微波消解-电感耦合等离子体原子发射光谱法测定炉渣中硼

Determination of boron in furnace slag by inductively coupled plasma atomic emission spectrometry with microwave digestion

使用盐酸-氢氟酸并采用微波消解处理炉渣样品,选择B 182.577nm或B249.678nm为分析线,在基体没有明显干扰的情况下,选择自动匹配法(FITTED)进行谱线校正并扣除相应背景,采用高纯物质进行基体匹配后,配制标准溶液系列,建立了使用电感耦合等离子体原子发射光谱法(ICP-AES)测定炉渣系列样品中硼元素含量的方法。硼的质量分数为0.000 6%~0.25%(B 182.577nm)或0.000 8%~0.25%(B 249.678nm)范围内校准曲线呈线性,线性相关系数r均不小于0.999 8;方法中硼的检出限小于0.000 2%。方法应用于炉渣样品中硼的测定,结果的相对标准偏差(RSD,n=6)小于3%,加标回收率为96%~102%,与电感耦合等离子体质谱法(ICP-MS)进行比较,测定结果较为满意。

The furnace slag sample was treated by microwave digestion in hydrochloric acid-hydrofluoric acid system.B 182.577 nm or B 249.678 nm was selected as the spectral line.The automatic matching method(FITTED)was used for spectral correction and background deduction under the condition that the matrix had no obvious interference.The standard solution series and calibration curves were prepared by matrix matching method.The determination method of boron in furnace slag byinductively coupled plasma atomic emission spectrometry(ICP-AES)with microwave digestion was established.The calibration curves were linear when the mass fraction of boron was in range of 0.000 6%-0.25%(B 182.577 nm)or0.000 8%-0.25%(B 249.678 nm).The linear correlation coefficients(r)were not less than 0.999 8.The detection limit of boron in this method was less than 0.000 2%.The proposed method was applied for the determination of boron in furnace slag samples.The relative standard deviations(RSD,n=6)of determination results were less than 3%.The spiked recoveries were between 96% and 102%.The found results were consistent with those obtained by inductively coupled plasma mass spectrometry(ICP-MS).