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Preparation, crystal structure and thermal studies of cadmium perchlorate complex with 2,2′-bipyridine

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Abstract

The mixed-ligand mononuclear hexacoordinate cadmium perchlorate complex [Cd(2,2′-bipy)2(H2O)(ClO4)]ClO4 was synthesized and characterized by FT-IR, elemental analysis and X-ray crystal structure determination. Thermal characteristics of the complex were studied by thermogravimetry (TG), differential thermal analysis and differential scanning calorimetry. The complex is stable at normal temperature and undergoes dehydration in between the temperature range 95–200 °C with loss of coordinated water (2.8 %). Thereafter, on increasing temperature, dehydrated complex shows some gradual mass loss followed by fast decomposition at higher temperature (265–380 °C). The kinetic parameters for the decomposition of the complex were investigated by applying model-fitting and isoconversional method on isothermal TG data recorded at five different temperatures. To explore the response of complex to sudden high heat, explosion delay time was recorded at five different temperatures, and kinetics of explosion was investigated using these data.

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References

  1. Singh G, Kapoor IPS, Kumar D, Singh UP, Goel N. Preparation, X-ray crystallography and thermal decomposition of transition metal perchlorate complexes with perchlorate and 2,2′-bipyridyl ligands. Inorg Chim Acta. 2009;362:4091–8.

    Article  CAS  Google Scholar 

  2. Kumar D, Kapoor IPS, Singh G, Frohlich R. Preparation, characterisation and kinetics of thermolysis of nickel and copper nitrate complexes with 2,2′-bipyridine ligand. Thermochim Acta. 2012;545:67–74.

    Article  CAS  Google Scholar 

  3. Kumar D, Kapoor IPS, Singh G, Goel N, Singh UP. Preparation, X-ray crystallography and thermolysis of transition metal nitrates of 2,2′-bipyridine (part 63). J Therm Anal Calorim. 2012;107:325–34.

    Article  CAS  Google Scholar 

  4. Patil KC, Verneker Pai VR, Jain SR. Role of metal perchlorate ammines on ammonium perchlorate decomposition. Combust Flame. 1975;25:387–8.

    Article  CAS  Google Scholar 

  5. Singh G, Pandey DK. Studies on energetic compounds, part 27: kinetics and mechanism of thermolysis of bis(ethylenediamine) metal nitrates and their role in the burning rate of solid propellants. Propellants Explos Pyrotech. 2003;28:231–9.

    Article  CAS  Google Scholar 

  6. Singh G, Pandey DK. Studies on energetic compounds, part 43: effect of some BEMP complexes on the combustion and condensed phase thermolysis HTPB-AP composite solid propellants. Ind J Chem Technol. 2005;12:175–80.

    Google Scholar 

  7. Stoner CE Jr, Haggerty BS, Rheingold AL, Brill TB. Thermal decomposition of energetic materials: 55, metal complexes of diaminoglyoxime as potential burn rate modifiers in composite propellants. Propellants Explos Pyrotech. 1992;17:82–7.

    Article  CAS  Google Scholar 

  8. Sonawane SH, Gore GM, Polke BG, Nazare AN, Asthana SN. Transition metal carbohydrazide nitrates: burn- rate modifier for propellants. Def Sci J. 2006;56:391–8.

    Article  CAS  Google Scholar 

  9. Singh G, Kapoor IPS, Pandey DK. Hexammine metal perchlorates as energetic burning rate modifiers. J Energ Mater. 2002;20:223–44.

    Article  CAS  Google Scholar 

  10. Singh G, Pandey DK. Studies on energetic compounds, part 40: kinetics of thermal decomposition of some bis(propylenediamine)metal perchlorate complexes. J Therm Anal Calorim. 2005;82:353–60.

    Article  CAS  Google Scholar 

  11. Fedoroff BT, Sheffield OE. Encyclopedia of explosives and related items. Picatinny Arsenal Dover NJ. 1966;5:F217–23.

    Google Scholar 

  12. Koper JH, Jansen OG, Van der Berg PJ. A reaction mechanism for the decomposition of ammonium nitrate. Explosivstoffe. 1970;8:181–3.

    Google Scholar 

  13. Gillaspie Dane T, Tenent RC, Dillon AC. Metal-oxide films for electrochromic applications: present technology and future directions. J Mater Chem. 2010;20:9585–92.

