Mass Spectral Studies of Binuclear Metal Complexes: Copper(I) Carboxylates

Lin, Denis C. K.; Westmore, John B.

doi:10.1139/v73-446

Cited by 35 publications

(6 citation statements)

References 24 publications

(36 reference statements)

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“…Metal acetates are useful reagents, particularly in organic synthesis [1] and in the preparation of some industrially important metal and metal oxide catalysts [2]. The thermal decomposition of acetates under various conditions, has attracted attention owing to its importance in several fields of research, in solidstate and surface chemistry and catalysis [1,[3][4][5][6][7].…”

Section: Introductionmentioning

confidence: 99%

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Thermoanalytical investigations of the decomposition course of copper oxysalts

Mansour

1996

Journal of Thermal Analysis

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The thermal decomposition course of copper acetate monohydrate (CuAe) was examined on heating up to 600~ at various rates, by TG, DTA and DSC. Non-isothermal kinetic and thermodynamic parameters were determined in air or nitrogen. SEM was used to describe the decomposition course and the solid products were identified by IR and XRD analysis. The results indicated that CuAc was dehydrated at 190~ and then partially decomposed at 220~ giving rise to CuO in addition to a minor portion of CuzO and Cu403. The last two oxides seemed to faeilirate the decomposition of the rest of the anhydrous acetate. Cu20 and Cu403 were oxidized in air at >400~ in a process that did not occur in nitrogen.

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Section: Introductionmentioning

confidence: 99%

“…The thermal decomposition of acetates under various conditions, has attracted attention owing to its importance in several fields of research, in solidstate and surface chemistry and catalysis [1,[3][4][5][6][7].…”

Section: Introductionmentioning

confidence: 99%

Thermoanalytical investigations of the decomposition course of copper oxysalts

Mansour

1996

Journal of Thermal Analysis

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“…Two strategies could be proposed: continuous sampling coupled with fast analytical technique on one hand and in situ spectroscopic analysis on the other hand. Both approaches are complementary.Metal carboxylates are useful reagents particularly for organic synthesis [3] and applied in several fields of research as solid-state, surface chemistry and catalysis [3] [4] [5] [6]. The thermal decomposition of metal carboxylates is a feasible route to synthesize metal nanoparticles suitable for catalytic purposes [7] [8]…”

mentioning

confidence: 99%

“…Metal carboxylates are useful reagents particularly for organic synthesis [3] and applied in several fields of research as solid-state, surface chemistry and catalysis [3] [4] [5] [6]. The thermal decomposition of metal carboxylates is a feasible route to synthesize metal nanoparticles suitable for catalytic purposes [7] [8]…”

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confidence: 99%

“…Cho and co [21]. made infrared characterization of Cu-CH3 and listed 4 main bands at 1612 (Cu-H stretching in CH 3 -CuH − ), 1203 (CH 3 deform in CH 3 -Cu), 1012 (CH 3 deform in CH 3 -CuH − ) and 648 cm −1 . Corresponding bands at 1611, 1198, 1011 and 655 cm −1 were identified on DRIFT spectra (Figure 5(b) and Figure 6(b)) and appeared between 315 and 367˚C under Ar.…”

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Forward Looking Analysis Approach to Assess Copper Acetate Thermal Decomposition Reaction Mechanism

