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Crystal growth and characterization of mixed crystal potassium zinc vanadium sulphate

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Abstract

Mixed crystal, potassium zinc vanadium sulphate was grown from an aqueous solution containing equimolar proportions of K2Zn(SO4)2·6H2O (Tutton’s salt) and VOSO4 by slow evaporation at room temperature. Single crystal XRD analysis reveals that it belongs to monoclinic system with P21/c space group, and cell parameters are a = 9.006, b = 12.163, c = 1.36, and V = 649.6 Å3. The co-existence of VO(II)- and Zn in the Tutton’s salt crystalline matrix was confirmed by atomic absorption spectroscopy and energy dispersive X-ray spectroscopy. Scanning electron microscopy exhibits defect centres and crystal voids. The XRD and FT-IR analyses indicate the stress that the mixed crystal undergoes as a result of incorporation of vanadium. Thermal patterns of Tutton’s salt and the mixed crystal are compared. DTA curve exhibited a sharp endothermic peak at 420 °C for the pure K2Zn(SO)4·6H2O and at 410 °C for the mixed crystal.

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References

  1. Tutton AE. A comparative crystallographic study of the double selenites of the series R2M (SeO4)2 6H2O–salts in which M is zinc. Proc R Soc Lond. 1900;67:58–84.

    Article  Google Scholar 

  2. Marinova D, Georgiev M, Stoilova D. Vibrational behavior of matrix- isolated ions in Tutton compounds. I: infrared spectroscopic study of NH4 + and SO4 2− ions included in magnesium sulfates and selenates. J Mol Struct. 2009;929:67–72.

    Article  CAS  Google Scholar 

  3. Georgiev M, Marinova D, Stoilova D. Vibrational behavior of matrix- isolated ions in Tutton compounds. II: infrared spectroscopic study of NH4 + and SO4 2− ions included in copper sulfates and selenates. J Mol Struct. 2009;938:179–84.

    Article  Google Scholar 

  4. Marinova D, Georgiev M, Stoilova D. Vibrational behavior of matrix- isolated ions in Tutton compounds. V: infrared spectroscopic study of NH4 + and SO4 2− ions included in zinc sulfates and selenates. Solid State Sci. 2010;12:765–9.

    Article  CAS  Google Scholar 

  5. Georgiev M, Marinova D, Stoilova D. Vibrational behavior of matrix- isolated ions in Tutton compounds. III: infrared spectroscopic study of NH4 + and SO4 2− ions included in cobalt sulfates and selenates. Vib Spectrosc. 2010;53:233–8.

    Article  CAS  Google Scholar 

  6. Euler H, Barbier B, Klumpp S, Kirfel A. Crystal structure of Tutton’s salts, Rb2 [M″(H2O) 6] (SO4)2, M″ = Mg, Mn, Fe, Co, Ni. Zn. Z Kristallogr. NCS. 2000;215:473–6.

    CAS  Google Scholar 

  7. Euler H, Barbier B, Meents A, Kirfel A. Crystal structure of Tutton’s salts, Rb2 [M″(H2O) 6] (SeO4)2, M″ = Mg, Mn, Co. Zn. Z Kristallogr. NCS. 2003;218:265–8.

    CAS  Google Scholar 

  8. Euler H, Barbier B, Meents A, Kirfel A. Crystal structure of Tutton’s salts, Cs2 [M″(H2O) 6] (SO4)2, M″ = Mg, Mn, Fe, Co, Ni. Zn. Z Kristallogr. NCS. 2003;218:405–8.

    CAS  Google Scholar 

  9. Euler H, Barbier B, Meents A, Kirfel A. Crystal structure of Tutton’s salts, Cs2 [M″(H2O) 6] (SeO4)2, M″ = Mg, Mn, Fe, Co, Ni. Zn. Z Kristallogr. NCS. 2003;218:409–13.

    CAS  Google Scholar 

  10. Camargo MB, Stultz RD, Birnbaum M, Kotta M. Co2+: YSGG saturable absorber Q switch for infrared erbium lasers. Opt Lett. 1995;20:339–41.

