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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1.08~26.01mg/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。
The experiment focused on the effects of high carbon content on the determination of magnesium, aluminum, potassium, calcium, chromium, manganese, copper, barium, lead, cadmium and zinc in deashing dust samples and solved the problem of carbon removal. The samples were cleaned by high temperature muffle furnace and the contents of magnesium, aluminum, potassium, calcium, chromium, manganese, copper, barium, lead, cadmium and zinc were determined by digestion of hydrochloric acid-nitric acid-hydrofluoric acid- (ICP-AES) was established for the determination of magnesium, aluminum, potassium, calcium, chromium, manganese, copper, barium, lead and cadmium in high-carbon dust with ICP- AES , Zinc and other elements of the method. Under the best working condition of instrument, the linear correlation coefficient r of each element calibration curve is greater than 0.999 5, and the detection limit is 1.08 ~ 26.01 mg / kg. The method was applied to the determination of magnesium, aluminum, potassium, calcium, chromium, manganese, copper, barium, lead, cadmium and zinc in the deashing dust samples. The relative standard deviations (RSD, n = 11) were 0.90% -7.1% , And the recoveries of target elements were 90% ~ 117%. The determination of magnesium, aluminum, potassium, calcium and zinc in the dust by the experimental method was in good agreement with the results of flame atomic absorption spectrometry (FAAS).