Comparative evolved gas analytical and structural study on trans-diammine-bis(nitrito)-palladium(II) and platinum(II) by TG/DTA-MS, TG-FTIR, and single crystal X-ray diffraction

J. Madarász, P. Bombicz, M. Czugler, Ferenc Réti, Gábor Kiss, G. Pokol

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13 Citations (Scopus)

Abstract

Detailed study on identification and thermal decomposition of solid title compounds 1 and 2 crystallized from the used aqueous ammonia solutions of Pd(NH3)2(NO2)2 and Pt(NH3)2(NO2)2, has been carried out. Beyond the composition of complexes 1 and 2, their trans square planar configuration have already been recognized by reference IR spectra and powder XRD patterns, nevertheless their exact molecular and crystal structure as of trans-Pd(NH3)2(NO2)2 (1, Pd-NN) and trans-Pt(NH3)2(NO2)2 (2, Pt-NN) has been determined by single crystal X-ray diffraction (R = 0.0515 and 0.0341), respectively. Despite their compositional and configuration analogy, they crystallize in different crystal systems and space groups. The crystals of 1 (Pd-NN) are triclinic (space group No. 2, P-1, a = 5.003(1) Å, b = 5.419(1) Å, c = 6.317(1) Å, α = 91.34(2)°, β = 111.890(10)°, γ = 100.380(10)°), while those of 2 (Pt-NN) are monoclinic (space group No. 5, C2, a = 7.4235(16) Å, b = 9.130(2) Å, c = 4.4847(10) Å, β = 99.405(7)°). The pyrolytic processes of 1 and 2 (which might be sensitive to shock and heat) have been followed by simultaneous thermogravimetric and differential thermal analysis (TG/DTA), while the evolved gaseous species have been traced in situ by online coupled TG/DTA-EGA-MS and TG-EGA-FTIR instruments in He and air. Pd and Pt powders, forming as final solid products in single step, are captured and checked by TG and XRD. Whilst the unified evolved gas analyses report evolution of N2, H2O, NH3, N2O, NO, and NO2 gases as gaseous product components in the exothermic decomposition of both trans-Pd(NH3)2(NO2)2 (1) and trans-Pt(NH3)2(NO2)2 (2) starting from ca. 230 and 220 °C, in sealed crucibles with a pinhole on the top, respectively.

Original languageEnglish
Pages (from-to)51-59
Number of pages9
JournalThermochimica Acta
Volume490
Issue number1-2
DOIs
Publication statusPublished - Jun 1 2009

Fingerprint

Palladium
Platinum
Powders
Differential thermal analysis
palladium
thermal analysis
platinum
Gases
Single crystals
X ray diffraction
Crystals
single crystals
Crucibles
Ammonia
diffraction
gases
Molecular structure
decomposition
Pyrolysis
x rays

Keywords

  • CO sensors
  • Determination of molecular and crystal structure
  • Evolved gas analysis (EGA)
  • FTIR-spectroscopic gas cell
  • Mass spectrometry (MS)
  • Pt and Pd catalysts
  • Simultaneous thermogravimetry (TG) and differential thermal analysis (DTA)
  • Single crystal X-ray diffraction

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Condensed Matter Physics
  • Instrumentation

Cite this

@article{a1ba6510566c40b492c79eb6a7f7f925,
title = "Comparative evolved gas analytical and structural study on trans-diammine-bis(nitrito)-palladium(II) and platinum(II) by TG/DTA-MS, TG-FTIR, and single crystal X-ray diffraction",
abstract = "Detailed study on identification and thermal decomposition of solid title compounds 1 and 2 crystallized from the used aqueous ammonia solutions of Pd(NH3)2(NO2)2 and Pt(NH3)2(NO2)2, has been carried out. Beyond the composition of complexes 1 and 2, their trans square planar configuration have already been recognized by reference IR spectra and powder XRD patterns, nevertheless their exact molecular and crystal structure as of trans-Pd(NH3)2(NO2)2 (1, Pd-NN) and trans-Pt(NH3)2(NO2)2 (2, Pt-NN) has been determined by single crystal X-ray diffraction (R = 0.0515 and 0.0341), respectively. Despite their compositional and configuration analogy, they crystallize in different crystal systems and space groups. The crystals of 1 (Pd-NN) are triclinic (space group No. 2, P-1, a = 5.003(1) {\AA}, b = 5.419(1) {\AA}, c = 6.317(1) {\AA}, α = 91.34(2)°, β = 111.890(10)°, γ = 100.380(10)°), while those of 2 (Pt-NN) are monoclinic (space group No. 5, C2, a = 7.4235(16) {\AA}, b = 9.130(2) {\AA}, c = 4.4847(10) {\AA}, β = 99.405(7)°). The pyrolytic processes of 1 and 2 (which might be sensitive to shock and heat) have been followed by simultaneous thermogravimetric and differential thermal analysis (TG/DTA), while the evolved gaseous species have been traced in situ by online coupled TG/DTA-EGA-MS and TG-EGA-FTIR instruments in He and air. Pd and Pt powders, forming as final solid products in single step, are captured and checked by TG and XRD. Whilst the unified evolved gas analyses report evolution of N2, H2O, NH3, N2O, NO, and NO2 gases as gaseous product components in the exothermic decomposition of both trans-Pd(NH3)2(NO2)2 (1) and trans-Pt(NH3)2(NO2)2 (2) starting from ca. 230 and 220 °C, in sealed crucibles with a pinhole on the top, respectively.",
keywords = "CO sensors, Determination of molecular and crystal structure, Evolved gas analysis (EGA), FTIR-spectroscopic gas cell, Mass spectrometry (MS), Pt and Pd catalysts, Simultaneous thermogravimetry (TG) and differential thermal analysis (DTA), Single crystal X-ray diffraction",
author = "J. Madar{\'a}sz and P. Bombicz and M. Czugler and Ferenc R{\'e}ti and G{\'a}bor Kiss and G. Pokol",
year = "2009",
month = "6",
day = "1",
doi = "10.1016/j.tca.2009.02.006",
language = "English",
volume = "490",
pages = "51--59",
journal = "Thermochimica Acta",
issn = "0040-6031",
publisher = "Elsevier",
number = "1-2",

