Feasibility study of calibration strategy for direct quantitative measurement of K and Mg in plant material by laser-induced breakdown spectrometry

Daniel Menezes Silvestre, Felipe Miranda Barbosa, Bruno Teves Aguiar, Flávio Oliveira Leme, Cassiana Seimi Nomura
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引用次数: 17

Abstract

The calibration and quantitative measurement is the “Achilles heel” of the LIBS technique. This paper deals with a method developed for the direct measurement of K and Mg in plant samples. Instrumental parameters were optimized and the best condition found was a 50 μm spot size, 10 Hz laser repetition rate, 75 accumulated laser pulses with 25 mJ/pulse and 0.25 μs of delay time. For method calibration, the use of synthetic standard calibrating material prepared by the addition of increasing concentrations of K and Mg in wood, filter paper and babassu mesocarp was proposed in order to assess the feasibility of using these various matrices in plant samples analysis. The limits of detection of proposed method were 2–30 and 6–27 μg g−1 for K and Mg, respectively. The use of the carbon emission wavelength at 247.856 nm was used as internal standard to improve the analytical results. Certified reference materials of plants were used to check the accuracy of the proposed method and recovery around 82% and 100% were obtained in all cases.

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激光诱导击穿光谱法直接定量测定植物材料中钾、镁的校准策略的可行性研究
校准和定量测量是LIBS技术的“致命弱点”。本文研究了一种直接测定植物样品中钾和镁的方法。结果表明:光斑尺寸为50 μm,激光重复频率为10 Hz,累积激光脉冲75次,脉冲长度为25 mJ/脉冲,延迟时间为0.25 μs。为了评估在植物样品分析中使用这些不同基质的可行性,提出了在木材、滤纸和巴巴苏中果皮中添加浓度不断增加的K和Mg制备的合成标准校准材料。该方法对K和Mg的检出限分别为2 ~ 30和6 ~ 27 μg−1。采用247.856 nm碳发射波长作为内标,改进分析结果。采用植物标准物质验证方法的准确度,回收率分别为82%和100%。
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