Synthesis and Characterization of Gallosilicate Sodalite Containing NO2- Ions
Pure phase gallosilicate nitrite sodalite has been synthesized in a single step by low temperature (373 oK) hydrothermal technique. The product obtained was characterized using a combination of techniques including X-ray powder diffraction, IR, Raman spectroscopy, SEM, MAS NMR spectroscopy as well as thermogravimetry. Sodalite with an ideal composition was obtained after synthesis at 3730K and seven days duration using alkaline medium. The structural features of the Na8[GaSiO4]6(NO2)2 sodalite were investigated by IR, MAS NMR spectroscopy of 29Si and 23Na nuclei and by Reitveld refinement of X-ray powder diffraction data. The crystal structure of this sodalite has been refined in the space group P 4 3n; with a cell parameter 8.98386Å, V= 726.9 Å, (Rwp= 0.077 and Rp=0.0537) and Si-O-Ga angle is found to be 132.920 . MAS NMR study confirms complete ordering of Si and Ga in the gallosilicate framework. The surface area of single entity with stoichiometry Na8[GaSiO4]6(NO2)2 was found to be 8.083 x10-15 cm2/g.
[1] L. Pauling, The structure of sodalite and helvite, Z. Kristallogr., vol. 74,
pp. 213-225, 1930.
[2] L. Lons, and H. Schulz, Strukturverfeinerung von Sodalith,
Na8Si6Al6O24Cl2, Act. Crystallogr., vol. 23, pp.434-436, 1967.
[3] C. Z. Van Doorn, D. J. Schipper and P. T. Bolwijn, Optical Investigation
of Cathodochromic Sodalite, J. Electrochem. Soc., vol. 119, pp. 85-92,
1972.
[4] S. D. Mclaughan and D. J. Marshall, Paramagnetic resonance of F-type
centres in photochromic sodalites, Phys. Lett., vol. 32A, pp. 343-344,
1970.
[5] P. T. Bolwijn, D. J. Schipper and C. Z. Van Doorn, Cathodrochromic
Properties of Sodalite, J. Appl. Phys., vol. 43, pp. 132-137, 1972.
[6] S. Kowalak, M. Pawlowska, M. Monika, et al., Synthesis of ultramarine
from synthetic molecular sieves, Colloids surfaces A, Physico Chem.
Eng. Aspects, vol. 101, pp.179-185, 1951..
[7] I. Chang, Synthesis of Photochromic and Cathodochromic Sodalite
J.Electrochem. Soc., vol. 121, pp. 815-820, 1974.
[8] K. Suzuki, Y. Kiyozumi, S. Shin, et al., Synthesis of new gallosilicate
zeolite with sodalite structure, Zeolites, vol. 5, pp. 11-14, 1985.
[9] L. B. McCusker, W. M. Meier, K. Suzuki, et al., The crystal structure of
a sodium gallosilicate sodalite, Zeolites, vol. 6, pp. 388-91, 1986.
[10] J. M. Newsam, and J. D. Jorgensen, Gallosilicate sodalite further
syntheses and structural details, Zeolites, vol. 7, pp. 569-73, 1987.
[11] G. M. Johnson, and M. T. Weller, Synthesis and characterisation of
gallium and germanium containing sodalites, Studies in Surface Science
and Catalysis, vol. 105A, pp. 269-275, 1987.
[12] B. Xianhui, F. Pingyun, G. Thurman., et al., Hydrothermal Synthesis and
Structural Characterization of Zeolite-like Structures Based on Gallium
and Aluminum Germanates, Journal of the American Chemical Society,
vol.120, pp. 13389-13397, 1998.
[13] G. M. Johnson, & M. T. Weller, A Powder Neutron Diffraction Study of
Lithium Substituted Gallosilicate and Aluminogermanate Halide
Sodalites, Inorganic Chemistry, vol.38, pp. 2442-2450, 1999.
[14] G. M. Johnson, P. J. Mead and M. T. Weller, Structural trends in the
sodalite family, Phys. Chem. Chem., vol. 1, pp. 3709-371, 1999.
[15] T. M. Gesing, Structure and properties of tecto-gallosilicates. I.
Hydrosodalites and their phase transitions, Z. Kristallogr., vol. 215, pp.
510-517, 2000.
[16] T. M. Gesing, Structure and properties of tecto-gallosilicates II. Sodium
chloride, bromide and iodide sodalites, Z. Kristallogr., vol. 222, pp. 289-
296, 2007.
