DOI: 10.5281/zenodo.14066304
title: Data set from: In situ heating cell for temperature dependent transmission X-ray absorption spectroscopy (XAS) measurement with a laboratory based spectrometer

description: Abstract: In this work a compact, easy to handle, transmission heating cell for in situ XAS (X-ray absorption spectroscopy) measurement in the tender to hard x-ray regime was developed. The main focus for the cell design was to investigate so called spin crossover (SCO) complexes which show a spin-transition at certain temperatures above room temperature (RT). Therefore a high temperature stability (preferably< 0.5 °C) as well as a minimal overheating of the set point temperatures (< 1 °C) was aimed and could be achieved. The SCO sample used in this work is [Fe(bzimpy)2](ClO4)2·0.25H2O (Fe-Bzimpy-Perchlorat) and was heated up to 250 °C. Several measurment with a laboratory spectrometer and at the BL10 of the DELTA storage ring has been performed to investigate the performance and reprocuability of the cell as well as comparing different heating modes.

This data set contains the raw data of the work “In Situ heating cell for temperature dependent transmission X-ray absorption spectroscopy (XAS) measurement with a laboratory based spectrometer” This includes  the pre-characterization (FTIR-ATR and UV-Vis-spectroscopy) of the investigated sample Fe-Bzimpy-Perchlorate (Fe(bzimpy)2(ClO4)2·0.25H2O), an iron(II) complex of the ligand 2,6-Bis(benzimidazol-2-yl) pyridine (abbreviated as bzimpy). The raw and normalized data sets of the XAS measurment in the laboratory and at the BL10 of the DELTA storage ring, the temperature profile data corresponding to the the XAS measurments and the data of the performance of the heating cell is included in this data set.

Information on data sets

XAS - This folder contains the XAS spectra of three different in situ measurments of the sample Fe-Bzimpy-Perchlorate, which are seperated in three sup-folders. Two folders are the measurments done at the BL10 at the DELTA storage ring, heating the sample from RT to 190 °C and from RT to 250 °C. The third folder is the measurment done with the laboratory spectrometer indicated with "LabXAFS" in the folder name. This in situ measurment was from RT to 220 °C. Each supfolder contains the raw and normalized data. For the laboratory measurment the data for each temperature is in one data file for the normalized and the raw data set. For the supfolder corresponding to the BL10 measurments, the raw data is in another supfolder "specs_raw" with each spectrum having their own data file. The normalized data is in seperate files e.g. "3-19_norm.dat" which contains the normalized data of nourmeres spectra indicted by the file name. Each folder of the three subolders contains a txt file "spec-t_meas_assignment_.....txt" which gives the average temprature for the corrsponding spectrum (spec). For the laboratory measurments the spectra are also named in the header of the files with the corresponding averaged temperature.

pre-chracterization - This folder contains the FTIR-ATR and the UV-Vis measurments of the sample Fe-Bzimpy-Perchlorate, which was the pre-chracterization of the sampel as a quality controll. 

temperature-profiles - This folder contains the temepratures profiles (t_set and t_meas) of the Insitu measurments in the XAS folder and the further performance measurments of the heating cell.

 

Addtionally to the three main folder the file heating-cell-temperature.distribution.xlsx contain the data of the study of the temeprature distribution in the cell.