start-ver=1.4 cd-journal=joma no-vol=29 cd-vols= no-issue=5 article-no= start-page=2150 end-page=2156 dt-received= dt-revised= dt-accepted= dt-pub-year=2017 dt-pub=20170302 dt-online= en-article= kn-article= en-subject= kn-subject= en-title= kn-title=Real-Time, in Situ Monitoring of the Oxidation of Graphite: Lessons Learned en-subtitle= kn-subtitle= en-abstract= kn-abstract= Graphite oxide (GO) and its constituent layers (i.e., graphene oxide) display a broad range of functional groups and, as such, have attracted significant attention for use in numerous applications. GO is commonly prepared using the gHummers methodh or a variant thereof in which graphite is treated with KMnO4 and various additives in H2SO4. Despite its omnipresence, the underlying chemistry of such oxidation reactions is not well understood and typically affords results that are irreproducible and, in some cases, unsafe. To overcome these limitations, the oxidation of graphite under Hummers-type conditions was monitored over time using in situ X-ray diffraction and in situ X-ray absorption near edge structure analyses with synchrotron radiation. In conjunction with other atomic absorption spectroscopy, UV?vis spectroscopy and elemental analysis measurements, the underlying mechanism of the oxidation reaction was elucidated, and the reaction conditions were optimized. Ultimately, the methodology for reproducibly preparing GO on large scales using only graphite, H2SO4, and KMnO4 was developed and successfully adapted for use in continuous flow systems. en-copyright= kn-copyright= en-aut-name=MorimotoNaoki en-aut-sei=Morimoto en-aut-mei=Naoki kn-aut-name= kn-aut-sei= kn-aut-mei= aut-affil-num=1 ORCID= en-aut-name=SuzukiHideyuki en-aut-sei=Suzuki en-aut-mei=Hideyuki kn-aut-name= kn-aut-sei= kn-aut-mei= aut-affil-num=2 ORCID= en-aut-name=TakeuchiYasuo en-aut-sei=Takeuchi en-aut-mei=Yasuo kn-aut-name= kn-aut-sei= kn-aut-mei= aut-affil-num=3 ORCID= en-aut-name=KawaguchiShogo en-aut-sei=Kawaguchi en-aut-mei=Shogo kn-aut-name= kn-aut-sei= kn-aut-mei= aut-affil-num=4 ORCID= en-aut-name=KunisuMasahiro en-aut-sei=Kunisu en-aut-mei=Masahiro kn-aut-name= kn-aut-sei= kn-aut-mei= aut-affil-num=5 ORCID= en-aut-name=BielawskiChristopher W. en-aut-sei=Bielawski en-aut-mei=Christopher W. kn-aut-name= kn-aut-sei= kn-aut-mei= aut-affil-num=6 ORCID= en-aut-name=NishinaYuta en-aut-sei=Nishina en-aut-mei=Yuta kn-aut-name= kn-aut-sei= kn-aut-mei= aut-affil-num=7 ORCID= affil-num=1 en-affil=Graduate School of Medicine, Dentistry, and Pharmaceutical Sciences, Division of Pharmaceutical Sciences, Okayama University kn-affil= affil-num=2 en-affil=Research Core for Interdisciplinary Sciences, Okayama University kn-affil= affil-num=3 en-affil=Graduate School of Medicine, Dentistry, and Pharmaceutical Sciences, Division of Pharmaceutical Sciences, Okayama Universit kn-affil= affil-num=4 en-affil=Japan Synchrotron Radiation Research Institute (JASRI), SPring-8 kn-affil= affil-num=5 en-affil=Toray Research Center, Inc., Surface Science Laboratories kn-affil= affil-num=6 en-affil=Center for Multidimensional Carbon Materials (CMCM), Institute for Basic Science (IBS) kn-affil= affil-num=7 en-affil=Research Core for Interdisciplinary Sciences, Okayama University kn-affil= END