[17] J. C. Buhl, T. M. Gesing, T. Hoefs, et. al., Synthesis and crystal structure
of gallosilicate and aluminogermanate tetrahydroborate sodalites
Na8(GaSiO4)6(BH4)2 and Na8(AlGeO4)6(BH4)2, Journal of Solid State
Chemistry, vol.179, pp. 3877-3882, 2006.
[18] M. M. Murshed, and T. M. Gesing, Isomorphous gallium substitution in
the alumosilicate sodalite framework: synthesis and structural studies of
chloride and bromide containing phases, Z. Kristallogr., 2007, vol. 222,
pp. 341-349, 2007.
[19] M. M. Murshed, and T. M. Gesing, Gallium substitution in the
alumosilicate framework: synthesis and structural studies of hydro
sodalites, Z. Kristallogr., vol. 223, pp. 178-185, 2008.
[20] M.M. Murshed, A. J. Baer, and T. M. Gesing, Isomorphous framework
cation substitution in the alumosilicatesodalites: synthesis, structural and
spectroscopic studies of nitritecontaining phases, Z. Kristallogr., vol.
223, pp. 575-583, 2008.
[21] R. M. Barrer, J. F. Cole, and H. Sticher, Chemistry of soil minerals. Part
V. Low temperature hydrothermal transformations of kaolinite J.
Chem. Soc, pp. 2475-2485, 1968.
[22] F. Hund, Nitrite, Cyanide und Rhodanid-Sodalite, Z. Anorg. Allg. Chem,
vol. 511, pp. 225-230, 1984.
[23] D. J. Schipper, C.Z. Van Doorn, and P. T. Bolwijn, Preparation of
Cathodochromic Sodalites, J. A. Ceramic. Soc., vol. 55, pp. 256-559,
1972.
[24] G. M. Johnson, P. J. Mead, and M. T. Weller, Synthesis of a range of
anion-containing gallium and germanium sodalites, Micro. and Meso.
Mate, vol. 38, pp. 445-460, 2000.
[25] S. Bachmann and J. C. Buhl, Crystallization, characterization and
structure of nitrite aluminogermanate sodalite Na8(AlGeO4)6(NO2)2,
Micro. and Meso. Mate., vol. 28, pp. 35-47, 1999.
[26] M. E. Fleet, Structures of sodium alumino-germanate sodalites
(Na8(Al6Ge6O24)A2, A = Cl, Br, I), Acta. Cryst, vol. C45, pp. 843-847,
1989.
[27] W. Kiefer, and H. Bernstein, Resonance Raman spectroscopic study on
iodine in various organic solvents: Spectroscopic constants and half
band widths of the I2 vibration J. Appl. Spectro., vol.25, pp. 500-509,
1971.
[28] R. D. Shannon, Revised effective ionic radii and systematic studies of
interatomic distances in halides and chalcogenides, Acta. Crystallgr.,
vol.A32, pp. 751-767, 1976.
[29] P. B. Kempa, G. Engelhardt, J. C. Buhl, et al., X-ray powder diffraction
crystal structure analysis and 29Si, 23Na MAS n.m.r. studies of nitrite
sodalite, Na8(AlSiO4)6 (NO2)2, at 295 K, Zeolites, vol. 11, pp. 558-562, 1991.
[30] G. Engelhardt, S. Luger, J. C. Buhl, et al., 29Si MAS n.m.r. of
aluminosilicate sodalites: Correlations between chemical shifts and
structure parameters, Zeolites, vol. 9, pp. 182-186, 1989.
[31] E. Kundla, A. Samson and E. Lippma, High-resolution NMR of
quadrupolar nuclei in rotating solids, Chem. Phy. Letters, vol.83, pp.
229-232, 1981.
[32] J. C. Buhl, Hydrothermal synthesis and characterization of nitrite
sodalite single crystals, J. Crystal Growth, vol. 108, pp. 143-149, 1991.
[33] J. C. Buhl, F. Stief, M. Fechtelkord, et al., Synthesis, X-ray diffraction
and MAS NMR characteristics of nitrate cancrinite Na7.6(AlSiO4)6(NO3)1.6(H2O)2, J. Alloys and Comp., vol.305, pp. 93-102,
2000.
[1] L. Pauling, The structure of sodalite and helvite, Z. Kristallogr., vol. 74,
pp. 213-225, 1930.
