Simple and sensitive determination of tramp elements in ferrous scrap

简单、灵敏地测定黑色金属废料中的杂质元素

基本信息

批准号：
09650897
负责人：
TANAKA Tatsuhiko
金额：
$ 2.18万
依托单位：
Science University of Tokyo
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
1997
资助国家：
日本
起止时间：
1997 至 1999
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-09650897/
关键词：
ferrous scrap tramp element stripping voltammetry trace analysis sensitive analysis steel analysis

项目摘要

A high sensitive method is described for the direct determination of tramp elements at the low ppm level in ferrous scrap based on stripping voltammetry without troublesome separation of iron matrix taking a lot of skill and time. The desired element in acidic medium was accumulated on and/or in a working electrode for a certain time, and the deposit was then electrolytically stripped at a scan rate of 20〜50 mV sィイD1-1ィエD1. A stripping curve was recorded by means of a differential pulse mode. The concentration of the desired element was determined by reference to a linear calibration curve (peak height or area vs. concentration) constructed with standard solutions. The interference of iron(III) was eliminated by reducing it to iron(II) with potassium iodide or L(+) -ascorbic acid or by adding phosphoric acid in order to complex iron (III). The possible interferences have been evaluated. Copper, arsenic, antimony, tin and molybdenum in iron and steel were determined by anodic stripping voltammetry, tellurium by cathodic stripping voltammetry, and chromium by adsorptive stripping voltammetry, with excellent precision and accuracy. Zinc, cadmium, and lead were simultaneously determined by anodic stripping technique, and copper, lead, and cadmium by constant-current stripping analysis. The relative standard deviations and the detection limits were several percents and 10ィイD1-8ィエD1〜10ィイD1-9ィエD1 M, respectively. The time required for an analysis was within 1 h. The advantages of the proposed methods include simple and rapid operations and lessening contamination hazards.

描述了一种基于溶出伏安法的高灵敏度方法，用于直接测定含铁废料中低 ppm 水平的杂质元素，无需费时费力地分离铁基体。或在工作电极中持续一定时间，然后以20至50mV D1-1的扫描速率电解剥离沉积物，通过记录剥离曲线。微分脉冲模式通过参考用标准溶液构建的线性校准曲线（峰高或面积与浓度）来确定所需元素的浓度，通过将其还原为铁（II）来消除铁（III）的干扰。通过与碘化钾或 L(+)-抗坏血酸或添加磷酸络合铁 (III) 来测定钢铁中的铜、砷、锑、锡和钼。阳极溶出伏安法、阴极溶出伏安法测定碲、吸附溶出伏安法测定铬，阳极溶出法同时测定锌、镉和铅，恒流溶出分析法同时测定铜、铅和镉。 .相对标准偏差和检测限为百分之几个百分点分别为10 D1-8 M，分析所需时间在1 h以内。该方法的优点包括操作简单、快速，并减少污染危险。