碱熔融电感耦合等离子体原子发射光谱法测定生铁中硅锰磷含量.pdfVIP

JOURNAL OF INSPECTION AND QUARANTINE 检验检疫学刊 Vol.24 No. 1 2014 年第 1 期 碱熔融电感耦合等离子体原子发射光谱法 测定生铁中硅锰磷含量 吴金龙 金献忠* （北仑出入境检验检疫局 浙江宁波 315800 ） 摘要摘要 提出了一种电感耦合等离子体原子发射光谱法测定生铁中硅、锰、磷含量的方法。生铁样品采用 氢氧化钠和过氧化钠在锆坩埚内熔融，盐酸浸取；研究了共存元素的影响，浓度在5.0 mg/mL-6.0 mg/mL之间 的钠元素、20 μg/mL 的锆元素以及样品中其他共存元素对各元素的测定结果无影响；考察了酸度效应，盐酸 用量在体积分数8%-12% 时，对各元素测定的影响可以忽略。以生铁标准物质作为样品进行分析，测定值和认 定值相吻合，RSD （n=5 ）为0.3% -1.0% 。 关键词关键词 电感耦合等离子体原子发射光谱法；生铁；硅；锰；磷 中图分类号中图分类号 O657.31; TG115.33 Determination of Silicon Manganese and Phosphorus in Pig Iron with Inductively Coupled Plasma Atomic Emission Spectrometry Wu Jinlong, Jin Xianzhong* (Beilun Entry-Exit Inspection and Quarantine Bureau, Ningbo, Zhejiang, 315012) Abstract: A method was proposed for the determination of silicon, manganese, and phosphorus in pig iron with inductively coupled plasma atomic emission spectrometry . Samples were fused with sodium hydroxide and sodium peroxide in zirconium crucibles and leached out with hydrochloric acid solution. The matrix effect were investigated, no effect on the measured elements by sodium between 5.0 mg/mL and 6.0 mg/mL, zirconium in 20μg/mL and other elements in pig iron was found. Acidity effect was discussed and the effect of the volume of hydrochloric acid between 8 percent and 12 percent was able to be ignored. CRMs of pig iron were analyzed, and good agreements were achieved on the detected levels and the certifi ed values with RSDs (n = 5) being in the range of 0.3 %-1.0%. Key Words: ICP; Pig Iron; Silicon; Manganese; Phosphorus 1 前言 体样品直接分析的技术， ICP-OES法和分光光度 生铁是含碳量2.11%-6.67% 的铁碳合金。根据 法都需要把样品溶解，然后进行分析。从目前的 生铁里碳存在形态的不同，可分为炼钢生铁、铸