The new 1,2,4-benzenetricarboxylates of lanthanide(III) of the formula Ln(btc)�nH2O, where btc is 1,2,4-benzenetricarboxylate; Ln is La-Lu, and n=2 for Ce; n=3 for La, Yb, Lu; and n=4 for Pr-Tm were prepared and characterized by elemental analysis, infrared spectra and X-ray diffraction patterns. Polycrystalline
complexes are isotructural in the two groups: La-Tm and Yb, Lu. IR spectra of the complexes show that all carboxylate groups
from 1,2,4-benzentricarboxylate ligands are engaged in coordination of lanthanide atoms.
The thermal analysis of the investigated complexes in air atmosphere was carried out by means of simultaneous TG-DTA technique.
The complexes are stable up to about 30�C but further heating leads to stepwise dehydration. Next, anhydrous complexes decompose
to corresponding oxides. The combined TG-FTIR technique was employed to study of decomposition pathway of the investigated
Authors:J. Mullens, G. Reggers, M. Ruysen, R. Carleer, J. Yperman, D. Franco, and L. Van Poucke
The oxidative degradation of HET-acid (1,4,5,6,7,7-hexachlorobicyclo [2.2.1] hept-5-en-2, 3-dicarboxylic acid) is studied
by the combination of TG, FTIR, MS and GC-MS. The gases evolved during the decomposition of this flame retardant are investigated
on-line by FTIR and by MS. Simultaneously the evolved gases are collected by an adsorbent and, after the thermal experiment,
desorbed to release the volatile products for identification using GC-MS. The combination of these techniques offers the unambiguous
identification of the evolved products as a function of temperature. The main identified products are CO2, H2O, Cl2, HCl, C2Cl4, maleic acid anhydride, HET-acid anhydride, chlorinated cyclic hydrocarbons and chlorinated unsaturated linear hydrocarbons.
Authors:R. Mrozek, Z. Rzączyńska, and M. Sikorska-Iwan
The thermal decomposition behaviour of the manganese(II) complexes with glycine: Mn(gly)Cl2(H2O)2, Mn(gly)2Cl2, Mn(gly)Br2(H2O)2, Mn(gly)2Br2(H2O)2 was investigated by means of TG-DTG-DTA, Hi-Res-TA and DSC techniques. The evolved gas analysis was carried out by means
of the coupled TG-FTIR system. Heating of the complexes results first in the release of water molecules. Next, the multi-stage
decomposition process with degradation of glycine ligand occurs. Water, carbon dioxide and ammonia were detected in the gaseous
products of the complexes decomposition. The temperature of NH3 evolution from the complexes is higher than from free glycine. The final residue in the air atmosphere is Mn2O3 which transforms into Mn3O4 at 930C. In a nitrogen atmosphere, the complexes decompose into MnO.
A novel PMR polyimides (TMBZ-15) based on substituted benzidines is examined and compared to state-of-the-art PMR-15. The
mechanism for the thermal decomposition of two specific PMR polyimides is obtained using TG/FTIR/MS techniques. In order to
verify the pathway of polyimide degradation, a pyrolysis/GC-MS technique was employed to evaluate the organic degradation
products, particularly the larger components that are destroyed in traditional TG/MS. A proposed degradation mechanism involves
two main stages of decomposition, each of which produce a variety of products. The first group includes aromatic hydrocarbons,
aromatic amines and nitriles, which correspond to partial fragments of polymer chains. The second group consists largely of
fluorene, naphthalene and phenanthrene, which are attributed to the isomerization, rearrangements and cyclizations of the
aforementioned pyrolyzates at high temperature.
Authors:B. Zapata, J. Balmaseda, E. Fregoso-Israel, and E. Torres-García
Thermal degradation of orange peel was studied in dynamic air atmosphere by means of simultaneous TG-DSC and TG-FTIR analysis.
According to the obtained thermal profiles, the orange peel degradation occurred in at least three steps associated with its
three main components (hemicellulose, cellulose and lignin). The volatiles compounds evolved out at 150–400 °C and the gas
products were mainly CO2, CO, and CH4. A mixture of acids, aldehydes or ketones C=O, alkanes C–C, ethers C–O–C and H2O was also detected. The Eα on α dependence reveled the existence of different and simultaneous processes suggesting that the combustion reaction is
controlled by oxygen accessibility, motivated by the high evolution low-molecular-mass gases and volatile organic compounds.
These results could explain the non-autocatalytic character of the reactions during the decomposition process.
Authors:T. Kaljuvee, M. Radin, D. Astahhov, and Y. Pelovski
TG-FTIR technique was used for identification of gaseous compounds evolved
at thermal treatment of six coal samples from different deposits (Bulgaria,
Russia, Ukraine). The experiments were carried out under dynamic heating conditions
up to 900C at heating rates of 5, 10 or 50 K min–1
in a stream of dry air. The emission of CO2, H2O,
CO, SO2, COS, methane, methanol, formic acid, formaldehyde,
acetaldehyde, chlorobenzene was clearly identified in FTIR spectra of the
samples studied. The formation of ethanol, ethane, ethylene and p-xylene, at least on the level of traces, was also
identified. At the heating rate of 5C min–1
the temperature of maximum intensities of the characteristic peaks of COS
was 270C, of formaldehyde, formic acid, ethane and methanol 330C,
of SO2, CO, acetic acid, ethylene and p-xylene
400C and of chlorobenzene 500C. At 10C min–1
and 50C min–1 these temperatures were
shifted, respectively, by 70–300C and 150–450C towards
higher temperatures and the respective absorption bands in FTIR spectra were,
as a rule, more intensive.
