过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铝合金中的铬铁钼硅
| 1. | 广西冶金研究院, 广西 南宁 530023 |
| 2. | 玉溪市环境监测站, 云南 玉溪 653100 |
Determination of Chromium, Iron, Molybdenum and Silicon in Ti-Al Alloy by Inductively Coupled Plasma-Optical Emission Spectrometry with Sodium Peroxide Alkali Fusion
| 1. | Guangxi Research Institute of Metallurgy, Nanning 530023, China |
| 2. | Yuxi Environmental Monitoring Station, Yuxi 653100, China |
摘要：应用电感耦合等离子体发射光谱法(ICP-OES)测定高钛含量的钛铝合金中铬铁钼硅时，单一酸不能使钛铝合金完全溶解；混合酸溶解样品后仍会出现少量杂质、溶解不完全的现象，且复溶时易出现沉淀现象，即使用浓王水也难以将沉淀再溶解。本实验在700℃温度下，采用过氧化钠进行碱熔20 min，盐酸酸化，建立了应用ICP-OES测定钛铝合金中的铬铁钼硅的方法。实验中采用钛基体匹配的方法降低了试液中钛浓度大于200 μg/mL时的钛基体干扰，通过控制过氧化钠使用量来降低待测溶液中的盐分含量保证了测定的稳定性。方法检出限为0.002~0.005 μg/mL，测定下限为0.007~0.017 μg/mL；采用国家标准物质(GBW02501)进行验证，方法的相对标准偏差(RSD)为0.90%~4.89%，相对误差为1.2%~3.6%，回收率为91.6%~103.8%。本方法与酸溶法相比，样品溶解完全，测定准确、可靠，适用于高钛含量的钛铝合金多元素测定。
Determination of Chromium, Iron, Molybdenum and Silicon in Ti-Al Alloy by Inductively Coupled Plasma-Optical Emission Spectrometry with Sodium Peroxide Alkali Fusion
ABSTRACT Single acid cannot completely dissolve Ti-Al alloy with high Ti content when determining chromium, iron, molybdenum and silicon by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). A small amount of impurity remains after dissolving the samples by mixed acid. Furthermore, the precipitation occurs readily during re-dissolution, even if using concentrated aqua regia. In this study, the Ti-Al alloys were fused with sodium peroxide for 20 min at 700℃ and were acidified by hydrochloric acid. The method for the determination of chromium, iron, molybdenum and silicon in Ti-Al alloy by ICP-OES was established. The interference from the titanium matrix in samples was improved by the titanium matrix matching method when the concentration of titanium was greater than 200 μg/mL. Additionally, the amount of salt content in solution was controlled by sodium peroxide to ensure the stability of determination. The detection limits and lower determination limits are 0.02-0.05 μg/mL and 0.07-0.17 μg/mL, respectively. The method has been verified by analyzing the national standard material (GBW02501). The relative standard deviations (RSDs) are 0.90%-4.89%, the relative errors are 1.2%-3.6% and the recoveries are 91.6%-103.8%. Compared with acid solution, the dissolution of the samples is complete using the proposed method. Moreover, the method is accurate, reliable, and suitable for multi-element determination of Ti-Al alloy with high titanium content.
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