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Silicon determination via a SiO rotational line using high-resolution graphite furnace molecular absorption spectrometry: A straightforward approach for the analysis of solid samples prepared as suspensions
Spectrochimica Acta Part B: Atomic Spectroscopy ( IF 3.2 ) Pub Date : 2021-07-27 , DOI: 10.1016/j.sab.2021.106266
Michele S.P. Enders 1 , Gilberto S. Coelho Junior 1 , Leticia Z. Pires 1, 2 , Daniel L.G. Borges 1
Affiliation  

High-resolution graphite furnace molecular absorption spectrometry combined with samples prepared as suspensions were used for the quantification of Si in geological and spent catalyst samples used for petrochemical processing. Measurements at the main Si resonance line at 251.6110 nm were proven unfeasible due to the formation of a quasi-continuous signal, which resulted in significant memory effect. An alternative was to monitor the fine rotational spectrum of SiO, which allowed memory effect-free measurements. A SiO rotational line centered at 231.9373 nm was therefore used to carry out quantitative analysis of Si at high percent concentrations in a variety of solid samples. Pyrolysis and vaporization temperatures were evaluated and optimized as 800 °C and 2400 °C, respectively, without the need to use a chemical modifier. Attempts to produce SiO molecules from acidified aqueous standards containing Si were unsuccessful, and the molecule could only be originated from solid samples, likely due to the formation mechanism that involves thermal decomposition of silicates. Hence, solid samples were prepared as suspensions in 0.14 mol L−1 HNO3. Calibration was performed using a series of suspensions prepared from a gabbro rock certified reference material (CRM), resulting in a limit of detection (LOD) of 0.5% (m/m). The accuracy of the method was attested by the analysis of several CRM, including rocks, soils and sediments. Solid spent petrochemical catalyst samples used for petrochemical processing were also analyzed and 97–114% recovery was obtained by spiking the catalyst suspensions with a CRM. The good accuracy demonstrated that the formation of SiO is free from matrix effects and highly efficient under the adopted conditions. Overall, the method was proven accurate and consists on a simple and fast alternative to determine Si in silicate-rich samples.



中文翻译:

使用高分辨率石墨炉分子吸收光谱法通过 SiO 旋转线测定硅:分析制备为悬浮液的固体样品的直接方法

高分辨率石墨炉分子吸收光谱法与制备成悬浮液的样品相结合,用于定量分析用于石油化工加工的地质和废催化剂样品中的 Si。由于在 251.6110 nm 处的主 Si 共振线的测量被证明是不可行的,因为形成了连续信号,从而产生显着的记忆效应。另一种方法是监测 SiO 的精细旋转光谱,这允许无记忆效应测量。因此,使用以 231.9373 nm 为中心的 SiO 旋转线对各种固体样品中的高百分比浓度的 Si 进行定量分析。热解和汽化温度分别评估和优化为 800 °C 和 2400 °C,无需使用化学改性剂。尝试从含有 Si 的酸化水溶液标准品中产生 SiO 分子的尝试没有成功,该分子只能来自固体样品,这可能是由于涉及硅酸盐热分解的形成机制。因此,固体样品在 0.14 mol L -1 HNO中制备为悬浮液3 . 使用由辉长岩认证参考材料 (CRM) 制备的一系列悬浮液进行校准,检测限 (LOD) 为 0.5% (m/m)。该方法的准确性通过对岩石、土壤和沉积物等多种 CRM 的分析得到证实。还分析了用于石化加工的固体废石化催化剂样品,通过向催化剂悬浮液中添加 CRM 获得了 97-114% 的回收率。良好的精度表明,在所采用的条件下,SiO的形成不受基体效应的影响且效率高。总体而言,该方法被证明是准确的,并且是一种简单快速的替代方法,可用于测定富含硅酸盐的样品中的硅。

更新日期:2021-07-27
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