}

TY - JOUR

T1 - Comparative evolved gas analytical and structural study on trans-diammine-bis(nitrito)-palladium(II) and platinum(II) by TG/DTA-MS, TG-FTIR, and single crystal X-ray diffraction

AU - Madarász, J.

AU - Bombicz, P.

AU - Czugler, M.

AU - Réti, Ferenc

AU - Kiss, Gábor

AU - Pokol, G.

PY - 2009/6/1

Y1 - 2009/6/1

N2 - Detailed study on identification and thermal decomposition of solid title compounds 1 and 2 crystallized from the used aqueous ammonia solutions of Pd(NH3)2(NO2)2 and Pt(NH3)2(NO2)2, has been carried out. Beyond the composition of complexes 1 and 2, their trans square planar configuration have already been recognized by reference IR spectra and powder XRD patterns, nevertheless their exact molecular and crystal structure as of trans-Pd(NH3)2(NO2)2 (1, Pd-NN) and trans-Pt(NH3)2(NO2)2 (2, Pt-NN) has been determined by single crystal X-ray diffraction (R = 0.0515 and 0.0341), respectively. Despite their compositional and configuration analogy, they crystallize in different crystal systems and space groups. The crystals of 1 (Pd-NN) are triclinic (space group No. 2, P-1, a = 5.003(1) Å, b = 5.419(1) Å, c = 6.317(1) Å, α = 91.34(2)°, β = 111.890(10)°, γ = 100.380(10)°), while those of 2 (Pt-NN) are monoclinic (space group No. 5, C2, a = 7.4235(16) Å, b = 9.130(2) Å, c = 4.4847(10) Å, β = 99.405(7)°). The pyrolytic processes of 1 and 2 (which might be sensitive to shock and heat) have been followed by simultaneous thermogravimetric and differential thermal analysis (TG/DTA), while the evolved gaseous species have been traced in situ by online coupled TG/DTA-EGA-MS and TG-EGA-FTIR instruments in He and air. Pd and Pt powders, forming as final solid products in single step, are captured and checked by TG and XRD. Whilst the unified evolved gas analyses report evolution of N2, H2O, NH3, N2O, NO, and NO2 gases as gaseous product components in the exothermic decomposition of both trans-Pd(NH3)2(NO2)2 (1) and trans-Pt(NH3)2(NO2)2 (2) starting from ca. 230 and 220 °C, in sealed crucibles with a pinhole on the top, respectively.

AB - Detailed study on identification and thermal decomposition of solid title compounds 1 and 2 crystallized from the used aqueous ammonia solutions of Pd(NH3)2(NO2)2 and Pt(NH3)2(NO2)2, has been carried out. Beyond the composition of complexes 1 and 2, their trans square planar configuration have already been recognized by reference IR spectra and powder XRD patterns, nevertheless their exact molecular and crystal structure as of trans-Pd(NH3)2(NO2)2 (1, Pd-NN) and trans-Pt(NH3)2(NO2)2 (2, Pt-NN) has been determined by single crystal X-ray diffraction (R = 0.0515 and 0.0341), respectively. Despite their compositional and configuration analogy, they crystallize in different crystal systems and space groups. The crystals of 1 (Pd-NN) are triclinic (space group No. 2, P-1, a = 5.003(1) Å, b = 5.419(1) Å, c = 6.317(1) Å, α = 91.34(2)°, β = 111.890(10)°, γ = 100.380(10)°), while those of 2 (Pt-NN) are monoclinic (space group No. 5, C2, a = 7.4235(16) Å, b = 9.130(2) Å, c = 4.4847(10) Å, β = 99.405(7)°). The pyrolytic processes of 1 and 2 (which might be sensitive to shock and heat) have been followed by simultaneous thermogravimetric and differential thermal analysis (TG/DTA), while the evolved gaseous species have been traced in situ by online coupled TG/DTA-EGA-MS and TG-EGA-FTIR instruments in He and air. Pd and Pt powders, forming as final solid products in single step, are captured and checked by TG and XRD. Whilst the unified evolved gas analyses report evolution of N2, H2O, NH3, N2O, NO, and NO2 gases as gaseous product components in the exothermic decomposition of both trans-Pd(NH3)2(NO2)2 (1) and trans-Pt(NH3)2(NO2)2 (2) starting from ca. 230 and 220 °C, in sealed crucibles with a pinhole on the top, respectively.

KW - CO sensors

KW - Determination of molecular and crystal structure

KW - Evolved gas analysis (EGA)

KW - FTIR-spectroscopic gas cell

KW - Mass spectrometry (MS)

KW - Pt and Pd catalysts

KW - Simultaneous thermogravimetry (TG) and differential thermal analysis (DTA)

KW - Single crystal X-ray diffraction

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U2 - 10.1016/j.tca.2009.02.006

DO - 10.1016/j.tca.2009.02.006

M3 - Article

AN - SCOPUS:64749087706

VL - 490

SP - 51

EP - 59

JO - Thermochimica Acta

JF - Thermochimica Acta

SN - 0040-6031

IS - 1-2

ER -