摘要:
样品经灼烧灰化后,用盐酸、硝酸溶解残渣,在稀王水介质中用电感耦合等离子体发射光谱法测定载金炭中的铜、铁、钙和镁。试验了烘样温度、灼烧坩埚的材质、温度和时间、测定介质及共存元素干扰等因素的影响。结果表明,载金炭的烘样温度宜选择150℃,石英材质的坩埚耐侵蚀性高于瓷坩埚,且空白值低、结果稳定,载金炭中共存元素不干扰铜、铁、钙和镁的测定。该方法用于样品的分析,相对标准偏差(RSD)为0.78%~2.69%,加标回收率为97.1%~104.5%,各元素的测定值与火焰原子吸收光谱法的结果基本一致。方法简便,实用性强。
关键词:
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载金炭
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铜
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铁
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钙
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镁
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电感耦合等离子体发射光谱法
Abstract:
This article introduces a method of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for the determination of copper, iron, calcium and magnesium in gold-loaded carbon. After incineration, the residua of the sample were dissolved by HCl and HNO3, and then the solution in diluted aqua regia was determined by ICP-AES. Factors such as sample drying temperature, the material of the crucible, incineration temperature, incineration time, and media for testing and the interference of the coexisting elements was studied in detail on how they influence the result. The results show that the proper sample drying temperature for the gold-loaded carbon was 150℃. The inoxidability of the quartz pot is higher than that of ceramic crucible, and it also has a lower blank, and stable results. Through an interference test, the coexisting elements in the gold-loaded carbon did not interfere with the determination of copper, iron, calcium and magnesium. This method was applied to the analysis of samples with the relative standard deviations (RSDs) for Cu, Fe, Ca and Mg in the range of 0.84%-1.45%, 0.80%-1.44%, 0.78%-2.69% and 0.96%-2.61%, respectively. Standard addition recoveries for Cu, Fe, Ca and Mg were in the range of 98.5%-100.9%, 99.4%-102.0%, 97.1%-102.5% and 100.7%-104.5%, repectively. The method was simple, and suitable for simultaneous determination of multiple elements.
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