密闭消解-电感耦合等离子体发射光谱(ICP-OES)法测定金镍铬铁硅硼合金粉末中铬、铁、硅含量
Determination of chromium,iron,silicon content in gold nickel chromium iron silicon boron alloys by inductively coupled plasma optical emission spectroscopy(ICP-OES)with sealed-digestion
鲁瑞智 1赵万春 1马媛 2陶赛祥 1付仕梅 1杨晓滔1
作者信息
- 1. 贵研检测科技(云南)有限公司,云南昆明 650106
- 2. 贵研检测科技(云南)有限公司,云南昆明 650106;贵研铂业股份有限公司稀贵金属综合利用新技术国家重点实验室,云南昆明 650106
- 折叠
摘要
金镍铬铁硅硼合金粉末是一种性能优良的钎焊材料,被广泛应用于航空航天领域,建立一种准确、简便、快速的检测方法对控制金镍铬铁硅硼合金粉末的产品质量具有重要意义.现有国标方法GB/T 39138.20-2020对溶解条件要求严苛,不易掌握.本文称取0.2 g合金粉末试样,采用聚四氟乙烯消化罐,在温度140 ℃±10℃,硝酸-盐酸-氢氟酸介质条件下,对合金粉末试样密闭消解60 min后,硼酸络合过量的氢氟酸,使用电感耦合等离体发射光谱(ICP-OES)对其中的Cr、Si、Fe含量进行同时测定,选取分析谱线 Cr284.325、Fe238.204、Si288.158进行结果计算,测定结果与国标方法GB/T 39138.20-2020测定结果吻合,加标回收率为97.2％～101.1％,相对标准偏差(RSD)为0.97％～1.41％,试验数据说明该方法具有可信度.该方法克服了现有国标方法溶解条件要求严苛的缺陷,使得溶解更加完全,不易造成Si损失,降低了试样前处理难度,是一种易于掌握、结果准确度高、环境友好的分析检测方法.
Abstract
Gold nickel chromium iron silicon boron alloys is a kind of excellent brazing material,which is widely used in aerospace field.It is of great significance to establish an accurate,simple and rapid detection method for guaranteeing the properties of gold-nickel-chromite ferrosilicon-boron alloy powders.The existing GB/T 39138.20-2020 has strict requirements on dissolution conditions and is difficult to master.In this paper,a sample of 0.2 g alloy powder was measured and dissolved by HNO3-HCl-HF with sealed-digestion at 140 ℃±10 ℃ and dilute solution 60 min and boric acid complex excess HF.The contents of chromium,iron and silicon were determined simultaneously by inductively coupled plasma optical emission spectrometry(ICP-OES).It is selection wavelength Cr284.325,Fe238.204,Si288.158 to result computation.The results were same with GB/T 39138.20-2020,the results adding standard recovery was 97.2％～101.1％,the results ofrelative standard deviationwas 0.97％～1.41％.The experimental data show that the method is reliable.This method overcomes the defects of the current national standard method with strict dissolution conditions,makes the dissolution more complete,avoids the loss of silicon content,and reduces the difficulty of sample pretreatment.It is an easy to master,high accuracy and environmentally friendly analysis method.
关键词
金镍铬铁硅硼合金粉末/电感耦合等离体发射光谱(ICP-OES)/密闭消解/铬/铁/硅Key words
gold-nickel-chromium-iron-silicon-boron alloys/ICP-OES/sealed-digestion/chromium/iron/silicon引用本文复制引用
出版年
2024
NETL
NSTL
万方数据