首页|选择性溶解分离-火花放电原子发射光谱法测定镀镍锡青铜带基材中锡磷铅锌镍

选择性溶解分离-火花放电原子发射光谱法测定镀镍锡青铜带基材中锡磷铅锌镍

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镀镍锡青铜带基材中锡、磷、铅、锌、镍的准确测定是保证产品质量的前提.采用由4.5 mol/L硝酸和1.25 g/L CM-911硝酸缓蚀剂组成的浸泡液,在水浴40 ℃对镀镍锡青铜带样品表面的镍镀层和锡青铜基材进行选择性溶解分离,经过清水和无水乙醇漂洗后,选择压力为70 t,压样时间为2 min,用冷压法将样品压制成块,选择青铜的工作曲线,采用锡青铜标准样品作为控样对工作曲线进行校准,实现了火花放电原子发射光谱法对镀镍锡青铜带基材中锡、磷、铅、锌、镍的测定.选择2卷不同牌号的锡青铜带样品,将其上下面均进行电镀镍工艺的加工,制成镀镍锡青铜样品,按照实验方法对镀镍锡青铜带基材中的锡、磷、铅、锌、镍进行测定,结果表明,当测定元素含量(质量分数,下同)在1%~10%之间时,测定结果的相对标准偏差(RSD,n=6)小于0.3%;当测定元素含量在0.01%~0.4%之间时,测定结果的相对标准偏差(n=6)小于4%.采用GB/T 5121系列方法对锡青铜带中各元素分析以进行方法对照.结果表明,两种方法的测定结果基本一致.方法实现了火花放电原子发射光谱法对多层材料基材的化学成分检测,解决了火花放电原子发射光谱法测定壁厚不足1 mm样品时易击穿样品的难题.
Determination of tin,phosphorus,lead,zinc and nickel in nickel-plated tin bronze strip substrate by selective dissolution separation-spark discharge atomic emission spectrometry
The accurate determination of tin,phosphorus,lead,zinc and nickel in nickel-plated tin bronze strip substrate is the precondition to ensure the product quality.The nickel coating and tin bronze substrate on the surface of nickel-plated tin bronze strip sample were selectively separated with soak solution com-posed of 4.5 mol/L nitric acid and 1.25 g/L CM-911 nitric acid corrosion inhibitor in water bath at 40 ℃.After rinsing with clean water and anhydrous ethanol,the sample was pressed to block by cold-press meth-od.The pressure was 70 t and the pressing time was 2 min.The working curve of bronze was selected.The standard sample of tin bronze was used as control sample for the calibration of working curve.The determi-nation of tin,phosphorus,lead,zinc and nickel in nickel-plated tin bronze strip substrate by spark discharge atomic emission spectrometry was realized.Two rolls of tin bronze sample with different brands were se-lected.The electro-nickeling was conducted for both top and bottom sides to prepare the nickel-plated tin bronze sample.The contents of tin,phosphorus,lead,zinc and nickel in nickel-plated tin bronze strip sub-strate were determined according to the experimental method.The results showed that the relative standard deviations(RSDs,n=6)of determination results were less than 0.3%when the contents(mass fraction,the same below)of elements were in range of 1%-10%.When the contents of testing elements were in range of 0.01%-0.4%,the RSDs(n=6)were less than 4%.GB/T 5121 was used to analyze the elements in tin bronze strip for the comparison.The results showed that the found results of two methods were basically consistent.The proposed method was applicable for the chemical composition detection of multilayer mate-rials by spark discharge atomic emission spectrometry,which solved the problem that the breakdown of sample easily occurred during spark discharge atomic emission spectrometric determination when its wall thickness was less than 1 mm.

selective dissolution separationspark discharge atomic emission spectrometrynickel coatingtin bronzetinphosphorusleadzincnickel

周西林、王娇娜、黄晴晴、弥海鹏、叶反修

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重庆市计量质量检测研究院,重庆 401123

国家铝镁合金及制品质量监督检验中心,重庆 408403

无锡市金义博仪器科技有限公司,江苏无锡 214151

选择性溶解分离法 火花放电原子发射光谱法 镍镀层 锡青铜

国家市场监督管理总局计划科技项目重庆市计量质量检测研究院科技攻关项目

S2023MK06372020研-5

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(1)
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