    Article  CAS  Google Scholar 

  11. Denisov IA, Demchuk ML, Kuleshov NV, Yumashec KV. Co2+: LiGa5O8 saturable absorber passive Q switch for 1.34 μm Nd3+: YAlO3 and 1.54 μm Er3+: glass lasers. Appl Phys Lett. 2000;77:2455–8.

    Article  CAS  Google Scholar 

  12. Duan L, Yuan DR, Wang IH, Yu FP, Cheng XF, Liu ZQ, Yan SS. Synthesis and optical properties of Co2+-doped ZnGa2O4 nanocrystals. J Cryst Growth. 2006;296:234–8.

    Article  CAS  Google Scholar 

  13. Kuleshov NV, Mikhailov VP, Scherbitsky VG, Prokoshin PV, Yumashev KV. Absorption and luminescence of tetrahedral Co2+ ion in MgAl2O4. J Lumin. 1993;55:265–9.

    Article  CAS  Google Scholar 

  14. Mao X, Xu F, Tang J, Gao W, Li S, Du Y. Effects of co-doping on the crystallization and magnetic properties of Cu-free nanocrystalline Fe–Nb–B alloys. J Magn Mater. 2005;288:106–10.

    Article  CAS  Google Scholar 

  15. Yumashev KV. Saturable absorber Co2+: MgAl2O4 crystal for Q Switching of 1.34-μm Nd3+: YAlO 3 and 1.54-μm Er3+: glass lasers. Appl Opt. 1999;38:6343–6.

    Article  CAS  Google Scholar 

  16. Misra SK, Kahrizi M. EPR of Mn2+-doped single crystals of ZnK2(SO4)2·6H2O and NiK2(SO4)2·6H2O: Mn2+-Ni2+ exchange constant. Phys Rev. 1983;28:5300–3.

    Article  CAS  Google Scholar 

  17. Kripal R, Misra MG, Durinechi P. EPR and optical absorption study of Cu2 + ions doped in potassium hexaaquazinc (II) sulphate (PHZS) single crystals. Appl Magn Reson. 2012;42:251–67.

    Article  CAS  Google Scholar 

  18. Kasthurirengan S, Soundararajan S. Electron paramagnetic resonance study of vanadyl ion in K2Zn(SO4)2·6H2O and K2 Mg(SO4)2·6H2O. J Magn Reson. 1975;19:357–64.

    CAS  Google Scholar 

  19. Anandalakshmi H, Rajendran TM, Venkatesan R, Sambasiva Rao P. Single crystal EPR study of VO(II)- doped magnesium potassium Tutton’s salt––Part 4. Spectra Chim Acta. A. 2000;56:2617–25.

    Article  CAS  Google Scholar 

  20. Sambasiva Rao P, Viswanath AK, Subramanian S. EPR of dynamic Jahn-Teller distortion in Cu(II)- doped magnesium Tutton’s salt. Spectra Chim Acta. A. 1992;48:1745–57.

    Article  Google Scholar 

  21. Sambasiva Rao P. Single crystal EPR study of Mn(II)- doped magnesium potassium Tutton’s salt. Spectra Chim Acta.A. 1993;49:897–901.

    Article  Google Scholar 

  22. Sambasiva RaoP. Single crystal EPR study of Fe(II)- doped magnesium potassium Tutton’s salt. Spectra Chim Acta. A. 1996;52:1127–34.

    Article  Google Scholar 

  23. Smith TS, Brutto RL, Pecoraro VL. Paramagnetic spectroscopy of vanadyl complexes and its applications to biological systems. Coord Chem Rev. 2002;228:1–18.

    Article  CAS  Google Scholar 

  24. Anandalakshmi H, Parthiban S, Parvati V, Thanikachalam V, Mojumdar SC. Thermal and optical properties of Cu(II)- doped magnesium rubidium sulfate hexahydrate crystals. J Therm Anal Calorim. 2011;104:963–7.

