NDLI: Evolved gas analyses on a mixed valence copper(I,II) complex salt with thiosulfate and ammonia by in situ TG-EGA-FTIR and TG/DTA-EGA-MS

Content Provider	Springer Nature Link
Author	Madarász, Jás
Copyright Year	2009
Abstract	Thermal decomposition of a mixed valence copper salt, Na$_{4}$[Cu(NH$_{3}$)$_{4}$][Cu(S$_{2}$O$_{3}$)$_{2}$]$_{2}$·0.5NH$_{3}$ (1) prepared from pentahydrates of sodium thiosulfate and copper sulphate of various molar ratios in 1:1 v/v aqueous ammonia solution, has been studied up to 1,000 °C in flowing air by simultaneous thermogravimetric and differential thermal analysis coupled online with quadrupole mass spectrometer (TG/DTA-MS) and FTIR spectrometric gas cell (TG-FTIR), in comparison. Compound 1 releases first but very slowly some of the included ammonia till 170 °C, then simultaneously ammonia (NH$_{3}$) and sulphur dioxide (SO$_{2}$) from 175 to 225 °C, whilst the evolution of SO$_{2}$ from thiosulfate ligands continues in several overlapping stages until 410 °C, and is escorted by explicit exothermic heat effects at around 237, 260, 358 and 410 °C. The former two exothermic DTA-peaks correspond to the simultaneous degradation and air oxidation processes of excess thiosulfate anions not reacted by formation of copper sulfides (both digenite, Cu$_{1.8}$S and covellite, CuS, checked by XRD) and sodium sulfate, while the last two exothermic peaks are accompanied also by considerable mass gains, as the result of two-step oxidation of copper sulfides into various oxosulfates. The mass increase continues further on until 580 °C, when the sample mass begins to decrease slowly, as a continuous decomposition of the intermediate copper oxosulfates, indicated also by re-evolution of SO$_{2}$. At 1,000 °C, a residual mass value of 64.3% represents a stoichiometric formation of Cu$^{II}$O and anhydrous Na$_{2}$SO$_{4}$.
Starting Page	111
Ending Page	116
Page Count	6
File Format	PDF
ISSN	13886150
Journal	Journal of thermal analysis
Volume Number	97
Issue Number	1
e-ISSN	15728943
Language	English
Publisher	Springer Netherlands
Publisher Date	2009-08-06
Publisher Place	Dordrecht
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Evolved gas analysis (EGA) Mass spectrometry (MS) FTIR-spectroscopic gas cell Simultaneous thermogravimetry and differential thermal analysis (TG/DTA) Mixed valence copper(II) and (I) complex Formation of SO$_{2}$ and NH$_{3}$ Digenite Covellite Copper(II)-oxo-sulfates Measurement Science and Instrumentation Inorganic Chemistry Polymer Sciences Analytical Chemistry Physical Chemistry
Content Type	Text
Resource Type	Article
Subject	Physical and Theoretical Chemistry Condensed Matter Physics

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