    Article  Google Scholar 

  14. Topalian Z. Nanostructured transition metal oxides in cleantech application. Acta Univ Ups Upps. 2011;369:809.

    Google Scholar 

  15. Bresser D, Muller F, Fiedler M, Krueger S, Kloespsch R, Baither D, Winter M, Paillaered E, Passerini S. Transition-metal-doped zinc oxide nanoparticles as a new lithium-ion anode material. Chem of Mater. 2013;25:4977–85.

    Article  CAS  Google Scholar 

  16. Shen SM, Chen S, Wu BH. The thermal decomposition of ammonium perchlorate (AP) containing a burning rate modifier. Thermochim Acta. 1993;223:135–42.

    Article  CAS  Google Scholar 

  17. Sharma JK, Srivastava P, Singh G. Review on nano catalysts: potential burning rate modifier for composite solid propellant. Mater Focus. 2014;3:81–91.

    Article  CAS  Google Scholar 

  18. Salehi B, Mehrabian S, Ahmadi M. Investigation of antibacterial effect of cadmium oxide nanoparticles on Staphylococcus Aureus bacteria. J Nanobiotechnol. 2014;12(26):1–8.

    Google Scholar 

  19. Khalilzadeh B, Hasanzadeh M, Sanati S, Saghatforoush L, Shadjou N, Dolatabadi JEN, Sheikhzadeh P. Preparation of a new electrochemical sensor based on cadmium oxide nanoparticles and application for determination of penicillamine. Int J Electrochem Sci. 2011;6:4164–75.

    CAS  Google Scholar 

  20. Kondawar S, Mahore R, Dahegaonkar A, Agrawal S. Electrical conductivity of cadmium oxide nanoparticles embedded polyaniline nanocomposites. Adv Appl Sci Res. 2011;2(4):401–6.

    CAS  Google Scholar 

  21. Rejitha KS, Mathew S. Thermal behaviour of nickel (II) sulphate, nitrate and halide complexes containing ammine and ethylenediamine as ligands: kinetics and evolved gas analysis. J Therm Anal Calorim. 2011;106:267–75.

    Article  CAS  Google Scholar 

  22. Walmsley F, Pinkertan AA, Walmsley JA. Synthesis and X-ray crystal structure of 1:1 complexes of nickel (II) nitrate with 1,10-phenanthroline and with 2,2′-bipyridine. Polyhedron. 1989;8:689–93.

    Article  CAS  Google Scholar 

  23. Rujiwatra A, Yimklan S, Prior TJ. A second crystal form of [Ni(2,2′-bipyridine)(H2O)(NO3)](NO3) featuring a different molecular orientation. Polyhedron. 2012;31:345–51.

    Article  CAS  Google Scholar 

  24. Mathew S, Manohar H. Redetermination of the structure of triaqua (2,2′-bipyridyle) nitrocopper (II) nitrate. Acta Cryst. 1991;C47:2213–4.

    Google Scholar 

  25. Jianmin L, Jianbin Z, Xintao K. A novel structure of bipyridyle coordinated with copper (II) [Cu(2,2′-bipyridine)(H2O)3(NO3)2]. Cryst Res Technol. 1996;31:589–93.

    Article  CAS  Google Scholar 

  26. Li Z, Zhou Z, Zhang T, Tang Z, Li Y, Zhang J. Energetic transition metal (Co/Cu/Zn) imidazole perchlorate complexes: synthesis, structural characterisation, thermal behaviour and non-isothermal kinetic analyses. Polyhedron. 2012;44:59–65.

    Article  Google Scholar 

  27. Singh G, Singh CP, Frohlich R. Preparation, characterisation and thermolysis of metal nitrate complexes with 4,4′-bipyridine. J Therm Anal Calorim. 2006;85:425–31.

    Article  CAS  Google Scholar 

  28. Kumar D, Kapoor IPS, Singh G. X-Ray crystallography and thermolysis of ammonium perchlorate and protoneted hexamethylenetetramine perchlorate prepared by newer methods: Part 69. J Energ Mater Chem Propul. 2010;9:549–60.

    Google Scholar 

  29. Singh G, Barnawal BP, Kapoor IPS, Kumar D. Frohlich Roland. Preparation X- ray crystallography and thermal decomposition of some transition metal perchlorate complexes of hexamethylenetetramine. J Phys Chem. 2007;A11:12972–6.

