摘要
利用固相萃取-高效液相色谱紫外荧光串联建立了染色废水中苯胺的检测方法。样品经MCX固相萃取小柱提取、净化后,采用Kromasil C18柱（250 mm×4.6 mm,内径5μm）分离,水/乙腈（20/80,体积比）为流动相,紫外检测波长为235 nm,荧光检测波长：λex为225 nm,λem为335 nm,外标法定量。试验结果显示,荧光检测条件下,苯胺在0.001-0.500 mg/L范围内呈良好的线性关系,最低检出限LOD为0.001 mg/L,定量检出限LOQ为0.003 mg/L。紫外检测条件下,苯胺在0.02-5.00 mg/L范围内呈良好的线性关系,最低检出限LOD为0.02 mg/L,定量检出限LOQ为0.06 mg/L,方法回收率在95.6%-101.8%,RSD为2.2%-5.2%,能满足测定要求。
A rapid, simple and accurate method for the determination of aniline in dyeing wastewater by solid-phase extraction （SPE）-high performance liquid chromatography-ultraviolet and fluorescence serial detector is developed. The sample is extracted and purified by MCX solid phase extraction column, seperated by chromatography column of Kromasil C18 column（250 mm × 4.6 ram, i.d. 5 μm）, with water/ acetonitrile （20/80, V/V） as a mobile phase, and then quantitated by UV-fluorescence serial detector per- formed at wavelength of 235 nm（UV）, 225 nm（Aex） and 335 nm（Aom） respectively. At fluorescence detec- tion conditions,the calibration curve of aniline has good linearity within the range of 0.001 - 0.5 mg/L, the limit of detection is 0.001 rag/L, and the limit of quantification is 0.003 mg/L. At UV detection conditions, the calibration curve of aniline is linear within the range of 0.02 - 5.0 mg/L, the limit of detection is 0.02 mg/L, the limit of quantification is 0.06 mg/L, the extraction recoveries are 95.6% - 101.8% and the RSD is 2.2% - 5.2%.
出处
《印染》
北大核心
2014年第22期40-43,共4页
China Dyeing and Finishing
