摘要
采用环氧树脂基多孔聚合物整体柱为管内萃取介质,与流动注射联用固相微萃取水中钴离子。考察了萃取流速、萃取时间和溶液pH值对萃取效果的影响,采用正交试验优化洗脱溶剂、洗脱时间、洗脱流速为:pH=7的钴离子水溶液,以流速0.3mL/min萃取30min,再用5%HNO3溶液以0.15mL/min流速洗脱20min,采用等离子体原子发射光谱法(ICP-AES)对钴离子进行检测。该方法在0.1~3.0μg/mL质量浓度范围内呈良好的线性关系,相关系数为0.9993,检出限(S/N=3)为0.03μg/mL,变异系数小于5%(n=5)。与直接进样相比,富集倍数为3倍,加标回收率高于85%。
An epoxy resin based polymer monolith was prepared as the extraction medium of in-tube solid-phase microextraction(SPME) and used to extract Co ion in water. The extraction conditions were investigated,including extraction flow rate, extraction time and pH value. An orthogonal test design was used to optimize the eluant solvent, eluant time and flow rate. The extraction was performed at a flow rate of 0.3 mL/min at pH 7 for 30 min,and the eluting was done in 5% HNOa at a flow rate of 0.15 mL/min for 20 min. The concentration of Co ion was detected by ICP-AES method. The result indicated that the calibration curve showed a good linear relationship in Co concentration range of 0.1-3.0ug/mL with a correlation coefficient of 0. 9993. The detection limit (S/N = 3) was 0. 03 ug/mL, and the coefficient of variation was less than 5 %. Compared with direct injection, an enrichment factor was 3, and the recoveries were more than 85 %.
出处
《分析科学学报》
CAS
CSCD
北大核心
2012年第6期795-798,共4页
Journal of Analytical Science
基金
浙江省科技厅公益性技术应用研究(No.2011C37008)
浙江省自然科学基金(No.Y4090258)
宁波市科技局自然科学基金(2010A610191)