    Article  Google Scholar 

  30. Ilyushin MA, Tselinskiy IV, Smirnove AV, Shugalei IV. Physicochemical properties and laser initiation of a copper perchlorate complex with 3(5)-hydrazino-4-amino-1,2,4-triazole (HATr) as a Ligand. Central Eur J Energ Mater. 2012;9:3–16.

    CAS  Google Scholar 

  31. Ilyushin MA, Alieksandrova MA, Bachurina IV, Smirnov AV, Taselinskii IV. Synthesis and properties of an energetic complex pentaaminecobalt(III) perchlorate with 4-amino-1,2,4-triazole as ligand. Rus J App Chem. 2010;83:94–8.

    Google Scholar 

  32. Singh CP, Srivastava AK, Singh A, Kumar B. Kinetics of thermolysis of nickel perchlorate complex with 2-aminopyridine ligand. Int J Eng Res and Sci Technol. 2013;2(4):143–52.

    Google Scholar 

  33. Singh CP. Singh Abhishek. Kinetics of copper(II) perchlorate complex with 4-aminopyridin. Energy Environ Focus. 2014;3:202–5.

    Article  Google Scholar 

  34. Nakamoto K. Infrared and Raman Spectra of inorganic and co-ordination compounds. New York: Wiley; 1978.

    Google Scholar 

  35. Robert CW. Handbook of physics and chemistry. Florida: CRC Press; 1996.

    Google Scholar 

  36. Miller FA, Wilkins CH. Infrared spectra and characteristic frequencies of inorganic ions. Anal Chem. 1952;24:1253–94.

    Article  CAS  Google Scholar 

  37. Hooft R. Data collection software, COLLECT, Nonius, BV. Delt. The Netherlands; 1998.

  38. Otowinowaski Z, Minor W. Processing of X-ray diffraction data collected in oscillation mode. Methods Enzymol. 1997;276:307–26.

    Article  Google Scholar 

  39. Sheldrick GM. A short history of SHELX. Acta Cryst. 2008;A64:112–22.

    Article  Google Scholar 

  40. Keller E. A computer program for the graphic representation of molecular and crystallographic models. Germany: University Freiburg; 1997.

    Google Scholar 

  41. Singh G, Singh RR. Indigenously fabricated TG apparatus for thermogravimetric analysis. Res Ind. 1978;23:92–3.

    CAS  Google Scholar 

  42. Singh G, Kapoor IPS, Vasudeva SK. Thermolysis of AP-PS additive mixtures. Ind J Technol. 1991;29:584–94.

    Google Scholar 

  43. Kumar D, Kapoor IPS, Singh G, Goel N, Singh UP. Preparation, characterisation and thermal behaviour of polymeric complex of cadmium hexamethylenetetramine nitrate. Solid State Sci. 2012;14:495–500.

    Article  CAS  Google Scholar 

  44. Brown ME, Dollimore D, Galway AK. Reactions in the solid state, comprehensive chemical kinetics. Amsterdam: Elsevier; 1997.

    Google Scholar 

  45. Vyazovkin S, Wight CA. Isothermal and non-isothermal reaction kinetics in solids: in search of ways towards consensus. J Phys Chem. 1997;A10:8279–84.

    Article  Google Scholar 

  46. Vyazovkin S, Wight CA. Model-free and model-fitting approaches to kinetic analysis of isothermal and non-isothermal data. Thermochim Acta. 1999;340:53–8.

    Article  Google Scholar 

  47. Vyazovkin S, Chrissafis K, Di Lorenzo ML, Koga N, Pijolat M, Roduit B, Sbirrazzuoli N, Suñol JJ. ICTAC Kinetics Committee recommendations for collecting experimental thermal analysis data for kinetic computations. Thermochim Acta. 2014;590:1–23.

    Article  CAS  Google Scholar 

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Acknowledgements

Thanks to Secretary, Board of Management, Principal and the Head of Department of Chemistry, D.B.S. College, Kanpur, for providing laboratory facilities and University Grants Commission, New Delhi, for financial assistance. Thanks are also due to Sophisticated Test and Instrumentation Centre, Cochin University of Science and Technology for CHN, FT-IR and TG–DSC analysis.

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Correspondence to Chandra Prakash Singh.

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Singh, C.P., Singh, A., Nibha et al. Preparation, crystal structure and thermal studies of cadmium perchlorate complex with 2,2′-bipyridine. J Therm Anal Calorim 121, 633–640 (2015). https://doi.org/10.1007/s10973-015-4613-1

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