微波消解GFAAS法测定动物骨中铅和镉

Microwave digestion of animal bones and determination of lead and cadmium by graphite furnace atomic absorption spectrometry

通过考察各种微波消解因素对微波消解效果的影响,以及通过对石墨炉原子吸收光谱法测定条件的优化,建立了用微波消解石墨炉原子吸收光谱法测定动物骨中铅和镉的分析方法.结果表明,最佳微波消解条件为消解压力15 MPa;消解时间5 min.最佳石墨炉测定条件为铅灰化温度800 ℃,原子化温度1 300 ℃;镉的灰化温度900 ℃,原子化温度1 200 ℃.方法线性范围为铅1.566～50 ng/mL;镉0.074 5～5 ng/mL.方法检出限为铅0.313 2 ng/mL;镉0.014 9 ng/mL.样品测定的RSD小于5.0%,加标回收率在88.36%～110%之间.

By testing all related factors which have effects on microwave digestion, optimizing the operation conditions of graphite furnace atomic absorption spectrometry （ GFAAS）, the research establishes a sensitive, effective method to determine lead （Pb）, cadmium （Cd） in animal bones. The result has shown that the optimized condition for microwave digestion is： digestion pressure 15 MPa, digestion length 5 min. The best condition for graphite furnace is： Pb （lead） ashing temperature 800 ℃, atomization temperature 1 300 ℃ ; Cd （cadmium） ashing temperature 900 ℃ , atomization temperature 1 200 ℃. The methodical linearity range is Pb 1. 566 -50 ng/mL; Cd 0. 0745 -5 ng/mL. The methodical detection limit is Pb 0. 3132 ng/mL; Cd 0. 0149 ng/mL. The tested RSD of the sample is less than 5%, and the sample assaying recovery rate is between 88.36% and 110%.