.
[5] 王爱菊,张新胜,徐苹,等.微分脉冲极谱法测定草酸[J].理化检验-化学分册,2009,45(6):738-739.
[6] 宋振华.高锰酸钾滴定法测定乙醛酸的含量[J].化工技术与开发,1999(4):50-51.
[7] 杜治平,喻幼卿,任慧,等.电位滴定用于乙醛酸的分析[J].化学世界,2002,43(4):181-184.
[8] 马祯,张新胜,李云飞,等.乙醛酸的微分脉冲极谱法定量分析[J].分析试验室,2007,26(2):30-32.
[9] 王玉萍,彭盘英,周耀明.紫外吸光光度法同时测定乙醛酸和乙二醛[J].理化检验-化学分册,2005,41(3):199-202.
[10] 关瑾,王慧泽,任丽艳,等.乙醛酸和草酸的毛细管区带电泳分析[J].色谱,2012,30(1):107-110.
[11] 王存进,杜晓磊.离子色谱法测定乙醛酸中的顺丁烯二酸和乙二酸[J].化学分析计量,2013,22(2):94-96.
[12] 杨秀平,张凤云,翟梅枝,等.气相色谱法测定乙醛酸含量[J].应用化工,2003,32(5):52-53.
[13] 刘树彬,陆敏,张星辰,等.乙醛酸和草酸的高效液相色谱分析[J].应用化工,2007,36(10):1027-1029.
[14] 卢立泓,陶建伟,陆庆宁,等.反相高效液相色谱测定在乙醇酸和草酸存在下的乙醛酸含量[J].理化检验-化学分册,2006,42(8):644-645.
[15] 林灵超.HPLC法测定乙醛酸水溶液中的草酸[J].应用化工,2013,42(4):756-757.