    Article  CAS  Google Scholar 

  25. Ramasamy G, Bhagavannarayana G, Meenakshisundaram S, Madhurambal G. Crystal growth, structure, crystalline perfection and characterization of zinc magnesium ammonium sulphate hexahydrate mixed crystals ZnxMg(1-x)(NH4)2(SO4)2·6H2O. J. Cryst Growth. 2012;352:147–52.

    Article  Google Scholar 

  26. Madhurambal G, Mojumdar SC, Hariharan S, Ramasamy P. TG, DTA, FTIR and Raman Spectral analysis of Zna/Mgb ammonium sulphate mixed crystals. J Therm Anal Calorim. 2004;78:125–33.

    Article  CAS  Google Scholar 

  27. Leszczynska A, Pieliehowski K. Application of thermal analysis methods for characterization of polymer/montmorillonite nanocomposites. J Therm Anal Calorim. 2008;93(3):677–87.

    Article  CAS  Google Scholar 

  28. Vasudevan G, Anbusrinivasan P, Madhurambal G, Mojumdar SC. Thermal analysis effect of dopants Spectral characterization and growth aspect of KAP crystals. J Therm Anal Calorim. 2009;96:99–102.

    Article  CAS  Google Scholar 

  29. Anbusrinivasan P, Madhurambal G, Mojumdar SC. Thermal and spectral properties and induction period, intrafacial energy and nucleation parameters of solution grown Anthracene. J Therm Anal Calorim. 2012;108:939–46.

    Article  CAS  Google Scholar 

  30. Ramalingam S, Anbusrinivasan P, Periandy S. FT-IR and FT-Raman spectral investigation, computed IR-Intensity and Raman activity analysis and frequency estimation analysis on 4-chloro-2-bromoacetophenone was – HF and DFT calculations. Spectrochim Acta part A. 2011;78:826–34.

    Article  CAS  Google Scholar 

  31. Mojumdar SC, Raki L. Preparation, thermal, spectral and microscopic studies of calcium silicate hydrate–poly (acrylic acid) nanocomposite materials. J Therm Anal Calorim. 2006;85:99–105.

    Article  CAS  Google Scholar 

  32. Ezhilvizhi R, Kalainathan S, Bhavannarayana G. Structural and micro hardness studies of urea and thiourea doped glycine phosphate single crystal. Cryst Rev Technol. 2008;43:778–82.

    Article  Google Scholar 

  33. Mojumdar SC. Processing-moisture resistance and thermal analysis of MDF material. J Therm Anal Calorim. 2001;64:1133–9.

    Article  CAS  Google Scholar 

  34. Madhurambal G, Ramasamy P, Anbusrinivasan P, Vasudevan G, Kavitha S, Mojumdar SC. Growth and characterization studies of 2- bromo-4″- chloro-acetophenone (BCAP) crystals. J Therm Anal Calorim. 2008;94:59–62.

    Article  CAS  Google Scholar 

  35. Mojumdar SC. Thermal properties, environmental deterioration and application of macro-defect-free cements. Res J chem Environ. 2005;9:23–7.

    CAS  Google Scholar 

  36. Madhurambal G, Mojumdar SC, Hariharan S, Ramasamy P. TG, DTA, FTIR and Raman spectral analysis of ZN\Mg, ammonium sulphate mixed crystals. J Therm Anal Calorim. 2004;78:125–33.

    Article  CAS  Google Scholar 

  37. Selvaraju K, Valluvan R, Kumararaman S. A new metal organic potassium thiourea chloride single crystal. Mat Lett. 2006;440:574–81.

    Google Scholar 

  38. Sawant SY, Verenkar VMS, Mojumdar SC. Preparation, thermal, XRD, chemical and FT-IR spectral analysis of NiMn2O4 nanoparticles and respective precursor. J Therm Anal Calorim. 2007;90:669–72.

    Article  CAS  Google Scholar 

  39. Porob RA, Khan SZ, Mojumdar SC, Verankar VMS. Synthesis, TG, DSC and infra-red spectral study of NiMn2(C2H4O4)36N2H4-A precursor for NiMn2O4 nanoparticles. J Therm Anal Calorim. 2006;86:605–8.

