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Determination of Total Nonylphenol Polyethoxylates in Wastewater by Reversed Phase High Performance Liquid Chromatography

机译:反相高效液相色谱法测定废水中总壬基酚聚乙氧基化物

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A new method based on SPE-RPLC-FLD was established for the quantitative determination of total NPnEO in wastewater. The sample was pretreated using SPE column of Oasis(R)HLB in Waters Corporation. The column was eluted by 6mL of 90% dichloromethane in methanol(v/v), and the eluting liquid was volatilized to 1ml capacity under breezing nitrogen gas current. The recovery of the process is 99.68%. NPnEO in the sample were separated by the Agilent 1100 LC instrument with ZORBAX Eclipse XDB C-18 liquid chromatography column and with the mobile phase of methanol and water at the flow rate of 1.0mL per min. Gradient elution, the proportion of methanol in water is increased from 70% to 100% gradually at 2.5 % per min, was applied to the process. The oven temperature is set at 23℃, and injection volume is 15μL. The component signals were detected by FLD with 313nm excitation wavelength and 230nm emission wavelength. External standard calibration method was chosen as quantitative analysis. Above 90% recovery of NPnEO was checked up by analyzing real sewage and additional sample using the method, and RSD was below 10%. The LOD of the method for NPnEO was from 0.097 to 0.190 microgrammes per liter. NPnEO concentration of some samples, including raw sewage, effluent of biotreatment system and reclaimed water, was analyzed by this method. The results show that the accuracy and precision of the method were satisfactory.
机译:建立了一种基于SPE-RPLC-FLD的新方法定量测定废水中总NPnEO的方法。使用Waters Corporation中的Oasis HLB的SPE柱对样品进行预处理。用6mL的90%二氯甲烷的甲醇溶液(v / v)洗脱柱,并在微风氮气流下将洗脱液挥发至1ml容量。该过程的回收率为99.68%。样品中的NPnEO通过配备ZORBAX Eclipse XDB C-18液相色谱柱的Agilent 1100 LC仪器以及流速为1.0mL / min的甲醇和水的流动相进行分离。梯度洗脱,将甲醇在水中的比例以每分钟2.5%的速度从70%逐渐增加到100%,应用于该过程。柱箱温度设置为23℃,进样量为15μL。组分信号通过FLD检测,激发波长为313nm,发射波长为230nm。选择外标法进行定量分析。通过使用该方法分析实际污水和其他样品,检查了NPnEO的回收率是否高于90%,RSD低于10%。 NPnEO方法的检测限为每升0.097至0.190微克。用该方法分析了一些样品的NPnEO浓度,包括原污水,生物处理系统的废水和再生水。结果表明,该方法的准确性和准确性令人满意。

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