电感耦合等离子体原子发射光谱法测定高碳除尘灰中11种元素

实验重点探讨了高含量碳对除尘灰样品中镁、铝、钾、钙、铬、锰、铜、钡、铅、镉、锌等元素测定的影响,并解决了除碳的问题。样品使用马弗炉高温除碳,采用盐酸-硝酸-氢氟酸-高氯酸消解样品灰分,选择了镁、铝、钾、钙、铬、锰、铜、钡、铅、镉、锌等元素的分析谱线和扣背景模式,建立了使用电感耦合等离子体原子发射光谱法(ICP-AES)测定高碳除尘灰中镁、铝、钾、钙、铬、锰、铜、钡、铅、镉、锌等元素的方法。在仪器最佳工作条件下,各元素校准曲线线性相关系数r均大于0.999 5,方法检出限在1.08～26.01 mg/kg之间。方法应用于除尘灰实际样品中镁、铝、钾、钙、铬、锰、铜、钡、铅、镉、锌的测定,结果的相对标准偏差(RSD,n=11)为0.90%～7.1%,目标元素的加标回收率为90%～117%;按照实验方法测定除尘灰中镁、铝、钾、钙、锌,结果与火焰原子吸收光谱法(FAAS)的测定结果相吻合。

Determination of eleven elements in high carbon dedusting ash byinductively coupled plasma atomic emission spectrometry

The influence of high content carbon on determination of magnesium, aluminum, potassium, calcium, chromium, manganese, copper, barium, lead, cadmium and zinc in high carbon dedusting ash was focused on and discussed. Meanwhile, the problem of carbon removal was also solved. After the carbon in dedusting ash sample was removed by high temperature in muffle furnace, the ashes were dissolved by hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid. Then, the analytical lines and background deduction mode of magnesium, aluminum, potassium, calcium, chromium, manganese, copper, barium, lead, cadmium and zinc were selected. Consequently, a determination method of magnesium, aluminum, potassium, calcium, chromium, manganese, copper, barium, lead, cadmium and zinc in high carbon dedusting ash was established by inductively coupled plasma atomic emission spectrometry(ICP-AES). Under the optimal working conditions of instrument, the linear correlation coefficients (r) of calibration curves were all higher than 0.999 5. The detection limits of method were in range of 1.08-26.01 mg/kg. The proposed method was applied to the determination of magnesium, aluminum, potassium, calcium, chromium, manganese, copper, barium, lead, cadmium and zinc in high carbon dedusting ash actual sample. The relative standard deviations (RSD, n=11) were between 0.90% and 7.1%. The recoveries were between 90% and 117%. The content of magnesium, aluminum, potassium, calcium and zinc in dedusting ash was determined by the experimental method, and the results were consistent with those obtained by flame atomic absorption spectrometry (FAAS).