Authors:S. Jingyan, L. Jie, D. Yun, H. Ling, Y. Xi, W. Zhiyong, L. Yuwen, and W. Cunxin
The thermal behavior of nicotinic acid under inert conditions was investigated by TG, FTIR and TG/DSC-FTIR. The results of
TG/DSC-FTIR and FTIR indicated that the thermal behavior of nicotinic acid can be divided into four stages: a solid-solid
phase transition (176–198°C), the process of sublimation (198–232°C), melting (232–263°C) and evaporation (263–325°C) when
experiment was performed at the heating rate of 20 K min−1. The thermal analysis kinetic calculation of the second stage (sublimation) and the fourth stage (evaporation) were carried
out respectively. Heating rates of 1, 1.5, 2 and 3 K min−1 were used to determine the sublimation kinetics.
The apparent activation energy, pre-exponential factor and the most probable model function were obtained by using the master
plots method. The results indicated that sublimation process can be described by one-dimensional phase boundary reaction,
g(α)=α. And the ‘kinetic triplet’ of evaporation process was also given at higher heating rates of 15, 20, 25, 30 and 35 K min−1. Evaporation process can be described by model of nucleation and nucleus growing,
Commercial light-cured dental composites were used in this study. Two laboratorial composites, Resilab (Wilcos/Brazil), Epricord
(Kuraray/Japan) were compared under cured and uncured conditions. Thermal analysis, infrared spectroscopy and scanning electron
microscopy were used to evaluate the dental composites. The mass change and heat flow signals (TG–DSC) were recorded simultaneously
by using STA 409 PC Luxx (NETZSCH), in the 25–800 °C temperature range at a heating rate of 10 °C/min under nitrogen atmosphere
(70 mL/min). Employing thermo-microbalance TG 209 C F1 Iris (NETZSCH) coupled to the BRUKER Optics FTIR TENSOR, the samples
were analyzed by combined thermogravimetric and spectroscopic methods (TG–FTIR). The initial sample mass was about ~12 mg,
the data collection have been done in the 35–800 °C temperature range at a heating rate of 20 K/min in nitrogen atmosphere
(flow rate: 40 mL/min). Finally, superficial topographic was analyzed by scanning electron microscopy (SEM). Dental composite
evaluation suggests a high thermal stability and inorganic content in RES D sample. Degrees of conversion (DC) values were
almost the same and there was no direct relationship between DC and amount of particles and size. Similar compositions were
found in all samples.
The cefadroxil (Cef) complexes with transition divalent metals of the formula MCefnH2O (where n=2 for M=Cu2+, Ni2+, Zn2+ and n=3 for Co2+) and CdCef1.54H2O were prepared and characterized by elemental and infrared spectra. The thermal analysis of the investigated complexes in
air atmosphere was carried out by means of simultaneous TG-DSC technique. During heating in air they lose bound water molecules
and then decompose to oxides: Co3O4, NiO, CuO, ZnO and CdO. The CdCef1.54H2O complex forms probably an intermediate product Cd2OSO4. The combined TG-FTIR technique was employed to study of decomposition pathway of the investigated complexes. The first mass
loss step is the water loss of the complexes. Next, decomposition of cefadroxil ligand occurs with evolution of CO2 and NH3. At slightly higher temperature COS is observed according to decomposition of cephem ring. Additionally, as decomposition
gaseous products: HCN, HNCO (HOCN), H2CNH, CO, SO2, hydrocarbons and carbonyl compounds were observed. The formation of metal sulfates is postulated as solid intermediate product
of decomposition in the argon atmosphere.
Authors:M. Beneš, V. Pla?ek, G. Matuschek, A. A. Kettrup, K. Györyová, W. D. Emmerich, and V. Balek
Thermal behavior of commercial PVC cable insulation both before and after extraction of plasticizers, fillers and other agents
were tested by TG/DTG and DSC during heating in the range 20-800C in air. The ultrasound enhanced hexane extraction and dissolution
in THF with subsequent precipitation of PVC were used to prepare 'extracted' and 'precipitated' samples. The total mass loss
measured for the 'non-treated', 'extracted' and 'precipitated' PVC samples was 71.6, 66.6 and 97%, respectively. In the temperature
range 200-340C the release of dioctylphthalate, HCl and CO2was observed by simultaneous TG/FTIR. From TG results measured at different heating rates (1.5, 5, 10, 15 K min-1) in the range 200-340C the non-isothermal kinetics of the PVC samples degradation was determined. Activation energy values
of the thermal degradation processes calculated by ASTM E 698 method, for 'non-treated', 'extracted' and 'precipitated' PVC
samples were 174.617 kJ min-1, 192.819 kJ min-1, 217.120 kJ min-1, respectively. These kinetic parameters were used for the lifetime simulation of the materials.