Modern methods for coupling quadrupole mass spectrometers with thermoanalyzers for temperatures up to 1500°C

doi:10.1016/0040-6031(77)85039-9

Thermochimica Acta

Volume 20, Issue 1, July 1977, Pages 45-52

https://doi.org/10.1016/0040-6031(77)85039-9 Get rights and content

Abstract

By coupling a quadrupole mass spectrometer (QMS) with a thermoanalyzer (TA), it is possible to obtain information on the gases evolving during the heating process and this combination has proved to be helpful for the interpretation of thermal processes^1–5. Necessary conditions for getting full and genuine mass spectrometric information are appropriate devices for sampling and sample tranfer, matched to the respective temperature program, atmosphere and condensation temperature and kind of evolving gases.

References (6)

H.G. Wiedemann
Thermal Analysis Proc.
(1969)
W. Dūnner et al.
Therm. Anal. Proc.
(1975)
H. Wyden et al.
Therm. Anal. Proc.
(1975)

There are more references available in the full text version of this article.

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Although thermogravimetric analysis is a powerful tool for polymer anlaysis its scope is limited as no information is obtained about the qualitative aspects of the evolved gases during polymer degradation. Both simultaneous and sequential techniques have been developed for identification of these gases and volatiles. Especially simultaneous TG-MS is a very powerful hyphenated technique combining the direct measurement of weight loss as a function of temperature with the use of a sensitive spectroscopic detector. In addition to the weight loss information, mass spectrometry permits temporal resolution of the gases that are evolved during thermal or thermo-oxidative degradation of a polymer in controlled atmospheric conditions. The characteristics of a broad variety of TG-MS instrumental solutions, which depend partly on the sample characteristics and the desired conditions of thermal degradation are considered, particularly in relation to polymer characterization.
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Synthesis and characterization of two new silica sodalites containing ethanolamine or ethylenediamine as guest species: [C<inf>2</inf>H<inf>7</inf>NO]<inf>2</inf>[Si<inf>6</inf>O<inf>12</inf>] <inf>2</inf> and [C<inf>2</inf>H<inf>8</inf>N<inf>2</inf>]<inf>2</inf>[Si<inf>6</inf>O <inf>12</inf>]<inf>2</inf>
1996, Zeolites
Two new clathrasils with sodalite structure were obtained using ethanolamine (EA) and ethylenediamine (ED), respectively, as structure-directing agents that also serve as solvents during the synthesis. Crystallization in the systems SiO₂-Na₂O-EA and SiO₂-Na₂O-ED, respectively, yields silica sodalites with each sodalite cage occupied by the corresponding organic molecule. The EA and ED molecules are the first amines that were found to direct the formation of silica sodalites. The two new silica sodalites were characterized by temperature-dependent powder X-ray diffraction, infrared and n.m.r. spectroscopy (¹H, ²⁹Si, ¹³C), thermal analysis, and differential scanning calorimetry. Their properties are discussed and compared with ethylene glycol silica sodalite.
Controlled rate evolved gas analysis: recent experimental set-up and typical results
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The equipment described is designed for the study of complex thermal decompositions. The heating of the sample is carried out under conditions of controlled transformation rate thermal analysis (CRTA) to enhance the information obtained from the computerized quadrupole gas analyser (especially, but not only, by improving the separation between steps). It operates between −20 and +1000°C. The thermolysis of hexahydrated nickel nitrate is briefly examined as an example.
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The direct coupling systems operating under vacuum and the systems in which the thermobalance works under atmospheric pressure are described in detail. In addition, the characteristics of the most widely used mass spectrometers and computer facilities are also discussed.
To illustrate the potential and limitations of this coupling, some typical cases of qualitative and quantitative applications are considered. These examples demonstrate that the coupling is used extensively for the identification of thermal degradation products, to determine their sequence of release and to resolve thermogravimetric curves. The technique is used only to a limited extent for quantitative analysis and kinetic studies.
X-ray powder diffraction crystal structure analysis and <sup>29</sup>Si, <sup>23</sup>Na MAS n.m.r. studies of nitrite sodalite, Na<inf>8</inf>[AlSiO<inf>4</inf>]<inf>6</inf> (NO<inf>2</inf>)<inf>2</inf>, at 295 K
1991, Zeolites
The crystal structure of nitrite sodalite, Na₈[AlSiO₄]₆(NO₂)₂ [space group P43n, a₀ = 893.0(1) pm], has been determined by X-ray powder diffraction data at 295 K. The aluminosilicate framework shows regular bonding with values of Si-O = 162.4(1) pm, Al-O = 174.3(1) pm, and Si-O-Al = 139.23(8)°. The ²⁹Si MAS n.m.r. chemical shift value of 85.5 ppm verifies the Si(O Al)₄ ordering of the framework constituents. The nitrite anion with the nitrogen atom located at the central position exhibits 12-fold orientational disorder within the [4⁶6⁸]-sodalite cage. The orientational disorder of the NO₂⁻ anion also affects the oxygen coordination of the sodium atoms. A considerable degree of dynamics in the oxygen coordination of the sodium atoms is suggested from ²³Na MAS n.m.r. spectra and heating X-ray powder diffraction data
The properties of salt-filled sodalites. I. Thermal decomposition reactions of hydroxoborate sodalite
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Differential scanning calorimetric investigations of tetrahydroxoborate sodalite Na₈[AlSiO₄]₆[B(OH)₄]₂ and low temperature polarization microscopic studies indicate structural phase transitions of sluggish character of different samples, covering the temperature range 270–300 K. Sodalite samples show cubic symmetry (a_o = 9.010(1) Å at 310 K) above 300 K but superstructure characteristics on single-crystal precession and Guinier powder diffraction photographs below 270 K. This pattern could be indexed to orthorhombic symmetry (a₀ = 25.510(1) Å, b₀ = 12.750(1) Å, c₀ = 9.020(1) Å at T ⩽ 270 K). Variations of the transition characteristics in the DSC curves of the species from the high temperature run (773 K) and those synthesized at 573 K are discussed.
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^☆: Presented at the 2nd Symposium of the German Society for Thermal Analysis held at the University of Konstanz from July 5–6, 1976.

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Modern methods for coupling quadrupole mass spectrometers with thermoanalyzers for temperatures up to 1500°C☆

Abstract

Thermal Analysis Proc.

Therm. Anal. Proc.

Therm. Anal. Proc.