Youssef¹,

Sall²,

Dintzer³

et al. 2019

AJAC

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Thermal decomposition course of copper acetate monohydrate was monitored by combining diffuse reflectance infrared Fourier transform spectroscopy (DRIFT) coupled with µ gas chromatography-mass spectrometry (µGC-MS) with other analytical techniques (thermogravimetry analysis and in situ X-ray diffraction). Non-isothermal kinetic was examined in air and Ar.A complete analysis of the evolution of infrared spectra matched with crystalline phase transition data during the course of reaction allows access to significant and accurate information about molecular dynamics. While thermogravimetry gives broad conclusion about two steps reaction (dehydration and decarboxylation), in line approach (in situ X-ray and in situ DRIFT coupled to µGC-MS) is proposed as an example of a new robust and forward-looking analysis. While decomposition mechanism of copper acetate monohydrate is still not well elucidated yet previously, the present in-line characterization results lead to accurate data making the corresponding mechanism explicit. techniques able to analyze data about different reaction media: powder, solid, liquid and gases. Two strategies could be proposed: continuous sampling coupled with fast analytical technique on one hand and in situ spectroscopic analysis on the other hand. Both approaches are complementary.Metal carboxylates are useful reagents particularly for organic synthesis [3] and applied in several fields of research as solid-state, surface chemistry and catalysis [3] [4] [5] [6]. The thermal decomposition of metal carboxylates is a feasible route to synthesize metal nanoparticles suitable for catalytic purposes [7] [8]

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Electron impact mass spectra of some salts of carboxylic acids with alkali (group Ia) metals

White¹

1978

Org. Mass Spectrom.

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Thirteen of the salts of the alkali metals (Li, Na, K, Rb, Cs) with acetic, 2,2-dimethylpropionic, trifluoroacetic and heptafluorobutyric acid have been found to be sufficiently volatile to give mass spectra under normal electron impact conditions. The metal containing ions observed include ( Electron impact mass spectra have been observed for a number of organo derivatives of the alkali (Group Ia) metals, including ethyllithiurn,' lithiomethyltrimethylsilane,' lithium' and potassium" t-butoxide, 1,3-diketone chelates; and some N-alkyl and N,Ndialkyldithio~arbamates.~ The carboxylate salts have generally been assumed to be insufficiently volatile to give electron impact spectra and have therefore been studied by other techniques such as radio frequency spark source6 and field desorption7.' mass spectrometry even though studies on cuprousg and argentous" (Group Ib) carboxylates have appeared. The reported exceptions are a mention of the similarity of the electron impact and field desorption spectra of sodium acetate by Schulten and Beckey' and the interesting studies by Chamberlin and Agtarap" on the sodium, potassium and rubidium salts of Monensin and related antibiotics in which the metal atom is coordinated by oxygen atoms within the molecule in a way very similar to the crown ether complexes. The spectrum of potassium benzoate under chemical ionization conditions using a field desorption emitter as a solid probe has also been reported."We have examined the behavior under normal electron impact conditions of the salts of the five alkali metals with four simple carboxylic acids chosen to maximize the volatility of the salts and to be representative of acids which may be present after the processing of biological samples. When metal containing ions were observed, the temperature is that required for an intense spectrum. Relative intensities changed somewhat during the course of the evaporation of the sample. RESULTS AND DISCUSSION Volatility and decomposition" Decomposition began at the indicated temperature. No metal containing ions were observed. decompose cleanly to give CO, and C,F,, and the trifluoroacetates decompose to give COz and material with a spectrum similiar to that of mixed perfluoroalkanes. In all cases, a white residue remains which is assumed to be the metal fluoride. This is supported in the case of the cesium salts by the observation of the spectrum of cesium fluoride when the residue is heated to 400°C.For all the acetates except potassium acetate (the least volatile), for all the 2,2-dirnethylpropionates7 and for lithium heptafluorobutyrate the spectrum was independent of the rate of heating and remained unchanged throughout evaporation of the entire sample, thus strongly indicating that these salts volatilize without decomposition. The temperatures needed are surprisingly low with vaporization occurring within or only modestly above the temperature range generally used for nonionic compounds. As expected, the temperatures required to volatilize the salts decrease when the bulky less polar 2...

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Mass Spectral Studies of Binuclear Metal Complexes: Copper(I) Carboxylates

Cited by 35 publications

References 24 publications

Thermoanalytical investigations of the decomposition course of copper oxysalts

Thermoanalytical investigations of the decomposition course of copper oxysalts

Forward Looking Analysis Approach to Assess Copper Acetate Thermal Decomposition Reaction Mechanism

Electron impact mass spectra of some salts of carboxylic acids with alkali (group Ia) metals

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