Universidade Federal do Paraná, Departamento de Química, 81531-980, Curitiba, Paraná, Brazil.
Universidad Nacional de Colombia Sede Manizales, Caldas, Colombia.
Talanta. 2021 Jan 1;221:121457. doi: 10.1016/j.talanta.2020.121457. Epub 2020 Jul 31.
The complexity of aerodynamic particulate matter's (PM) matrices poses a challenge for the extraction and quantification of metals, especially for analytes with low concentration. Aiming to solve this issue, a precise and accurate protocol with the ultrasound extraction combined with microwave radiation digestion (USMW), was applied to PM samples with excellent compensations in sample throughput, digestion efficiency, and energy consumption. After the digestion and extraction procedures, the inorganic analytes, including rare earth elements, were determined by ICP OES. Two types of particulate matter sampled from two stations, Gobernacion (GOB10 and GOB2.5) and Milan (MIL10), corresponding to PM and PM, were digested with a combination between HF, HNO, and HBO. The absolute limits of detection ranged from 0.42 pg m³ for V, to 3459 pg m³ for As. The accuracy of the experimental study was assessed using two certified reference materials (CRMs), Coal Fly Ash (NIST1633b) and Fly Ash (BCR176). The method presented good accuracy, with recoveries ranging from 90 to 115%, except for Al (120%) and Fe (123%). Considering the replicates for the determination of analyte elements, the repeatability was below 10% for the relative standard deviation (RSD). A cloud point extraction (CPE) procedure, with parameters optimized for the determination of Pd and Pt, was successfully applied in digested PM samples with detection limits of 1.43 and 2.05 pg m³ for Pd and Pt in MIL10 sample, respectively, and 76.6 pg m³ for Pd and 110 pg m³ for Pt, in samples GOB10 and GOB2.5, respectively.
大气颗粒物(PM)基质的复杂性给金属的提取和定量带来了挑战,特别是对于浓度较低的分析物。为了解决这个问题,我们采用了一种精确、准确的方法,即超声提取结合微波辐射消解(USMW),该方法在样品通量、消解效率和能耗方面具有出色的补偿效果。在消化和提取过程之后,通过电感耦合等离子体发射光谱法(ICP-OES)测定无机分析物,包括稀土元素。使用 HF、HNO 和 HBO 的组合对从两个站点(Gobernacion [GOB10 和 GOB2.5] 和 Milan [MIL10])采集的两种类型的颗粒物(PM 和 PM )进行消化。绝对检出限范围从 V 的 0.42 pg m³到 As 的 3459 pg m³。使用两种经过认证的参考物质(CRM),煤飞灰(NIST1633b)和粉煤灰(BCR176)评估实验研究的准确性。该方法的准确度良好,回收率在 90%至 115%之间,除了 Al(120%)和 Fe(123%)。考虑到分析物元素的测定重复次数,相对标准偏差(RSD)的重复性低于 10%。成功应用了一种浊点萃取(CPE)程序,该程序针对 Pd 和 Pt 的测定进行了优化,在 MIL10 样品中,Pd 和 Pt 的检出限分别为 1.43 和 2.05 pg m³,在 GOB10 和 GOB2.5 样品中,Pd 的检出限分别为 76.6 pg m³和 Pt 的检出限为 110 pg m³。