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Large Temperature-Jump and Nanosecond Hyperquenching for Time-Resolved Structural Studies 时间分辨结构研究中的大温度跃变和纳秒超淬火
Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2023-01-04 DOI: 10.1002/cmtd.202200050
Dr. Alexey V. Cherepanov, Prof. Dr. Harald Schwalbe
{"title":"Large Temperature-Jump and Nanosecond Hyperquenching for Time-Resolved Structural Studies","authors":"Dr. Alexey V. Cherepanov,&nbsp;Prof. Dr. Harald Schwalbe","doi":"10.1002/cmtd.202200050","DOIUrl":"10.1002/cmtd.202200050","url":null,"abstract":"<p>The quest for atomic structures of microsecond reaction intermediates is at the frontline of modern biochemistry. Currently, there is a clear lack of experimental methods for preparing necessary time-resolved samples. Here, we report the development of a single-turnover technique for nanosecond initiation and suspension of biomolecular reactions with kinetic resolution in the microsecond time domain. Reactions can be started by large temperature-jump or direct mixing and arrested by hyperquenching in liquid cryogen at a target temperature of 77 K. Diverse morphology of nanoscale glassy bodies feature among others thin field-of-view plane sheets that can be used for structure analyses of freeze-trapped macromolecules by transmission electron cryomicroscopy. We also report the ultra-high vacuum sublimation at 77 K – a novel method for concentrating reaction intermediates for structural studies by low-temperature techniques.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"3 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202200050","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47793688","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}
引用次数: 1
Cover Picture: Following Cu Microstructure Evolution in CuZnO/Al2O3(−Cs) Catalysts During Activation in H2 using in situ XRD and XRD-CT (Chem. Methods 1/2023) 封面图片：CuZnO/Al2O3（−Cs）催化剂在H2中活化过程中的Cu微观结构演变 原位XRD和XRD-CT（化学方法1/2023）
Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2022-12-21 DOI: 10.1002/cmtd.202200078
Dr. Daniela M. Farmer, Dr. Simon D. M. Jacques, Dr. David Waller, Dr. Sara Boullosa Eiras, Dr. Kanak Roy, Dr. Georg Held, Prof. Gopinathan Sankar, Prof. Andrew M. Beale
{"title":"Cover Picture: Following Cu Microstructure Evolution in CuZnO/Al2O3(−Cs) Catalysts During Activation in H2 using in situ XRD and XRD-CT (Chem. Methods 1/2023)","authors":"Dr. Daniela M. Farmer,&nbsp;Dr. Simon D. M. Jacques,&nbsp;Dr. David Waller,&nbsp;Dr. Sara Boullosa Eiras,&nbsp;Dr. Kanak Roy,&nbsp;Dr. Georg Held,&nbsp;Prof. Gopinathan Sankar,&nbsp;Prof. Andrew M. Beale","doi":"10.1002/cmtd.202200078","DOIUrl":"https://doi.org/10.1002/cmtd.202200078","url":null,"abstract":"<p><b>The Front Cover</b> shows how X-rays can be used to obtain spatially resolved chemical imaging insight from within an industrial catalytic reactor. Understanding how the microstructure of the active Cu<sup>0</sup> component in the commercially applicable Cu/ZnO/Al<sub>2</sub>O<sub>3</sub>(−Cs<sub>2</sub>O) low-temperature water-gas shift catalyst evolves under various H<sub>2</sub> partial pressures in the presence/absence of a Cs promoter during thermal activation has been the subject of the present investigation. More information can be found in the Research Article by Daniela M. Farmer et al..\u0000 <figure>\u0000 <div><picture>\u0000 <source></source></picture><p></p>\u0000 </div>\u0000 </figure>\u0000 </p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"3 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-12-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202200078","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"50139790","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}
引用次数: 0
Following Cu Microstructure Evolution in CuZnO/Al2O3(−Cs) Catalysts During Activation in H2 using in situ XRD and XRD-CT CuZnO/Al2O3（−Cs）催化剂在H2中活化过程中Cu微观结构的演变 原位XRD和XRD-CT
Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2022-12-21 DOI: 10.1002/cmtd.202200077
Dr. Daniela M. Farmer, Dr. Simon D. M. Jacques, Dr. David Waller, Dr. Sara Boullosa Eiras, Dr. Kanak Roy, Prof. Georg Held, Prof. Gopinathan Sankar, Prof. Andrew M. Beale
{"title":"Following Cu Microstructure Evolution in CuZnO/Al2O3(−Cs) Catalysts During Activation in H2 using in situ XRD and XRD-CT","authors":"Dr. Daniela M. Farmer,&nbsp;Dr. Simon D. M. Jacques,&nbsp;Dr. David Waller,&nbsp;Dr. Sara Boullosa Eiras,&nbsp;Dr. Kanak Roy,&nbsp;Prof. Georg Held,&nbsp;Prof. Gopinathan Sankar,&nbsp;Prof. Andrew M. Beale","doi":"10.1002/cmtd.202200077","DOIUrl":"https://doi.org/10.1002/cmtd.202200077","url":null,"abstract":"<p>Invited for this month's cover is the group of Andrew M. Beale at the University College London and at the Research Complex at Harwell (UK). The cover picture demonstrates how X-rays can be used to obtain spatially resolved chemical imaging insight from within an industrial catalytic reactor. Understanding how the microstructure of the active Cu<sup>0</sup> component in the commercially applicable Cu/ZnO/Al<sub>2</sub>O<sub>3</sub>(−Cs<sub>2</sub>O) low-temperature water-gas shift catalyst evolves under various H<sub>2</sub> partial pressures in the presence/absence of a Cs promoter during thermal activation has been the subject of the present investigation. Read the full text of their Research Article at 10.1002/cmtd.202200015.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"3 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-12-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202200077","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"50139789","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}
