摘要
变形镍基高温合金牌号众多,组分复杂,各元素含量范围宽.高含量的铬、钼、铌、钛、钒、钨、锆等难熔元素不仅对试样前处理造成阻碍,而且其元素间的光谱干扰会对测定结果造成影响.实验采用5 mL盐硝混酸(体积比为9∶1)-2 mL过氧化氢-2 mL氢氟酸的酸溶体系,在 180 ℃ 下密闭消解 2 h,选择 Al 237.312 nm、Cr 206.550 nm、Cu 327.395 nm、Fe 239.563 nm、Mn 257.610 nm、Mo 203.846 nm、Nb 269.706 nm、Si 288.158 nm、Ti 337.280 nm、V 292.401 nm、W 203.000 nm、Zr 343.823 nm作为分析线,采用基体匹配法配制标准溶液系列消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定上述元素,建立了密闭消解-ICP-AES测定变形镍基高温合金中铝、铬、铜、铁、锰、钼、铌、硅、钛、钒、钨、锆等12种主次元素的方法.各元素校准曲线在线性范围内呈良好的线性关系,相关系数均大于0.999.按照实验方法测定7个变形镍基高温合金标准物质中铝、铬、铜、铁、锰、钼、铌、硅、钛、钒、钨、锆,结果的相对标准偏差(RSD,n=6)为0.50％～4.56％.按照实验方法测定8个变形镍基高温合金标准物质中上述12种元素,测定值与认定值无显著性差异.
Abstract
There are brands of deformed nickel-based superalloy.The composition is complex and the con-tent range of elements is wide.High content refractory elements such as chromium,molybdenum,niobium,titanium,vanadium,tungsten and zirconium not only hinder the pretreatment of sample,but also cause the influence on the determination results due to the spectral interference among elements.In experiments,the sample was dissolved with 5 mL of hydrochloric acid-nitric acid mixture,2 mL of hydrogen peroxide,and 2 mL of hydrofluoric acid.The sample was digested at 180 ℃ for 2 h in the closed system.Al 237.312 nm,Cr 206.550 nm,Cu 327.395 nm,Fe 239.563 nm,Mn 257.610 nm,Mo 203.846 nm,Nb 269.706 nm,Si 288.158 nm,Ti 337.280 nm,V 292.401 nm,W 203.000 nm and Zr 343.823 nm were selected as the ana-lytical lines.The standard solution series were prepared by matrix matching method to eliminate the influ-ence of matrix effect.The above elements were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The method for the determination of 12 major and minor elements(including alu-minum,chromium,copper,iron,manganese,molybdenum,niobium,silicon,titanium,vanadium,tungsten and zirconium)in deformed nickel-based superalloy by ICP-AES after digestion in closed system was estab-lished.The calibration curves of elements showed good linearity within the linear range,and the correlation coefficients were all higher than 0.999.The contents of aluminum,chromium,copper,iron,manganese,mo-lybdenum,niobium,silicon,titanium,vanadium,tungsten and zirconium in seven certified reference materi-als of deformed nickel-based superalloy were determined according to the experimental method.The relative standard deviations(RSDs,n=6)of determination results were between 0.50％and 4.56％.Above twelve elements in eight certified reference materials of deformed nickel-based superalloy were determined accord-ing to the experimental method,and the found results had no significant difference with the certified val-ues.
NETL
NSTL
维普
万方数据