ANEXO I This readme.txt file was generated on 2023-05-25 by Alvaro Colina Santamaría GENERAL INFORMATION 1. TITLE OF DATASET: Dataset of the work “Simultaneous Raman and reflection UV/Vis absorption spectroelectrochemistry” 2. AUTHORSHIP: Name: Sheila Hernandez Institution: Departamento de Quimica. Universidad de Burgos e-mail: shmunoz@ubu.es ORCID: 0000-0002-0466-8759 Name: Juan Victor Perales Rondon Institution: Departamento de Quimica. Universidad de Burgos e-mail: jvperales@ubu.es ORCID: 0000-0001-7182-6289 Name: Aranzazu Heras Institution: Departamento de Quimica. Universidad de Burgos e-mail: maheras@ubu.es ORCID: 0000-0002-5068-2164 Name: Alvaro Colina Institution: Departamento de Quimica. Universidad de Burgos e-mail: acolina@ubu.es ORCID: 0000-0003-0339-356X DESCRIPTION 1. DATASET LANGUAGE: English 2. KEYWORDS: Spectroelectrochemistry, surface enhanced Raman spectroscopy (SERS), Raman, ultraviolet and visible (UV/Vis), absorption, nanoparticles 3. ABSTRACT: In the present work, a new combination of Raman and ultraviolet and visible (UV/Vis) absorption spectroelectrochemistry in reflection mode is proposed. The new experimental setup allows obtaining the two kinds of spectroscopic data without interferences concomitantly with the electrochemical information. To the best of our knowledge, it is the first time to report the simultaneous obtention of electrochemical, electronic, and vibrational information in the same experiment. This new combination provides time-resolved information about the processes that are taking place on the electrode/solution interface which has significant implications in different fields of chemistry, such as modification of electrodes, studies of electrocatalytic reaction mechanisms, development of sensors, among others. Two different systems were used to demonstrate the advantages and capabilities of the brand-new technique, namely, the oxidation of potassium ferrocyanide, an out-sphere system that is usually employed in the validation of SEC techniques, and the electrochemical-surface enhanced Raman spectroscopy (EC-SERS) detection of crystal violet by in-situ formation of the silver SERS substrate, where the UV/Vis spectra were used to follow the formation of the SERS substrate, whereas the Raman response of a probe molecule was used to confirm either the formation of a nanostructured surface and to obtain the fingerprint of the molecule with a high time resolution. The brand-new experimental setup has shown to be useful, versatile, robust, compact, and easy to use for future applications. 4. DATE OF DATA COLLECTION: 2020-2022 5. DATE OF DATASET PUBLICATION: 29-05-2023 6. FUNDING: Authors acknowledge the financial support from Ministerio de Ciencia e Innovacion (No. PID2020-113154RB-C21), Ministerio de Economía, Industria y Competitividad (No. CTQ2017-83935-RAEI/FEDERUE), Junta de Castilla y Leon (No. BU297P18), and Ministerio de Ciencia, Innovacion y Universidades (No. RED2018-102412-T). J.V.P-R acknowledges Spanish Ministry of Economy, Industry, and Competitiveness for the Juan de la Cierva postdoctoral (No. FJCI-2017-32458) and the University of Alcala (No. CCG19/CC-071). S.H. thanks JCyL and European Social Fund for her predoctoral fellowship. ACCESS INFORMATION 1. LICENSE: This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/) 2. Dataset DOI: https://doi.org/10.36443/10259/7685 3. RELATED PUBLICATIONS: Article published in NanoResearch, 15 (2022) 5340-5346 (Springer) https://doi.org/10.1007/s12274-022-4137-5 METHODOLOGICAL INFORMATION SERS SEC was performed by using a customized SPELECRAMAN instrument (SPELECRAMAN, Metrohm-DropSens), which integrates a spectrophotometer, a bipotentiostat/galvanostat, and a laser source of 785 nm. Laser power in all experiments was set at 185 mW (588 W·cm-2). This instrument was connected to a reflection probe (DRP-RAMANPROBE, Metrohm-DropSens). The UV/Vis spectra were collected using a customized SPELEC instrument (SPELEC, Metrohm-DropSens). The deuterium-halogen lamp of the instrument was used as light source. Two bare optical fibers (Ocean Optics), one of 600 um in diameter to illuminate the sample and another of 400 ?m to collect the reflected light beam, were used to sample the solution/electrode interface using a three-electrode system. It should be noted that other combination of diameters could be used to obtain a reliable optical response. A notch filter of 785 nm (Edmund Optics) was used to block the laser light beam, avoiding reaching the UV/Vis spectrometer. A home-made spectroelectrochemical cell was developed and will be fully described below. All the experiments were performed in a dark Faraday case to avoid optical and electromagnetic interferences. DropView SPELEC software (Metrohm-DropSens) was used to control the instrument, which allows obtaining real-time and synchronized spectroelectrochemical data. Our group has developed, in collaboration with Metrohm-DropSens, a modification of the DropView SPELEC software to synchronize any two SPELEC instruments. In all cases the SPELECRAMAN instrument triggered the SPELEC instrument. Screen-printed electrodes (SPE: Ag-SPE, DRP-C013 and Pt-SPE, DRP-550 Metrohm-DropSens) were used for the SEC experiments. These devices consisted of a flat ceramic substrate on which a three-electrode system comprising the electrochemical cell was screen-printed. The working electrodes consisted of a circular Ag or Pt disk, with a diameter of 1.6 mm (DRP-C013) and 4 mm (DRP-550), respectively, the auxiliary electrode was made of carbon paste (DRP-C013) or Pt (DRP-550) and a Ag electrode acted as a pseudo reference electrode in the two cases. All potentials in the experiments referred to this pseudo reference electrode. All measurements were collected using DropView SPELEC software, capable of triggering the UV/Vis spectroscopic measurements and the Raman spectra collection to the electrochemical experiment by combining the two SPELEC instruments. Matlab R2018a is the software used for the treatment and analysis of the data generated. FILE OVERVIEW E01_CV_10uM_AgClO4_10mM_LiClO4_0_1M_AgSPE013_Raman_1.csv E01_CV_10uM_AgClO4_10mM_LiClO4_0_1M_AgSPE013_UVvis_1.csv E10_K4FeCN6_50mM_KNO3_1M_PtSPE5500_Raman_10mVs_1.csv E10_K4FeCN6_50mM_KNO3_1M_PtSPE5500_UVvis_10mVs_1.csv E11_AgClO4_5mM_AU_0_16mM_Ag_SPE_50mVs_Raman.csv E11_AgClO4_5mM_AU_0_16mM_Ag_SPE_50mVs_UVVis.csv DATA-SPECIFIC INFORMATION Each “.csv” experiment includes a file with a matrix that include information about time, potential, current, Raman shift and Raman intensity.