引用次数: 0
Cover Picture: (Chem. Methods 12/2022) 封面图片:(化学)方法12/2022)
Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2022-12-01 DOI: 10.1002/cmtd.202200065
{"title":"Cover Picture: (Chem. Methods 12/2022)","authors":"","doi":"10.1002/cmtd.202200065","DOIUrl":"https://doi.org/10.1002/cmtd.202200065","url":null,"abstract":"<p>\u0000 <figure>\u0000 <div><picture>\u0000 <source></source></picture><p></p>\u0000 </div>\u0000 </figure>\u0000 </p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"2 12","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://chemistry-europe.onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202200065","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91784294","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}
引用次数: 0
Comment on ‘PRISMA: A robust and intuitive tool for high-throughput processing of chemical spectra’ 评论“PRISMA：一种强大而直观的化学光谱高通量处理工具”
Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2022-11-22 DOI: 10.1002/cmtd.202200013
Prof. Robert J. Meier
{"title":"Comment on ‘PRISMA: A robust and intuitive tool for high-throughput processing of chemical spectra’","authors":"Prof. Robert J. Meier","doi":"10.1002/cmtd.202200013","DOIUrl":"10.1002/cmtd.202200013","url":null,"abstract":"<p>The analysis of spectral data, and in particular the quantification of these, highly depends on curve fitting the spectra with suitable methods. The required methodologies have been known for very long. However, even today it is a regular problem that this, i.e. physically correct analyzing spectral data, is not practiced.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"2 11","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://chemistry-europe.onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202200013","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48504828","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}
引用次数: 0
Rapid Screening of Kinetic Models for Methane Total Oxidation using an Automated Gas Phase Catalytic Microreactor Platform 利用自动化气相催化微反应器平台快速筛选甲烷全氧化动力学模型
Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2022-11-11 DOI: 10.1002/cmtd.202200049
Solomon Gajere Bawa, Arun Pankajakshan, Dr. Conor Waldron, Dr. Enhong Cao, Dr. Federico Galvanin, Prof. Asterios Gavriilidis
{"title":"Rapid Screening of Kinetic Models for Methane Total Oxidation using an Automated Gas Phase Catalytic Microreactor Platform","authors":"Solomon Gajere Bawa,&nbsp;Arun Pankajakshan,&nbsp;Dr. Conor Waldron,&nbsp;Dr. Enhong Cao,&nbsp;Dr. Federico Galvanin,&nbsp;Prof. Asterios Gavriilidis","doi":"10.1002/cmtd.202200049","DOIUrl":"10.1002/cmtd.202200049","url":null,"abstract":"<p>An automated flow micropacked bed catalytic reactor platform was developed to conduct pre-planned experiments for rapid screening of kinetic models. The microreactor was fabricated using photolithography and deep reactive ion etching of a silicon wafer, with a reaction channel width and depth of 2 mm and 420 μm respectively. It was packed with ca. 10 mg of 5 wt. % Pd/Al<sub>2</sub>O<sub>3</sub> catalyst to perform methane combustion, which was the selected reaction to test the developed platform. The experimental system was monitored and controlled by LabVIEW to which Python scripts for online design of experiments and data analysis were integrated. Within each experimental campaign, the platform automatically adjusted the experimental conditions, and the analysis of the product stream was conducted by online gas chromatography. The experimental platform demonstrated the capability of identifying the most probable kinetic models amidst potential models within two days.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"3 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-11-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202200049","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44789256","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}
引用次数: 1
Easy Structural Dereplication of Natural Products by Means of Predicted Carbon-13 Nuclear Magnetic Resonance Spectroscopy Data** 利用预测碳- 13核磁共振波谱数据对天然产物进行简单的结构复制**
Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2022-11-07 DOI: 10.1002/cmtd.202200054
Stefan Kuhn, Jean-Marc Nuzillard
