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%.