整体式吸附萃取搅拌棒在检测环境水样中镉离子含量方面的应用

Determination of Cd Ion in Environmental Water Sample by Sorption Extraction Stir Bar Based on Monolithic Material

通过逐步聚合反应制备了一种新型整体式吸附萃取搅拌棒，将其应用于环境水中镉离子的吸附萃取。考察了介质酸度、搅拌速率、吸咐时间、解吸溶剂和时间等实验条件对吸附量的影响。控制溶液pH为6．0，搅拌棒转速为300r／min，吸附30min，5％HNO，作为解吸液解吸10min，采用等离子体原子发射光谱仪对Cd离子进行检测。该方法在0．1～50mg／L的Cd离子质量浓度范围内呈较好的线性关系，相关系数为0．9972。相对标准偏差和检出限（30-）分别为4．6％和3．8μg·L^-1，加标回收率为97％～104％。表明该方法具有较好的重复性和可靠性。

A novel sorption extraction stir bar（SBSE） based on the polymer monolithic material was prepared by in-situ stepwise polymerization of epoxy resin（EP） and diethlenetriamine（DETA） using polyethylene glycol （PEG-1540） as porogen. The SBSE was used for the adsorption and extraction for Cd ion in environmental water sample. The experimental conditions such as pH value, stir rate, extraction time, desorption solution and time were optimized. The SBSE operation was performed at a stirring rate of 300 r/min at pH 6.0 for 30 min, and the desorption was done in 5% HNO3 for 10 min. The concentration of Cd ion was detected by ICP - AES method. The result indicated that the calibration curve showed a good linear relationship in the Cd concentration range of 0. 1 -50 mg/L with a correlation coefficient of 0. 997 2. The relative standard deviation and detection limit （ 3σ ） were 4. 6% and 3.8 μg · L^-1, respectively, and the recoveries ranged from 97% to 104%. The method could be applied to the determination of Cd ion in environmental water samples with good reproducibility and reliability.