{"title":"Easy Structural Dereplication of Natural Products by Means of Predicted Carbon-13 Nuclear Magnetic Resonance Spectroscopy Data**","authors":"Stefan Kuhn,&nbsp;Jean-Marc Nuzillard","doi":"10.1002/cmtd.202200054","DOIUrl":"10.1002/cmtd.202200054","url":null,"abstract":"<p>The present article reports the creation and usage of a general natural product database for the structural dereplication of natural products. This database, acd_lotusv7, derives from the LOTUS natural products database as the sole source of chemical structures. Database construction also relies on the commercial “ACD/C+H Predictors and DB” software for the prediction of the carbon-13 nuclear magnetic resonance (NMR) spectral data associated with structures. The linkage of each natural compound with a Wikidata resource identifier already present in LOTUS accelerates the access to the primary literature data such as biologic origin and bibliographic references. The open source nmrshiftdb2 web interface and search engine provide a simple and free way to retrieve compound structures stored in acd_lotusv7 from carbon-13 data and to analyze search results. Dereplication is illustrated by the easy and free retrieval of the structure of three natural compounds of low, medium, and high complexity from published lists of carbon-13 NMR chemical shifts.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"3 4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202200054","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42733162","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}
引用次数: 2
Cover Picture: (Chem. Methods 11/2022) 封面图片:(化学)方法11/2022)
Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2022-11-02 DOI: 10.1002/cmtd.202200061
{"title":"Cover Picture: (Chem. Methods 11/2022)","authors":"","doi":"10.1002/cmtd.202200061","DOIUrl":"https://doi.org/10.1002/cmtd.202200061","url":null,"abstract":"<p>\u0000 <figure>\u0000 <div><picture>\u0000 <source></source></picture><p></p>\u0000 </div>\u0000 </figure>\u0000 </p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"2 11","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://chemistry-europe.onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202200061","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91806643","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}
引用次数: 0
The Mechanochemical Beckmann Rearrangement over Solid Acids: From the Ball Mill to the Extruder 固体酸的机械化学贝克曼重排:从球磨机到挤出机
Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2022-10-27 DOI: 10.1002/cmtd.202200058
Daniel M. Baier, Tilo Rensch, Desislava Dobreva, Carolina Spula, Stephen Fanenstich, Marisol Rappen, Konrad Bergheim, Dr. Sven Grätz, Prof. Dr. Lars Borchardt
{"title":"The Mechanochemical Beckmann Rearrangement over Solid Acids: From the Ball Mill to the Extruder","authors":"Daniel M. Baier,&nbsp;Tilo Rensch,&nbsp;Desislava Dobreva,&nbsp;Carolina Spula,&nbsp;Stephen Fanenstich,&nbsp;Marisol Rappen,&nbsp;Konrad Bergheim,&nbsp;Dr. Sven Grätz,&nbsp;Prof. Dr. Lars Borchardt","doi":"10.1002/cmtd.202200058","DOIUrl":"10.1002/cmtd.202200058","url":null,"abstract":"<p>Beckmann rearrangement was carried out in the solid state in a ball mill using metal oxides as solid acids. After a comprehensive investigation of different reaction parameters, acids as well as further additives, a combination of aluminosilicate materials, phosphorus pentoxide, and para-toluenesulfonic acid was identified as the optimal system. This allowed the model compounds ϵ-caprolactam and acetanilide to be obtained in yields of 46 % and 94 %, respectively, while the robustness of the method was demonstrated by applying it to additional substrates. Finally, we scaled up our optimized reaction into a continuous process using a twin screw extruder. With this, yields beyond 90 % could be achieved in a residence time as low as seven minutes.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"3 4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-10-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202200058","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46090632","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}
引用次数: 2
Beginner's Guide to Raman Spectroelectrochemistry for Electrocatalysis Study 初级指南拉曼光谱电化学电催化研究
Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2022-10-26 DOI: 10.1002/cmtd.202200042
Dr. Weiran Zheng
{"title":"Beginner's Guide to Raman Spectroelectrochemistry for Electrocatalysis Study","authors":"Dr. Weiran Zheng","doi":"10.1002/cmtd.202200042","DOIUrl":"10.1002/cmtd.202200042","url":null,"abstract":"<p>The need for continuous observation of electrocatalytic processes under operating conditions has promoted the popularity of in situ techniques coupled with electrochemical tests. In situ Raman spectrometer coupled with electrochemistry (or Raman spectroelectrochemistry) is a powerful tool to provide real-time structural information related to the dynamic electrolyte/electrode interface. To make it more accessible among the electrocatalysis community, we provide an essential experimental guideline of in situ Raman spectroelectrochemistry to beginners. After the necessary background of the technical principle and primary applications, we focus on the experimental considerations, from electrode preparation, cell design, and laser parameters to the electrochemical sequence and data process. The recent efforts to make this technique more affordable are also highlighted. We hope this review can help beginners to understand and use Raman spectroelectrochemistry.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"3 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-10-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202200042","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42020167","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}
引用次数: 5
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