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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%。
A monoclinic spindle-shaped nanosized zirconia (ZrO2) was synthesized by hydrothermal method. The method for the determination of trace Ni2 + with monoclinic spindle-shaped nanostructured ZrO2 as adsorbent and inductively coupled plasma mass spectrometry (ICP-MS) was established. The detection limit of this method for Ni2 + was 0.029 μg / L with a relative standard deviation of 2.7% (n = 6). The results showed that the adsorption rate of Ni2 + by nano-ZrO2 was over 99% at pH 9.0 for 10 min ; 2 mL 0.5 mol / L HCl as eluent for 30 min, the amount of Ni2 + adsorbed on the nano-ZrO2 can be eluted quantitatively, and the elution rate reaches more than 98%; the static adsorption capacity of nano ZrO2 for Ni2 + is 198 μg / Enrichment factor up to 250 times; investigated the impact of co-existing ions and their regeneration performance. The method was applied to the determination of trace nickel in actual water samples. The recovery rate was 96.3% ~ 101.4%.