作者：刘攀^1,2, 李治亚¹, 杜米芳¹, 高灵清^1,3, 韩华云⁴

作者单位：1. 中国船舶重工集团公司第七二五研究所（洛阳船舶材料研究所），河南 洛阳 471023;
2. 国家新材料生产应用示范平台（先进海工与高技术船舶材料），河南 洛阳 471023;
3. 河南省船舶及海工装备结构材料技术与应用重点实验室，河南 洛阳 471023;
4. 郑州大学化学与分子工程学院，河南 郑州 450000

关键词：石墨炉;原子吸收法;非合金钢;低合金钢;碳素钢;痕量铅

摘要：

建立石墨炉-原子吸收法测定非合金钢（碳素钢）和低合金钢中痕量铅的分析方法，并优化消解用酸、介质酸度、灰化温度、原子化温度等条件参数，考察铁基体和共存元素的干扰影响。确定的最佳工作条件和试验方法如下：石墨炉的灰化温度为500 ℃，原子化温度为2100 ℃，分析谱线波长为283.3 nm。样品称取0.125 g，采用硝酸（1+1）消解，并以5%硝酸定容至25 mL。采用基体匹配法、以铁基体溶液建立系列校准曲线，校准曲线的线性相关关系为0.9999，方法的定量限为1.8 ng/mL（质量浓度）或0.00004%（质量分数），加标回收率为87%~112%。按实验方法测定有证标准样品（YSB C 41102-04）中痕量铅，其结果为0.00029%，与认定值（w(Pb)=0.0003%）相符。

Determination of trace lead content in non-alloy steel and low-alloy steel by graphite furnace atomic absorption spectrometry
LIU Pan^1,2, LI Zhiya¹, DU Mifang¹, GAO Lingqing^1,3, HAN Huayun⁴
1. Luoyang Ship Material Research Institute, Luoyang 471023, China;
2. National New Material Production and Application Demonstration Platform (Advanced Marine Engineering and High-tech Ship Materials), Luoyang 471023, China;
3. Henan Key Laboratory of Technology and Application of Structural Materials for Ship and Marine Equipment, Luoyang 471023, China;
4. College of Chemistry and Molecular Engineering, Zhengzhou University, Zhengzhou 450000, China
Abstract: Working conditions for the determination of trace lead in non-alloy steel (carbon steel) and low-alloy steel by graphite furnace atomic absorption spectrometry were optimized, such as the acid for digestion, acidity of the solution, ashing temperature and atomization temperature. The effect of iron matrix and coexisting ions on the measurement results of trace lead were studied. The optimal operating conditions were obtained as below: the ashing temperature of 500 ℃, atomization temperature of

℃ and analysis line wavelength of 283.3 nm. Sample of 0.125 g was dissolved in nitric acid (1+1), then the volume was made up to 25 mL by 5% nitric acid. The calibration curve was established by a series of iron matrix solutions with the linear correlation of 0.999 9. The quantification limit of the method was 1.8 ng/mL (mass concentration) or

% (mass fraction), and the recoveries were between 87% and 112%. The trace lead in the certified standard sample (YSB C 41102-04) was determined applying the experimental method, and the result was

%, which was consistent with the certified value (w(Pb)=

%).
Keywords: graphite furnace;atomic absorption spectrometry;non-alloy steel;low-alloy steel;carbon steel;trace lead
2021, 47(7):55-59  收稿日期: 2020-07-30;收到修改稿日期: 2020-09-21
基金项目: 先进海工与高技术船舶材料生产应用示范平台（TC180A6MR/2）
作者简介: 刘攀(1989-),男,江苏邳州市人,工程师,从事无机分析化学与冶金材料测试工作
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