选择性溶解分离-电感耦合等离子体原子发射光谱法测定含油轴承中青铜材料中铅和锡  

Determination of lead and tin in bronze materials in oil bearings by selective dissolution separation-inductively coupled plasma atomic emission spectrometry

作　　者：周西林 王娇娜 黄晴晴 弥海鹏 李晓锋 ZHOU Xilin;WANG Jiaona;HUANG Qingqing;MI Haipeng;LI Xiaofeng(Chong Qing Academy of Metrology and Quality Inspection,Chongqing 401123,China;National Quality Supervision and Inspection Center for Aluminum Magnesium Alloys and Products,Chongqing 408403,China)

机构地区：[1]重庆市计量质量检测研究院,重庆401123 [2]国家铝镁合金及制品质量监督检验中心,重庆408403

出　　处：《冶金分析》2024年第2期18-23,共6页Metallurgical Analysis

基　　金：国家市场监督管理总局计划科技项目(S2023MK0637);重庆市计量质量检测研究院科技攻关项目[2020(研)-5]。

摘　　要：青铜含油轴承是碳素钢与青铜两种材质的结合体。测定青铜材料中铅和锡时,首先采用选择性溶解分离法,使用含有80 mL过氧化氢、75 g过硫酸铵、60 g柠檬酸铵、2 g六次甲基四胺、40 g氯化铵溶于水中并定容至1 L,组成的浸泡液溶解青铜;在pH值为8~9,温度为(35±2)℃,结合超声波将青铜材料从碳素钢钢背完全脱落在浸泡液中;煮沸除去多余的化学试剂,加入王水,溶解浸泡液中不溶物至溶液清亮;采用基体匹配法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)测定铅和锡,从而建立了选择性溶解分离-电感耦合等离子体原子发射光谱法测定含油轴承中青铜材料中铅和锡的方法。铅在5.0~50.0 mg/L、锡在1.0~20.0 mg/L时,与其相应的发射光谱强度呈良好的线性关系,线性相关系数均大于0.999;方法中铅和锡的检出限分别为0.5 mg/L和0.1 mg/L。按照实验方法测定3个含油轴承中青铜材料中铅和锡,结果的相对标准偏差(RSD,n=5)在2%以内;回收率在99.0%~101.4%之间;分别采用实验方法与GB/T 5121国标方法进行比对,结果相一致。The bronze oil bearing is the combination of two materials,i.e.,carbon steel and bronze.For the determination of lead and tin in bronze materials,the selective dissolution separation method was used.The immersion solution was prepared by dissolving 80 mL of hydrogen peroxide,75 g of ammonium persulfate,60 g of ammonium citrate,2 g of hexamethylenetetramine and 40 g of ammonium chloride in water followed by dilution to 1 L.The bronze sample was digested using the immersion solution prepared.The bronze material was completely released from the carbon steel back in the immersion solution at pH 8-9 and(35±2)℃by ultrasonic.The excessive chemicals were removed by boiling.Then aqua regia was added to dissolve the insoluble matters in the immersion solution until the solution was clear.The influence of matrix effect was eliminated by matrix matching method.The contents of lead and tin were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The method for the determination of lead and tin in bronze materials in oil bearings by ICP-AES after selective dissolution separation was established.The concentration of lead(5.0-50.0 mg/L)and tin(1.0-20.0 mg/L)showed good linear relationship with the corresponding emission intensity,and the linear correlation coefficients were higher than 0.999.The limits of detection for lead and tin were 0.5 mg/L and 0.1 mg/L,respectively.The contents of lead and tin in three oil bearing samples were determined according to the experimental method,and the relative standard deviations(RSD,n=5)of determination results were within 2%.The spiked recoveries were between 99.0%and 101.4%.The experimental method was compared with the national standard method GB/T 5121,and the found results were consistent.

关 键 词：选择性溶解分离法 电感耦合等离子体原子发射光谱法(ICP-AES) 青铜含油轴承 铅 锡 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学]