Evolved gas analyses on a mixed valence copper(I,II) complexsalt with thiosulfate and ammonia by in situ TG-EGA-FTIRand TG/DTA-EGA-MS

Janos Madarasz

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Evolved gas analyses on a mixed valence copper(I,II) complexsalt with thiosulfate and ammonia by in situ TG-EGA-FTIRand TG/DTA-EGA-MS

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Thermal decomposition of a mixed valencecopper salt, Na_4Cu(NH_3)_4S_2O_2_2·0.5NH_3(1) pre-pared from pentahydrates of sodium thiosulfate andcopper sulphate of various molar ratios in 1:1 v/v aqueousammonia solution, has been studied up to 1,000 ℃ inflowing air by simultaneous thermogravimetric and differ-ential thermal analysis coupled online with quadrupolemass spectrometer (TG/DTA-MS) and FTIR spectrometricgas cell (TG-FTIR), in comparison. Compound 1 releasesfirst but very slowly some of the included ammonia till170 ℃, then simultaneously ammonia (NH_3) and sulphurdioxide (SO_2) from 175 to 225℃, whilst the evolution ofSO_2from thiosulfate ligands continues in several overlap-ping stages until 410 ℃, and is escorted by explicit exo-thermic heat effects at around 237, 260, 358 and 410 ℃.The former two exothermic DTA-peaks correspond to thesimultaneous degradation and air oxidation processes ofexcess thiosulfate anions not reacted by formation of coppersulfides (both digenite, Cu _(1.8)Sand covellite, CuS, checkedby XRD) and sodium sulfate, while the last two exothermicpeaks are accompanied also by considerable mass gains, asthe result of two-step oxidation of copper sulfides intovarious oxosulfates. The mass increase continues further onuntil 580℃,when the sample mass begins to decreaseslowly, as a continuous decomposition of the intermediatecopper oxosulfates, indicated also by re-evolution of SO_2.At 1,000 ℃, a residual mass value of 64.3 represents astoichiometric formation of Cu~(II)O and anhydrous Na_2SO_4.

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来源
《Journal of thermal analysis and calorimetry》 |2009年第1期|111-116|共6页
作者
Janos Madarasz;
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作者单位

Department of Inorganic and Analytical Chemistry,Budapest University of Technology and Economics,Szt. Gellert ter 4, 1521 Budapest, Hungary;

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正文语种英语
中图分类物理化学（理论化学）、化学物理学;
关键词
Evolved gas analysis (EGA); Mass spectrometry (MS); FTIR-spectroscopic gas cell; Simultaneous thermogravimetry and differential thermalanalysis (TG/DTA); Mixed valence copper(II) and (I)complex; Formation of SO_2and NH_3; Digenite; Covellite; Copper(II)-oxo-sulfates;

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Evolved gas analyses on a mixed valence copper(I,II) complexsalt with thiosulfate and ammonia by in situ TG-EGA-FTIRand TG/DTA-EGA-MS

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