Abstract The influence of the particle size distribution of a petroleum coke sample compared to its sulfur content was investigated. For this matrix, an optimization procedure of the Suspension Assisted Analysis (SAA) by Total-reflection X-Ray Fluorescence (TXRF) quantitative method was developed. SAA-TXRF sulfur recoveries were evaluated for three particle size distributions of the same coke sample. The sulfur recovery increased when the particle size distribution was smaller. The observed behaviour was correlated and validated with CHNS elemental analysis and microwave-assisted digestion TXRF measurements. The results indicate that the sulfur signal is strongly influenced by the particle size distribution and the deposition morphology of the petroleum coke material. This effect could be explained by the presence of a strong absorption effect for the sulfur signal in combination with the distortion of the X-ray Standing Waves (XSW) field observed between the analyte, S, and the elements Ti and Co, which were used as an internal standard. The variation in sulfur observed was up to 45.5% lower than the higher recovery obtained by CHNS. This investigation suggests that for an adequate application of the SAA-TXRF method in petroleum coke or similar matrices, careful optimization of the final particle dispersion of the ground coke is crucial and necessary. In this case, the use of a high- power ultrasound probe was the key.

中文翻译：

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全反射X射线荧光悬浮辅助分析石油焦中的硫

摘要 研究了石油焦样品的粒度分布与其硫含量相比的影响。对于该基质，开发了通过全反射 X 射线荧光 (TXRF) 定量方法进行悬浮辅助分析 (SAA) 的优化程序。针对同一焦炭样品的三种粒度分布，评估了 SAA-TXRF 硫回收率。当粒度分布较小时，硫回收率增加。观察到的行为与 CHNS 元素分析和微波辅助消解 TXRF 测量相关和验证。结果表明，硫信号受石油焦材料的粒度分布和沉积形态的强烈影响。这种效应可以通过硫信号的强吸收效应的存在以及在分析物、S 和元素 Ti 和 Co 之间观察到的 X 射线驻波 (XSW) 场的畸变来解释。作为内部标准。观察到的硫变化比 CHNS 获得的更高回收率低 45.5%。该调查表明，为了在石油焦或类似基质中充分应用 SAA-TXRF 方法，仔细优化粉状焦的最终颗粒分散是至关重要且必要的。在这种情况下，使用高功率超声探头是关键。观察到的硫变化比 CHNS 获得的更高回收率低 45.5%。这项调查表明，为了在石油焦或类似基质中充分应用 SAA-TXRF 方法，仔细优化焦炭的最终颗粒分散是至关重要且必要的。在这种情况下，使用高功率超声探头是关键。观察到的硫变化比 CHNS 获得的更高回收率低 45.5%。这项调查表明，为了在石油焦或类似基质中充分应用 SAA-TXRF 方法，仔细优化焦炭的最终颗粒分散是至关重要且必要的。在这种情况下，使用高功率超声探头是关键。