微波消解-电感耦合等离子体原子发射光谱法测定钼铁合金中的钼含量 |
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引用本文: | 赵炳建,赵浩年,赵越,史琦,李小林,袁辉. 微波消解-电感耦合等离子体原子发射光谱法测定钼铁合金中的钼含量[J]. 分析测试技术与仪器, 2022, 28(4): 422-426. DOI: 10.16495/j.1006-3757.2022.04.009 |
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作者姓名: | 赵炳建 赵浩年 赵越 史琦 李小林 袁辉 |
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作者单位: | 1.唐山钢铁集团有限责任公司,河北 唐山 063000 |
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基金项目: | 河钢唐钢2022年科技项目(2022科11001C、2022科11002C),河钢唐钢2022年专家课题(ZJ22-05G) |
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摘 要: | 采用电感耦合等离子体原子发射光谱法(ICP-OES)测定钼铁合金试样(钼质量分数为55%~65%)中的钼含量,单点校准获得了较好的线性.样品经酸化后微波消解处理,采用钇元素作为内标以减少仪器波动的影响,在波长202.030 nm的分析谱线处测得钼元素的最佳发射强度.检测结果显示微波消解的样品溶解时间可缩短为重量法的14%,检测结果的相对标准偏差为0.17%~0.22%,采用标准样品验证结果的准确度与重量法无显著差异,可以为ICP-OES法检测高含量组分提供参考.
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关 键 词: | 电感耦合等离子体原子发射光谱法 微波消解 钼铁合金 |
收稿时间: | 2022-09-28 |
Determination of Ferromolybdenum Alloy by Microwave Digestion-Inductively Coupled Plasma Atomic Emission Spectrometry |
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Affiliation: | 1.Tangshan Iron and Steel Co. Ltd., Tangshan 063000, Hebei China2.Miami College of Henan University, Kaifeng 475000, Henan China |
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Abstract: | The ferromolybdenum alloy (molybdenum content 55%~65%) was determined by inductively coupled plasma atomic emission spectrometry (ICP-OES), and good linearity was obtained using the single point calibration. The sample was acidified and microwave digestion was carried out, yttrium was added as the internal standard element to reduce the influence of instrument fluctuation and the optimum emission intensity of molybdenum was measured at the analytical line of 202.030 nm. The results showed that the microwave digestion can reduce the dissolution time of the sample to 14% of the weight method, and the relative standard deviation was 0.17%~0.22%. The accuracy of the validation results for standard samples was equaled to that of the gravimetric method, which provides a reference for the ICP-OES method to detect high content components. |
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