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Extraction and pre-concentration of platinum and palladium from microwave-digested road dust via ion exchanging mesoporous silica microparticles prior to their quantification by quadrupole ICP-MS

机译:在四极杆ICP-MS定量分析之前通过离子交换介孔二氧化硅微粒从微波消化的道路灰尘中提取和预浓缩铂和钯

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摘要

We report on the use of mesoporous silica microparticles (μPs) functionalized with quarternary amino groups for the isolation of platinum and palladium tetrachloro complexes from aqueous road dust digests. The μPs have a size ranging from 450 to 850 nm and are suspended directly in the aqueous digests, upon which the anionic Pt and Pd complexes are retained on the cationic surface. Subsequently, the μPs are separated by centrifugation. Elements that cause spectral interferences in ICP-MS determination of Pt and Pd can be quantitatively removed by adding fresh 0.240 mol L−1 HCl to the μPs and by repeating the centrifugation step. The analyte-loaded μPs are then dissolved in 0.1 mL of 2 mol L−1 HF, diluted to 2 mL, and the solutions thus obtained are analyzed by quadrupole ICP-MS. This method avoids analyte elution from the sorbent. This “dispersed particle extraction” approach yielded a run-to-run relative standard deviation ≤ 5 % for Pt and ≤ 4 % for Pd (at 0.1 ng mL−1, n = 4 road dust digests). Method detection limits (expressed as concentrations in the dust samples) are 2 and 1 ng g−1 for Pt and Pd, respectively. The method was validated by analysis of a reference material (BCR CRM 723) and applied to the analysis of road dust samples collected in downtown Vienna. Pt and Pd concentrations in samples collected in summer and in winter were compared, with concentrations ranging from 205 to 1445 ng g−1 for Pt and from 201 to 1230 ng g−1 for Pd.>Graphical AbstractMesoporous silica microparticles (μPs) functionalized with quarternary amino groups were used for isolating platinum and palladium from aqueous road dust digests. The μPs were suspended directly in the aqueous digests, and the analyte-loaded μPs were analyzed using “dispersed particle extraction”.
机译:我们报告了使用具有季氨基功能化的介孔二氧化硅微粒(μPs)从水性道路扬尘消化物中分离铂和钯四氯配合物。 μP的大小范围为450至850 nm,直接悬浮在水性消化液中,其上的阴离子Pt和Pd络合物保留在阳离子表面上。随后,通过离心分离μP。在ICP-MS中测定Pt和Pd时引起光谱干扰的元素可以通过向μPs中添加新鲜的0.240 mol L -1 HCl并重复离心步骤来定量去除。然后将加载了分析物的μPs溶解在0.1mL的2mol L -1 HF中,稀释至2mL,然后通过四极杆ICP-MS分析由此获得的溶液。该方法避免了分析物从吸附剂上洗脱。这种“分散的颗粒提取”方法产生了Pt的运行相对运行相对标准偏差≤5%和Pd的≤4%(在0.1 ng mL -1 ,n = 4道路扬尘消化率下) 。 Pt和Pd的方法检出限(以粉尘样品中的浓度表示)分别为2和1ng g -1 。该方法通过对参考材料(BCR CRM 723)的分析进行了验证,并应用于分析在维也纳市中心收集的道路扬尘样品。比较了夏季和冬季采集的样品中的Pt和Pd浓度,Pt的浓度范围为205至1445ng g -1 ,而Pt的浓度范围为201至1230ng g -1 for Pd。<!-fig ft0-> <!-fig @ position =“ anchor” mode = article f4-> <!-fig mode =“ anchored” f5-> >图形摘要<!-fig / graphic | fig / alternatives / graphic mode =“ anchored” m1-> <!-标题a7->使用经季胺基官能化的介孔二氧化硅微粒(μP)从中分离铂和钯水性道路灰尘消化物。将μP直接悬浮在水性消化液中,然后使用“分散颗粒提取”分析负载分析物的μP。

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