使用2.0 mL硝酸和10.0 mL盐酸溶解样品,选择As 188.979 nm、Sn 189.927 nm、Sb 206.836 nm为分析线并采用两点校正法扣除背景,建立了使用电感耦合等离子体原子发射光谱法(ICP-AES)测定船用钢中砷、锡和锑的分析方法.采用基体匹配法配制标准溶液系列并绘制校准曲线,方法中各元素校准曲线线性关系良好,相关系数均不小于0.999;方法中各元素的检出限不大于0.0002%(质量分数).按照实验方法测定低合金钢标准样品中砷、锡和锑,结果的相对标准偏差(RSD,n=10)为0.38%~3.0%,测定结果与认定值相吻合;方法应用于船用钢样品中砷、锡、锑的测定,结果的相对标准偏差(RSD,n=10)不大于5%,测定结果与采用氢化物-原子荧光光谱法的测定结果一致.
The sample was dissolved using 2.0 mL of nitric acid and 10.0 mL of hydrochloric acid .As 188.979 nm ,Sn 189 .927 nm and Sb 206 .836 nm were selected as the analysis lines .The background was deducted by two-point correction method .The analysis method of arsenic ,tin and antimony in steel for ship by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established .The standard solution series were prepared by matrix matching method for the plotting of calibration curve .The linearity of calibration curve for each element was good with correlation coefficient higher than 0 .999 .The detection limits were less than 0 .0002% (mass fraction) .The content of arsenic ,tin and antimony in standard sam-ple of low alloy steel was determined according to experimental method .The relative standard deviations (RSD ,n=10) were between 0 .38% and 1 .9% .The determination results were consistent with the certi-fied values .The proposed method was also applied to the determination of arsenic ,tin and antimony in steel sample for ship .RSD (n=10) was less than 5% and the found results were consistent with those ob-tained by hydride generation-atomic fluorescence spectrometry .
参考文献
| [1] | 武映梅;宋兆华;萧民强.X射线荧光光谱法测定低合金钢中的12个元素[J].南方金属,2005(1):27-29,31. |
| [2] | 王明军;何雪梅;焦万里;梁征.微波消解-电感藕合等离子体质谱法测定钢铁中砷、铅、锑、锡、铜[J].化工矿产地质,2011(1):58-60. |
| [3] | 马尚.利用电感耦合等离子体质谱仪分析技术联合测定合金中的锡、锑、磷[J].黑龙江科技信息,2013(03):78. |
| [4] | 郑善峰;吴长浩.应用发射光谱法测定钢中砷、锡、铅、锑、铋的含量[J].一重技术,2004(3):37-39. |
| [5] | 陆伟星;朱伟长.ICP-AES法直接测定钢中铅、锡、砷、锑和铋[J].安徽工业大学学报（自然科学版）,2009(4):386-389,393. |
| [6] | 赵江林.ICP法测定钢中铅锡砷锑铋[J].商情,2013(25):258. |
| [7] | 张伟东;周春丽;李建梅;何安元;张杰;郝静.氢化物发生-电感耦合等离子体原子发射光谱法测定钢中微量砷、锑、铋[J].理化检验：化学分册,2012(10):1161-1163. |
| [8] | 支国瑞;刘吉红;马宏彦;王艳莉;石晓风.ICP-AES法直接测定钢中微量砷、锡、锑[J].光谱实验室,2002(4):485-487. |
| [9] | 刘金祥,李文彪.电感耦合等离子体原子发射光谱法同时测定低合金钢中常量及痕量元素[C].2008年全国化学及光谱分析学术会议论文集,2008:91-94. |
| [10] | 韩华云;唐静;王哲光;张西林.氢化物发生-原子荧光光谱法测定钢中微量锡[J].冶金分析,2008(6):45-48. |
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