High-performance liquid chromatography coupled with mass spectrometry for analysis of ultrasmall palladium nanoparticles

In recent studies it has been demonstrated that the privileged reactivity of higher-order metal clusters can be exploited in widely applied catalytic processes, particularly cross-coupling reactions and hydrogenative transformations. Relatively small, well-defined Pd n clusters have been known since the 1960s. Unique reactivity, reaction (product) selectivity, and catalyst behavior have been recently uncovered, from which there is much potential in catalyst design and application. Ligated Pd n clusters of a smaller size (where n is less than 6) may form upon degradation of mononuclear Pd species en route to larger particulate Pd (from <5 nm particles to large moribund forms in the >1 μm range). This review presents the catalytic applications of Pd n clusters. We pay particular attention to the underlying structure of the Pd n clusters, linked to their reactivity. A hypothesis that ligated Pd n clusters may constitute a mechanism by which higher-order Pd species may form (as a bridging point for monoligated Pd species through to PdNPs) is further discussed. Where appropriate, we mention other catalytic reaction processes that complement the discussion focused on cross-coupling and hydrogenation processes.

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“…. Choi et al employed an LC-MS method to detect small Pd clusters stabilized by DMF (Pd 10 –Pd 20 ; <3 nm) …”

Section: Catalytic Activity Of Pd N Speciesmentioning

confidence: 91%

Well-Defined Pd_n Clusters for Cross-Coupling and Hydrogenation Catalysis: New Opportunities for Catalyst Design

2022

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“…It is further anticipated that RP-HPLC combined with MS can be applied to investigate the growth mechanism of Pd NPs. 216 Resonant mass measurement microelectro-mechanical system (RMM-MEMS) is a technique used to detect and count subvisible and sub-micron particles in a material, and to measure their size and mass and the distributions of these properties. A micro electro-mechanical system (MEMS) sensor, containing a resonating cantilever with a microfluidic channel embedded in its surface, is employed.…”

Section: X-ray-based Techniquesmentioning

confidence: 99%

Characterization techniques for nanoparticles: comparison and complementarity upon studying nanoparticle properties

2018

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Nanostructures have attracted huge interest as a rapidly growing class of materials for many applications. Several techniques have been used to characterize the size, crystal structure, elemental composition and a variety of other physical properties of nanoparticles. In several cases, there are physical properties that can be evaluated by more than one technique. Different strengths and limitations of each technique complicate the choice of the most suitable method, while often a combinatorial characterization approach is needed. In addition, given that the significance of nanoparticles in basic research and applications is constantly increasing, it is necessary that researchers from separate fields overcome the challenges in the reproducible and reliable characterization of nanomaterials, after their synthesis and further process (e.g. annealing) stages. The principal objective of this review is to summarize the present knowledge on the use, advances, advantages and weaknesses of a large number of experimental techniques that are available for the characterization of nanoparticles. Different characterization techniques are classified according to the concept/group of the technique used, the information they can provide, or the materials that they are destined for. We describe the main characteristics of the techniques and their operation principles and we give various examples of their use, presenting them in a comparative mode, when possible, in relation to the property studied in each case.

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“…Herein, we describe only the results of our research. However, more detail on work in this field by other research groups, such as the Murray group, 147,246,255,284,285,471,567,579,580,602,850 Choi group, 157,236,466,710 Bürgi group, 67,235,341,505,556,711720,864,915 and Whetten group, 338,707,910913 can be found elsewhere. In Sections 4.14.3, we first describe a research example of metal clusters having hydrophobic ligands (hereinafter referred to as hydrophobic metal clusters), and in Section 4.4, an example concerning metal clusters protected by hydrophilic ligands (hereinafter referred to as hydrophilic metal clusters) is described.…”

Section: Separations Achieved and Information Obtained By Hplcmentioning

confidence: 99%

Deepening the Understanding of Thiolate-Protected Metal Clusters Using High-Performance Liquid Chromatography

Niihori

Yoshida

Hossain

et al. 2018

Bulletin of the Chemical Society of Japan

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He received his Ph.D. degree in chemistry in 2001 under the supervision of Prof. Atsushi Nakajima from Keio University. Before joining Tokyo University of Science in 2008, he was employed as an assistant professor at Keio University and at the Institute for Molecular Science (IMS). His current research interests include the precise synthesis of stable and functionalized metal nanoclusters and their applications in energy and environmental materials. Yoshiki Niihori Yoshiki Niihori was born in Ibaraki, Japan, in 1986. He was a postdoctoral researcher in the Negishi group at Tokyo University of Science and is currently assistant professor at Rikkyo University. He received his B.Sc. (2009), M.Sc. (2011), and Ph.D. (2014) degrees in chemistry from Tokyo University of Science. His research interests include the development of precise synthesis methods for noble metal nanoclusters based on highperformance liquid chromatography. Kana Yoshida Kana Yoshida was born in Tokyo, Japan, in 1994. She is currently a master's degree student in the Negishi group at Tokyo University of Science. She received her B.Sc. (2017) in chemistry from Tokyo University of Science. Her research interests include the development of high-resolution separation methods for noble metal nanoclusters.

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High-performance liquid chromatography coupled with mass spectrometry for analysis of ultrasmall palladium nanoparticles

Cited by 10 publications

References 62 publications

Well-Defined Pd_n Clusters for Cross-Coupling and Hydrogenation Catalysis: New Opportunities for Catalyst Design

Well-Defined Pd_n Clusters for Cross-Coupling and Hydrogenation Catalysis: New Opportunities for Catalyst Design

Characterization techniques for nanoparticles: comparison and complementarity upon studying nanoparticle properties

Deepening the Understanding of Thiolate-Protected Metal Clusters Using High-Performance Liquid Chromatography

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High-performance liquid chromatography coupled with mass spectrometry for analysis of ultrasmall palladium nanoparticles

Cited by 10 publications

References 62 publications

Well-Defined Pdn Clusters for Cross-Coupling and Hydrogenation Catalysis: New Opportunities for Catalyst Design

Well-Defined Pdn Clusters for Cross-Coupling and Hydrogenation Catalysis: New Opportunities for Catalyst Design

Characterization techniques for nanoparticles: comparison and complementarity upon studying nanoparticle properties

Deepening the Understanding of Thiolate-Protected Metal Clusters Using High-Performance Liquid Chromatography

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Product

Resources

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Well-Defined Pd_n Clusters for Cross-Coupling and Hydrogenation Catalysis: New Opportunities for Catalyst Design

Well-Defined Pd_n Clusters for Cross-Coupling and Hydrogenation Catalysis: New Opportunities for Catalyst Design