    Article  CAS  Google Scholar 

  40. Mojumdar SC, Varshney KG, Agarval A. Hybrid fibrous ion exchange materials: past, prevent and failure. Res J Chem Environ. 2006;10:89–103.

    CAS  Google Scholar 

  41. Doval M, Palou M, Mojumdar SC. Hydration behavior of C2S and C2AS nanomaterial synthesized by sol–gel method. J Therm Anal Calorim. 2006;86:595–9.

    Article  CAS  Google Scholar 

  42. Varshney G, Agarwal A, Mojumdar SC. Pyridine based cerium (IV) phosphate hybrid fibrous ion exchanger synthesis characterization and thermal behavior. J Therm Anal Calorim. 2007;90:731–4.

    Article  CAS  Google Scholar 

  43. Mojumdar SC, Melinik M, Jona E. Thermal and spectral properties of Mg(II) and CU(II) complexes with heterocyclic N-donor ligands. J Anal Appl Pyrolysis. 2000;53:149–60.

    Article  CAS  Google Scholar 

  44. Mojumdar SC, Sain M, Prasad RC, Sun L, Venart JES. Selected thermoanalytical methods and their applications from medicine to construction. J Therm Anal Calorim. 2007;60:653–62.

    Article  Google Scholar 

  45. Mojumdar SC, Simon P, Krutosikova A. [1] Benzofuro [3,2-c] pyridine: synthesis and coordination reactions. J Therm Anal Calorim. 2009;96:103–9.

    Article  CAS  Google Scholar 

  46. Mojumdar SC, Miklovic J, Krutosikova A, Valigura D, Stewart JM. Furopyridine-Ni(II) complexes-Synthesis, thermal and spectral characterization. J Therm Anal Calorim. 2005;81:211–5.

    Article  CAS  Google Scholar 

  47. Mojumdar SC. Thermoanalytical and IR spectroscopy investigation of Mg(II) complexes with hetrocyclic ligands. J Therm Anal Calorim. 2001;64:629–36.

    Article  CAS  Google Scholar 

  48. Narayanamoolaya B, Dharmaprakash SM. Synthesis, growth and characterization of nonlinear optical crystal l-tyrosine hydrobromide. Cryst growth. 2006;290:498–503.

    Article  Google Scholar 

  49. Jayalakshmi D, Kumar J. Growth and characterization of bisthiourea zinc acetate. Cryst Res Technol. 2006;41:37–40.

    Article  CAS  Google Scholar 

  50. Mojumdar SC, Mazanec K, Drabik M. Macro-detect-free (MDF) cements: synthesis, thermal, chemical, SEM and magnetometric study and moisture resisistance. J Therm Anal Calorim. 2006;83:135–9.

    Article  CAS  Google Scholar 

  51. Kubranová M, Jóna E, Rudinská E, Nemčeková K, Ondrušová D, Pajtášová M. Thermal properties of Co-, Ni-and Cu-exchanged montmorillonite with 3-hydroxypyridine. J Therm Anal Calorim. 2003;74:251–7.

    Article  Google Scholar 

  52. Kubelka P, Munk F. Ein beitrag zur optik der farbanstriche. Z Tech Physik. 1931;12:593–601.

    Google Scholar 

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Authors and Affiliations

  1. Department of Chemistry, Annamalai University, Annamalai Nagar, Chidambaram, 608002, India

    J. Vijila Manonmoni, G. Ramasamy, S. P. Meenakshisundaram & M. Amutha

  2. Department of Chemistry, University of Guelph, Guelph, ON, Canada

    S. C. Mojumdar

  3. Department of Chemical Technology and Environment, Trencin University of A. Dubceck, Puchov, Slovakia

    S. C. Mojumdar

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  1. J. Vijila Manonmoni
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Manonmoni, J.V., Ramasamy, G., Meenakshisundaram, S.P. et al. Crystal growth and characterization of mixed crystal potassium zinc vanadium sulphate. J Therm Anal Calorim 119, 969–974 (2015). https://doi.org/10.1007/s10973-014-4110-y

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  • DOI: https://doi.org/10.1007/s10973-014-4110-y

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