FI-KR-FAAS空气混合吸附二次气体分隔洗脱法测定海洋生物样中的痕量铅  

FI-KR-FAAS Twice Gas Isolation Elution Method for the Determination of Trace Lead in Marine Biological Samples

作　　者：王中瑗[1] 张宏康[2] 倪志鑫[1] 刘景钦[1] 陈欣 李胜勇[1] 杨启津 张灿 WANG Zhong-yuan;ZHANG Hong-kang;NI Zhi-xin;LIU Jing-qin;CHEN Xin;LI Sheng-yong;YANG Qi-jin;ZHANG Can(South China Sea Environment Monitoring Center,State Oceanic Administration ,Guangzhou 510300,China;College of Light Industry and Food,Zhongkai University of Agriculture and Engineering,Guangzhou 510225,China)

机构地区：[1]国家海洋局南海环境监测中心,广东广州510300 [2]仲恺农业工程学院轻工食品学院,广东广州510225

出　　处：《光谱学与光谱分析》2018年第11期3578-3582,共5页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金青年基金项目(41406093)资助

摘　　要：建立了流动注射(flow injection,FI)空气混合吸附预富集编结反应器(knotted reactor,KR)二次气体分隔洗脱法与火焰原子吸收光谱法(flame atomic absorption spectrum,FAAS)联用测定海洋生物样中的痕量铅。在预富集步骤,空气、络合剂和铅溶液在线混合,空气的引入,大大提高了铅的螯合物在KR内壁的吸附效果。在洗脱前,通入一段空气流,在洗脱过程中,即在非完全洗脱时,加入一段空气流,两段空气流的引入,大大降低了被分析物在洗脱液中的分散,提高了信号响应值,从而提高了浓集系数(enhancement factor,EF)。将空气混合吸附预富集与二次气体分隔洗脱法联用,使得KR吸附富集效果和洗脱效果达到了更高的水平。和微柱的低寿命、高反压相比,KR反压小,耐酸耐碱,寿命几乎无限长,对蠕动泵的要求很低,不易造成溶液渗漏等问题。在洗脱过程进行到第5秒时输入1s空气流作为间隔,而不是等整个洗脱过程完成以后再输入空气流,此方法的优点是:洗脱完全,而且大大降低了被分析物在洗脱过程中的分散,吸收信号值大大增加。如果单纯地把洗脱时间降到5s,那么洗脱会非常不完全,也就是没有洗脱干净,在管路中还会残存大量的被分析物,残存的被分析物被带入下一个样品分析中,会对整个实验造成很大的误差,所有的实验数据都将不准,失去数据利用价值。所以完全的洗脱是非常必要的,必须保证一定的洗脱时间。由于随着洗脱过程的进行,洗脱下来的被分析物呈逐渐减小的趋势,在以往洗脱方法中,等到整个洗脱过程全部进行完以后,被分析物在洗脱液中的分散已经相当严重了,导致所得到吸收信号值大大减小。在洗脱过程中插入空气流,即在非完全洗脱时插入空气流,降低了被分析物在洗脱过程中的分散,同时保证了洗脱的完全,大大提高了吸收信号峰值。优化了络合剂种类、浓度和酸度,样品In this paper,trace lead in marine biological samples was determined by using flow injection(FI)air mixture adsorption preconcentration and twice gas isolation elution method in knotted reactor(KR)coupled with flame atomic absorption spectrometry(FAAS).Air,complexing reagent and lead solution were mixed on-line during the preconcentration step,and the introduction of air greatly improved the adsorption effects of the lead chelate on the inner walls of KR.By the introduction of air flow before elution and adding part of air flow during elution,through these two parts of the introduction of air flow bubble partition,the dispersion of the lead chelate in KR was greatly reduced,and the peak of the atomic absorption signal was increased,and the enhancement factor(Enhancement factor,EF)was increased.By the combination with the KR of the air mixing sorption preconcentration and twice gas isolation elution method,the KR adsorption effect and elution effect reached a higher level,and compared with high back pressure and short lifetime of the micro column,KR has the characteristics such as acid and alkali resistance,low back pressure and almost unlimited lifetime.What’s more,it has no critical requirement for the peristaltic pump and is not easy to cause leakage of the solution.In the elution process,1 s air flow was used as a spacer at the fifth second,instead of entering the air flow after the entire elution process was completed.The advantage of this method is not only being eluted completely,but also greatly reducing the dispersion of the analyte during the elution process,and the value of the absorption signal is greatly increased.If the elution time is simply put down to 5 s,then the elution will be very incomplete,the tube being not clean,a large number of analytes still remaining in the tube,and the remnants of the analyte were brought into the analysis of the next sample.All the experimental data will be inaccurate,and the value of data utilization will be lost.So complete elution is necessary and must ensure a

关 键 词：流动注射 二次气体分隔 火焰原子吸收 海洋生物样 铅 

分 类 号：O657.3[理学—分析化学]