单斜相纺锤形纳米ZrO_2富集分离电感耦合等离子体质谱法测定痕量Ni(Ⅱ)  

Determination of Trace Nickel(Ⅱ) by Inductively Coupled Plasma Mass Spectrometry after Pre-concentration/ Separation with Monoclinic Fusiform Nanometer-Size Zirconium Dioxide

作　　者：杜英秋[1,2] 尹贻东[1] 范乃英[1] 陈鹏刚[1] 张晓波[2] 金海涛[2] 单宏[2] 屈秋瑶[1] 孙智博[1] 陈月鑫[1] 

机构地区：[1]黑龙江大学化学化工与材料学院,哈尔滨150080 [2]农业部谷物及制品质量监督检验测试中心,哈尔滨150086

出　　处：《分析化学》2012年第12期1890-1896,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.20871043)资助

摘　　要：采用水热法合成单斜相纺锤形纳米二氧化锆(ZrO2),建立以单斜相纺锤形纳米ZrO2为吸附剂电感耦合等离子体质谱(ICP-MS)测定痕量Ni2+的方法。本方法对Ni2+的检出限为0.029μg/L,相对标准偏差为2.7%(n=6);结果表明,在pH 9.0、吸附10 min时,纳米ZrO2对Ni2+的吸附率可达99%以上;以2 mL 0.5mol/L HCl为洗脱剂洗脱30 min,可定量洗脱纳米ZrO2上吸附的Ni2+,洗脱率达98%以上;纳米ZrO2对Ni2+的静态吸附容量为198μg/g、富集倍数可达250倍;考察了共存离子的影响以及其再生性能。将本方法应用于实际水样中痕量镍的测定,方法回收率为96.3%～101.4%。Monoclinic fusiform zirconium dioxide（ZrO2） nanoparticles were synthesized by hydrothermal method,a method for the determination of Nickel2＋ was developed by inductively coupled plasma mass spectrometry（ICP-MS） with monoclinic fusiform nanometer-sized ZrO2 as absorbent.The detection limit to Ni2＋ was 0.029 μg/L and the relative standard deviation was 2.7%（n=6）.Optimal adsorption and elution conditions of nanometer-sized ZrO2 to Ni2＋ were studied,adsorption percentage of nanometer-sized ZrO2 to Ni2＋ was more than 99% under pH 9.0 and 10 min,2 mL 0.5 mol/L HCl was sufficient for elution to Ni2＋ more than 98%.The static adsorption capacity of ZrO2 to Ni2＋ was 198.4 μg/g and enrichment factor reached 250.Effects of co-existing ions and regeneration properties were discussed.The method has been applied to the determination of trace Ni2＋ in real water samples,the recoveries were 96.3%-101.4%.

关 键 词：纳米二氧化锆 富集 分离 电感耦合等离子体质谱(ICP-MS) 镍 

分 类 号：O614.813[理学—无机化学] O657.63[理学—化学]