Use of emanation thermal analysis and evolved gas analysis in thermal study of zinc(II) benzoate complex compounds
769
Intensity of m=76/A*E–10
1,5
heating the compounds to 600 °C. From the smooth
exponential-like increase of the radon release rate observed
by ETA on sample heating from 650 up to 850 °C it fol-
lowed that no microstructure changes can be expected with
the zinc oxide samples in this temperature range. The break
and subsequent decrease of radon release rate observed by
ETA on heating above 900 °C makes it possible to assume
the growth or sintering of fine grains of the zinc oxide
powders.
1,8
1,6
1,4
1,2
1,0
60+
0,5
76+
0,0
100 200 300 400 500 600 700 800 900 1000
Intensity of m=44/A*E–9
6
4,5
4,0
3,5
5
1,0
0,5
0,0
4
18+
3
Acknowledgements This work was supported by the Ministry of
Education of the Slovak Republic (Project VEGA No. 1/0122/08) and
by the Ministry of Education, Youth and Sports of the Czech Republic
(Project INGO No. LA-292). This financial support is gratefully
acknowledged.
44+
3,0
2,5
46+
2
1
100 200 300 400 500 600 700 800 900 1000
0,16
0,12
0,08
0,04
ETA
References
1. Kimura E, Koike T. Intrinsic properties of zinc(II) ion pertinent
to zinc enzymes. Adv Inorg Chem. 1997;44:229–61.
100 200 300 400 500 600 700 800 900 1000
2. Berg JM, Shi Y. The galvanization of biology: a growing
appreciation for the roles of zinc. Science. 1996;27:1081–5.
3. Lewandowski W, Kalinowska M, Lewandowska H. The influence
of metals on the electronic system of biologically important
ligands. Spectroscopic study of benzoates, salicylates, nicotinates
and isoorotates. J Inorg Biochem. 2005;99:1407–23.
DTG/(mg*min–1
DTG
)
DTA/µV
0
-20
-60
-40
-20
0
0,00
-0,04
-0,08
-0,12
-0,16
-40
DTA
TG
-60
ˇ
}
´
´
´ˇ
´
4. Chomic J, Gyoryova K, Szunyogova E, Kovarova J. Thermal
study of zinc(II) salicylate complex compounds with bioactive
ligands. J Therm Anal Calorim. 2004;76:33–41.
-80
-100
100 200 300 400 500 600 700 800 900 1000
Temperature/°C
´
ˇ
´
´
ˇ´
5. Gyoryova K, Chomic J, Szunyogova E, Piknova L, Zelenak V,
Vargova Z. Thermal study of zinc(II) 4-chlorosalicylate complex
}
´
Fig. 3 Results of thermogravimetry (TG/DTG), differential thermal
analysis (DTA), evolved gas analysis (EGA) with MS detection and
emanation thermal analysis (ETA) of the Zn(C6H5COO)2ꢀu2 com-
pound measured on heating in air
compounds with bioactive ligands. J Therm Anal Calorim.
2006;84:727–32.
}
´
ˇ
´ˇ
´
6. Gyoryova K, Chomic J, Kovarova J. Thermal behaviour of
zinc(II) 5-chlorosalicylate complex compounds. J Therm Anal
Calorim. 2005;80:375–80.
ˇ´
7. Zelenak V, Sabo M, Massa W, Llewellyn P. Preparation,
morphology changes took place in the zinc oxide up to
850 °C. The break and subsequent decrease of radon
release rate E(T) on heating above 900 °C makes it
possible to expect the growth or sintering of fine grains
of the zinc oxide powder prepared by the thermal
degradation of the Zn(II) benzoate complex with urea.
characterisation and crystal structure of two zinc(II) benzoate
complexes with pyridine-based ligands nicotinamide and methyl-
3-pyridylcarbamate. Inorg Chim Acta. 2004;357:2049–59.
´
8. Szunyogova E, Gyoryova K, Hudecova D, Piknova L, Chomic J,
Vargova Z, et al. Thermal, spectral and biological properties of
´
´
´
ˇ
}
´
Zn(II) complex compounds with phenazone. J Therm Anal
Calorim. 2007;88:219–23.
9. Gusejnov GA, Musajev FN, Usubaliev BT, Amiraslanov IR,
Mamedov KhS. Koord Khim. 1984;10:117–22.
´
10. Findorakova L, Gyoryova K, Kovarova J, Balek V, Nour El-Dien
FA, Halas L. Novel zinc(II) benzoate complex compounds with
´
}
´
´ˇ
´
Conclusions
´
caffeine and urea. J Therm Anal Calorim. 2009;95:923–8.
}
It was found that the oxidative degradation of urea with
CO2 or caffeine with CO2 from the investigated Zn(II)
benzoate complex compounds takes place as the first step
of their thermal degradation. In the second step of thermal
degradation diphenylketone was release.
11. Balek V, Tolgyessy J. Emanation thermal analysis and other
radiometric emanation methods. Amsterdam: Elsevier; 1984. p.
43–71.
12. Balek V. Emanation thermal analysis and its application
potential. Thermochim Acta. 1991;192:1–17.
}
´
13. Balek V, Subrt J, Mitsuhashi T, Beckman IN, Gyoryova K.
Emanation thermal analysis: ready to fulfill the future needs of
materials characterization. J Therm Anal Calorim. 2002;67:15–35.
14. Ziegler JF, Biersack JP. The stopping and range of ions in solids.
New York: Pergamon Press; 1985.
Intermediate products of thermal degradation of the
zinc(II) benzoate complex compound were determined by
evolved gas analysis. Microstructure changes that accom-
panied the degradation of the samples were characterized
by emanation thermal analysis on heating. Zinc oxide was
determined as the final product of thermal degradation after
15. Zhang J, Yuan L, Yuan J, Sun J. Mechanism of thermal
decomposition of barium benzoate. J Therm Anal Calorim.
1999;58:287–92.
123