离子色谱-化学发光法测定环境水样中痕量间苯二酚和间苯三酚  

Determination of Resorcinol and Phloroglucinol in Environmental Water Samples Using Ion Chromatography with Chemiluminescence Detection

作　　者：吴宏伟[1,2] 陈梅兰[3] 寿旦[4] 朱岩[2] 

机构地区：[1]浙江大学西溪校区化学系,杭州310028 [2]新乡医学院基础医学院,新乡453002 [3]浙江树人大学生环学院,杭州310000 [4]浙江省中医药研究院,杭州310007

出　　处：《分析化学》2012年第11期1747-1751,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.J0830413);浙江省自然科学基金(No.Y5100280);浙江省分析测试基金(No.2011C 37034)资助项目

摘　　要：建立了离子色谱分离化学发光法同时检测环境水样中痕量间苯二酚和间苯三酚的方法。利用IonPacAS19阴离子交换分析柱进行分离,以50 mmol/LNaOH作为流动相洗脱待测物质后,再用鲁米诺K_2Fe(CN)_6化学发光体系在碱性介质中对其进行测定。最佳发光条件为:鲁米诺浓度为6.0×10^(-4)mol/L,K_4Fe(CN)-6浓度为0.1 mol/L,K_3Fe(CN)_6浓度为5.5×10^(-5)mol/L。本方法分离时不需使用甲醇、乙腈等有机改进剂,环境友好,同时提高了化学发光的强度。采用本方法测定的间苯二酚和间苯三酚线性范围为0.05～1.0 mg/L,检出限(3σ)分别为4.0和4.3μg/L。对0.1 mg/L的间苯二酚和间苯三酚标准溶液进行11次测定,相对标准偏差(RSD)分别为0.9%和1.1%。将本方法应用于实际水样中痕量间苯二酚和间苯三酚的检测,结果满意。A novel method was established for the simultaneous determination of resorcinol and phloroglucinol in environmental water samples by ion chromatography with chemiluminescence detection.Using 50 mmol NaOH solution as eluent,resorcinol and phloroglucinol can be well separated with IonPac AS19 column and determined based on the chemiluminescence reaction of luminol and potassium ferricyanide in an alkaline medium.The optimal CL conditions were 6.0×10^（-4） mol/L luminol,0.1 mol/L potassium ferrocyanide and 5.5×10^（-5） mol/L potassium ferricyanide. The absence of methanol and acetonitrile in mobile phase made the proposed method more sensitive. Under the optimal conditions,the detection limits（LOD） of resorcinol and phloroglucinol were 4.0μg/L and 4.3μg/L,respectively.The method showed good linearity within the range of 0.05—1.0 mg/L.The relative standard deviations（RSD） for 0.1 mg/L resorcinol and phloroglucinol standard solutions were 0.9%and 1.1%（n=11）.The method has been applied to the determination of resorcinol and phloroglucinol in environmental water samples successfully.

关 键 词：离子色谱 化学发光 环境水样 间苯二酚 间苯三酚 

分 类 号：X832[环境科学与工程—环境工程] O657.75[理学—分析化学]