不同消解方法对纳米二氧化钛浓度测定的影响  

Effect of different digesting methods on the detection of titanium dioxide nanoparticles concentration

作　　者：刘志远[1] 于水利[1] 刘贵彩[1] 杜欣俊[1] 汪雪格 

机构地区：[1]同济大学污染控制与资源化研究国家重点实验室,上海200092 [2]中国市政工程东北设计研究总院,长春130000

出　　处：《环境化学》2013年第4期666-670,共5页Environmental Chemistry

基　　金：国家自然科学基金资助项目(50978068);国际科技合作项目(中日韩)(2010DFA92460)资助

摘　　要：建立了氢氟酸硝酸微波消解-电感耦合等离子光谱法(ICP-OES)检测水中纳米二氧化钛浓度的分析方法.分析对比了国内外三大类纳米二氧化钛消解方法的回收率,考察了电感耦合等离子光谱仪(ICP-OES)测定钛离子的精密度.实验对比发现,过硫酸铵碱熔法回收率最低,加热板消解法的回收率低于微波消解法.在微波消解法中,以氢氟酸硝酸为消解剂时,回收率最高.因此,氢氟酸硝酸微波消解法最适合消解纳米二氧化钛;在选定条件下,钛的标准曲线在10—1000μg.L-1的范围内线性关系良好(最大误差<5%).RSD小于10%;检出限(MDL)和测定限(RQL)均低于1μg.L-1.加标回收率在119%—122%之间,满足标准的要求.因此,氢氟酸硝酸微波消解法结合ICP-OES,是一种较适合测定纳米二氧化钛浓度的方法.A new method for the determination of titanium dioxide nanoparticles in water by means of microwave digestion method coupled with ICP-OES was established. The recoveries of three principal types of digestion methods were compared and the precision of ICP-OES for concentration detection was also analyzed. The results showed that the method using ammonium persulfate as fusing reagent had the lowest recovery, while the microwave digestion＇s recovery was higher than the open hot-plate digestion method. Herein, the microwave digestion method using hydrofluoric-nitric acid solution as the digestion solution had the highest recovery. So the hydrofluoric-nitric acid microwave digestion method is the suitable method for digesting titanium dioxide nanoparticles; under the optimum conditions, a maximum error （ 〈 5% ） was obtained when the linear range was 10--1000 μg· L^-1. The relative standard deviation （RSD） was less than 10%. Both the method detection limit （MDL） and the determination limits （RQL） were less than 1 μg· L^-1. The labeled recoveries were 119%--122%, meeting the demands of relative digestion method coupled with ICP-OES is a kind dioxide nanoparticles. regulations. Therefore, hydrofluoric-nitric acid microwave of suitable method for detecting the concentration of titanium

关 键 词：电感耦合等离子光谱仪(ICP-OES) 纳米二氧化钛 消解方法 

分 类 号：X832[环境科学与工程—环境工程]