电感耦合等离子体原子发射光谱法测定高炉灰中锌  

Determination of zinc in blast furnace dust by inductively coupled plasma atomic emission spectrometry

作　　者：葛青锋 GE Qingfeng(Manufacturing Management Department,Shanghai Meishan Iron and Steel Co.,Ltd.,Nanjing 210039,China)

机构地区：[1]上海梅山钢铁股份有限公司制造管理部,江苏南京210039

出　　处：《冶金分析》2023年第6期85-89,共5页Metallurgical Analysis

摘　　要：准确测定高炉灰中锌含量对高炉灰的科学再利用有着重要指导意义。高炉灰组分复杂,含有矿石、耐火材料、煤焦等,样品前处理过程复杂,检测难度大。以盐酸-硝酸-氢氟酸-过氧化氢为消解体系,用微波消解法处理样品,实现了样品的消解完全;选择Zn 206.201 nm为分析线,用电感耦合等离子体原子发射光谱法(ICP-AES)对样品溶液进行测定,建立了测定高炉灰中锌的方法。在优化的实验条件下,锌的质量浓度在5.00~100.00μg/mL范围内与其对应的发射强度呈线性关系,线性相关系数为0.9999;方法检出限为0.00092%(质量分数)。考察了基体效应,结果表明,高炉灰中铁基体对锌的测定无显著性影响。按照实验方法测定高炉灰样品中锌,结果的相对标准偏差(RSD,n=11)为0.23%~0.87%,加标回收率为98%~102%。The rapid and accurate determination of zinc content in blast furnace dust has important guiding significance for the scientific reuse of blast furnace dust.The composition of blast furnace dust is complex which contains ore,refractory matters,tar oil and other materials.The pretreatment of sample is complicated with high detection difficulty.The sample was treated by microwave digestion with hydrochloric acid-nitric acid-hydrofluoric acid-hydrogen peroxide system,realizing the complete digestion of sample.The sample solution was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES)with Zn 206.201 nm as the analytical line.Consequently,a method for determination of zinc in blast furnace dust was established.Under the optimal experimental conditions,the mass concentration of zinc in the range of 5.00-100.00μg/mL had a linear relationship with its corresponding emission intensity.The linear correlation coefficient was 0.9999.The limit of detection of this method was 0.00092%(mass fraction).The matrix effect was discussed,and it was found that iron matrix in blast furnace dust had no significant influence on the determination of zinc.The contents of zinc in blast furnace dust samples were determined according to the proposed method.The relative standard deviations(RSD,n=11)of determination results were between 0.23%and 0.87%,and the recoveries were between 98%and 102%.

关 键 词：锌 微波消解 电感耦合等离子体原子发射光谱法(ICP-AES) 高炉灰 

分 类 号：O657.31[理学—分析化学] TF547[理学—化学]