Mass spectrometric determination of kinetic parameters for solid state decomposition reactions. Part 1. Method; calcium oxalate decomposition

Price, Dennis; Dollimore, D.; Fatemi, Navid S.; Whitehead, R.

doi:10.1016/0040-6031(80)85093-3

Cited by 52 publications

(22 citation statements)

References 14 publications

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“…Minor difficulties may arise from the possibility that calcium oxalate crystals form over a long period of time while the tree is living, and possibly undergo some isotopic exchange during this period. More significantly, it is conceivable that there is an exchange of CO molecules between the wood ash and the air during the combustion process (Price et al 1980). A high-temperature exchange process between CO 2 and bone mineral is suspected to occur for cremated bones (Zazzo et al 2009).…”

Section: Introductionmentioning

confidence: 99%

Radiocarbon Concentrations of Wood Ash Calcite: Potential for Dating

et al. 2011

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ABSTRACT. Ash is formed when plant calcium oxalate crystals (CaC 2 O 4 ) decompose to form calcite (CaCO 3 ). We found that ash does retain the original calcium oxalate radiocarbon concentration, but in addition, there is another minor 14 C source. This is shown by the presence of a consistent small shift in the pMC and  13 C levels when comparing cellulose and ash from modern and archaeological woods. Possible mechanisms for 14 C exchange during combustion or due to diagenesis are considered in order to define parameters for identifying better-preserved wood ash samples.

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Section: Introductionmentioning

confidence: 99%

Radiocarbon Concentrations of Wood Ash Calcite: Potential for Dating

et al. 2011

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“…A large number of gas analytical techniques like gas chromatography (Jemal and Khattech 1989), Fourier transform infrared spectroscopy (FT-IR) (Mullens et al 1992) and mass spectrometry (MS) (Price et al 1980;Barnes 1987) and sometimes combination of more than one of the above (Mullens et al 1997) are used for interfacing with TGA. However, mass spectrometry is a preferred choice for the analysis of evolved gases because of its *Author for correspondence advantages like high specificity, sensitivity, fast response, low detection limits, multiple ion and isotope detection capability.…”

Section: Introductionmentioning

confidence: 99%

Thermogravimetry-evolved gas analysis-mass spectrometry system for materials research

et al. 2003

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Abstract. Thermal analysis is a widely used analytical technique for materials research. However, thermal analysis with simultaneous evolved gas analysis describes the thermal event more precisely and completely. Among various gas analytical techniques, mass spectrometry has many advantages. Hence, an ultra high vacuum (UHV) compatible mass spectrometry based evolved gas analysis (EGA-MS) system has been developed. This system consists of a measurement chamber housing a mass spectrometer, spinning rotor gauge and vacuum gauges coupled to a high vacuum, high temperature reaction chamber. A commercial thermogravimetric analyser (TGA: TG + DTA) is interfaced to it. Additional mass flow based gas/vapour delivery system and calibration gas inlets have been added to make it a versatile TGA-EGA-MS facility. This system which gives complete information on weight change, heat change, nature and content of evolved gases is being used for (i) temperature programmed decomposition (TPD), (ii) synthesis of nanocrystalline materials, (iii) gas-solid interactions and (iv) analysis of gas mixtures. The TPD of various inorganic oxyanion solids are studied and reaction intermediates/products are analysed off-line. The dynamic operating conditions are found to yield nanocrystalline products in many cases. This paper essentially describes design features involved in coupling the existing EGA-MS system to TGA, associated fluid handling systems, the system calibration procedures and results on temperature programmed decomposition. In addition, synthesis of a few nanocrystalline oxides by vacuum thermal decomposition, gas analysis and potential use of this facility as controlled atmosphere exposure facility for studying gas-solid interactions are also described.

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“…(b) there is a non‐baseline‐corrected O 2 ( m/z 32) signal which is non‐zero throughout the run except during evolution of CO. During the evolution of CO the O 2 signal drops to undetectable limits, and we get a rise in CO 2 , an indication that reaction is occurring. It has also been noted previously that reaction can also occur when the system is not under vacuum.…”

Section: Resultsmentioning

confidence: 99%

“…Decomposition analysis was performed by decomposing 16.5 mg CaC 2 O 4 •H 2 O in a helium atmosphere. This system has been shown to be a good standard for TG, [19] but has also been studied previously by TG-MS. [19,20] The sample was heated from room temperature to 1000 C at a rate of 20 C/min with the transfer line heated to 200 C while the evolved gases were monitored by MS.…”

Section: Methodsmentioning

confidence: 99%

Simple, inexpensive mass spectrometric analyzer for thermogravimetry

Selck

Woodfield

Boerio‐Goates

et al. 2012

Rapid Comm Mass Spectrometry

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A low-cost mass spectrometer attachment for thermogravimetric analysis has been constructed from readily available commercial instruments and components. The benefits of this set-up include excellent mass-flow repeatability, simple design, and significantly lower adoption cost as opposed to ready-built commercial solutions. The inclusion of an open source software package allows semi-automated, highly simplified data analysis. The results from the instrument show excellent sensitivity for small volumes of evolved gas, as well as highly reproducible signal strengths. The GUI-based software package provides data analysis in a way that is very intuitive and that can be easily modified to work with a broad range of TG instruments.

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Mass spectrometric determination of kinetic parameters for solid state decomposition reactions. Part 1. Method; calcium oxalate decomposition

Cited by 52 publications

References 14 publications

Radiocarbon Concentrations of Wood Ash Calcite: Potential for Dating

Radiocarbon Concentrations of Wood Ash Calcite: Potential for Dating

Thermogravimetry-evolved gas analysis-mass spectrometry system for materials research

Simple, inexpensive mass spectrometric analyzer for thermogravimetry

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