{"title":"Decoding Voltammograms at the Molecular Frontier: Integration of Voltammetry and Mass Spectrometry","authors":"Adarsh Koovakattil Surendran, Jana Roithová","doi":"10.1002/cmtd.202400003","DOIUrl":"10.1002/cmtd.202400003","url":null,"abstract":"<p>Electrochemical reactions are better understood by gaining insight into the molecular transformations at the electrodes. This paper introduces a straightforward experimental arrangement in which the voltammetry experiment in a standard electrochemical cell integrates with online electrospray-ionization mass-spectrometry. The procedure allows for monitoring of the ions produced at the working electrode. The ionic species sampling is facilitated by a silica capillary embedded in the working electrode and connected directly to the electrospray ionization source. This integration configures real-time monitoring of the ions produced at the working electrode, enhancing our knowledge of the electrochemical process. The methodology is thoroughly described and exemplified by monitoring the reactive intermediates and products that arise during the electrochemical oxidation of carbazole. This design provides an opportunity to study intermediates in electrochemical reactions with advanced mass spectrometry methods such as ion mobility separation or ion spectroscopy.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"4 6","pages":""},"PeriodicalIF":6.1,"publicationDate":"2024-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202400003","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140742907","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Non-Conventional Methodologies for the Synthesis of N-Nitrosamines","authors":"Rojan Ali, Campbell S. Wolfe, Prof. Thomas Wirth","doi":"10.1002/cmtd.202300053","DOIUrl":"10.1002/cmtd.202300053","url":null,"abstract":"<p><i>N</i>-Nitrosamines acting as contaminants in our environment is a topic of increasing concern. Detection methods are required, necessitating analytical standards. Herein, we discuss some conventional methodologies to prepare <i>N</i>-nitrosamines and compare them with unconventional pathways towards their synthesis. These methods are often more environmentally benign and safer.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"4 4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202300053","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140266892","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dr. Karla A. Erickson, Dr. Stephen S. Parker, Dr. Marisa J. Monreal
{"title":"Thermal Elimination of Pyridine from a Uranium Trichloride Precursor","authors":"Dr. Karla A. Erickson, Dr. Stephen S. Parker, Dr. Marisa J. Monreal","doi":"10.1002/cmtd.202300052","DOIUrl":"10.1002/cmtd.202300052","url":null,"abstract":"<p>Renewed interest in advanced nuclear reactors, such as Molten Salt Reactors (MSRs), has spurred studies in actinide halide chemistry and property measurements. Several proposed research-scale and commercial MSR designs incorporate uranium trichloride (UCl<sub>3</sub>) fuel. There are relatively few preparations for isolated actinide halides reported in the literature, therefore novel methods for the isolation of pure material are desired. This communication describes the thermal elimination of pyridine (py) from the coordination complex UCl<sub>3</sub>py<sub>2</sub> to yield gram-scale quantities of UCl<sub>3</sub>. The purity of the UCl<sub>3</sub> product was determined through powder X-ray Diffractometry (pXRD) and Elemental Analysis (EA).</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"4 5","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202300052","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140091135","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dr. Jiaqi Shen, Guanwei Zhou, Prof. Dr. Wenjing Wang
{"title":"Chemogenetic Tools in Focus: Proximity, Conformation, and Sterics","authors":"Dr. Jiaqi Shen, Guanwei Zhou, Prof. Dr. Wenjing Wang","doi":"10.1002/cmtd.202300051","DOIUrl":"10.1002/cmtd.202300051","url":null,"abstract":"<p>Chemogenetic tools are genetically encoded systems regulated by user-defined chemicals. Their ability to temporally modulate protein functions in specific cell populations has facilitated in-depth understanding of dynamic biological systems. Many chemogenetic domains have been developed for regulating a wide range of biological processes, ranging from cellular events to animal behaviors. These tools share some common mechanisms, including proximity regulation, conformational change and allosteric control, as well as steric hinderance control. Here in this review, we aim to provide an overview of different chemogenetic tool designs that utilize the above three common mechanisms to control cellular events.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"4 6","pages":""},"PeriodicalIF":6.1,"publicationDate":"2024-02-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202300051","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140417031","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
H. A. Suarez Orduz, S.-L. Heck, Dr. P. Dolcet, Dr. Y. Watier, Dr. M. Casapu, Prof. Dr. J.-D. Grunwaldt, Dr. P. Glatzel
{"title":"Versatile Spectroscopic Cell for Operando Studies in Heterogeneous Catalysis Using Tender X-ray Spectroscopy in Fluorescence Mode","authors":"H. A. Suarez Orduz, S.-L. Heck, Dr. P. Dolcet, Dr. Y. Watier, Dr. M. Casapu, Prof. Dr. J.-D. Grunwaldt, Dr. P. Glatzel","doi":"10.1002/cmtd.202300044","DOIUrl":"10.1002/cmtd.202300044","url":null,"abstract":"<p>The design and commissioning of a cell suitable for <i>operando</i> studies using high-energy-resolution fluorescence-detected X-ray absorption near-edge structure (HERFD-XANES) spectroscopy in the tender X-ray regime is reported. The cell is optimized for measurements within the energy range of 1.5 keV to 4.5 keV. It has a plug-flow geometry and can be used for sieved powder samples, analogous to reactors employed for laboratory tests. The functionality of the spectroscopic cell is demonstrated in the area of emission control using CO oxidation as target reaction over 1 wt.% Rh/γ-Al<sub>2</sub>O<sub>3</sub> as catalyst. We show how HERFD-XANES at the Rh L<sub>3</sub>-edge captures variations in the noble metal structure resulting from the interaction with the support material and reactant molecules. Moreover, distinct structural changes were identified along the catalyst bed as a function of temperature and local gas mixture.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"4 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-01-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202300044","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139618687","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}