[2] L. Lons, and H. Schulz, Strukturverfeinerung von Sodalith,
Na8Si6Al6O24Cl2, Act. Crystallogr., vol. 23, pp.434-436, 1967.
[3] C. Z. Van Doorn, D. J. Schipper and P. T. Bolwijn, Optical Investigation
of Cathodochromic Sodalite, J. Electrochem. Soc., vol. 119, pp. 85-92,
1972.
[4] S. D. Mclaughan and D. J. Marshall, Paramagnetic resonance of F-type
centres in photochromic sodalites, Phys. Lett., vol. 32A, pp. 343-344,
1970.
[5] P. T. Bolwijn, D. J. Schipper and C. Z. Van Doorn, Cathodrochromic
Properties of Sodalite, J. Appl. Phys., vol. 43, pp. 132-137, 1972.
[6] S. Kowalak, M. Pawlowska, M. Monika, et al., Synthesis of ultramarine
from synthetic molecular sieves, Colloids surfaces A, Physico Chem.
Eng. Aspects, vol. 101, pp.179-185, 1951..
[7] I. Chang, Synthesis of Photochromic and Cathodochromic Sodalite
J.Electrochem. Soc., vol. 121, pp. 815-820, 1974.
[8] K. Suzuki, Y. Kiyozumi, S. Shin, et al., Synthesis of new gallosilicate
zeolite with sodalite structure, Zeolites, vol. 5, pp. 11-14, 1985.
[9] L. B. McCusker, W. M. Meier, K. Suzuki, et al., The crystal structure of
a sodium gallosilicate sodalite, Zeolites, vol. 6, pp. 388-91, 1986.
[10] J. M. Newsam, and J. D. Jorgensen, Gallosilicate sodalite further
syntheses and structural details, Zeolites, vol. 7, pp. 569-73, 1987.
[11] G. M. Johnson, and M. T. Weller, Synthesis and characterisation of
gallium and germanium containing sodalites, Studies in Surface Science
and Catalysis, vol. 105A, pp. 269-275, 1987.
[12] B. Xianhui, F. Pingyun, G. Thurman., et al., Hydrothermal Synthesis and
Structural Characterization of Zeolite-like Structures Based on Gallium
and Aluminum Germanates, Journal of the American Chemical Society,
vol.120, pp. 13389-13397, 1998.
[13] G. M. Johnson, & M. T. Weller, A Powder Neutron Diffraction Study of
Lithium Substituted Gallosilicate and Aluminogermanate Halide
Sodalites, Inorganic Chemistry, vol.38, pp. 2442-2450, 1999.
[14] G. M. Johnson, P. J. Mead and M. T. Weller, Structural trends in the
sodalite family, Phys. Chem. Chem., vol. 1, pp. 3709-371, 1999.
[15] T. M. Gesing, Structure and properties of tecto-gallosilicates. I.
Hydrosodalites and their phase transitions, Z. Kristallogr., vol. 215, pp.
510-517, 2000.
[16] T. M. Gesing, Structure and properties of tecto-gallosilicates II. Sodium
chloride, bromide and iodide sodalites, Z. Kristallogr., vol. 222, pp. 289-
296, 2007.
[17] J. C. Buhl, T. M. Gesing, T. Hoefs, et. al., Synthesis and crystal structure
of gallosilicate and aluminogermanate tetrahydroborate sodalites
Na8(GaSiO4)6(BH4)2 and Na8(AlGeO4)6(BH4)2, Journal of Solid State
Chemistry, vol.179, pp. 3877-3882, 2006.
[18] M. M. Murshed, and T. M. Gesing, Isomorphous gallium substitution in
the alumosilicate sodalite framework: synthesis and structural studies of
chloride and bromide containing phases, Z. Kristallogr., 2007, vol. 222,
pp. 341-349, 2007.
[19] M. M. Murshed, and T. M. Gesing, Gallium substitution in the
alumosilicate framework: synthesis and structural studies of hydro
sodalites, Z. Kristallogr., vol. 223, pp. 178-185, 2008.
[20] M.M. Murshed, A. J. Baer, and T. M. Gesing, Isomorphous framework
cation substitution in the alumosilicatesodalites: synthesis, structural and
spectroscopic studies of nitritecontaining phases, Z. Kristallogr., vol.
223, pp. 575-583, 2008.
[21] R. M. Barrer, J. F. Cole, and H. Sticher, Chemistry of soil minerals. Part
V. Low temperature hydrothermal transformations of kaolinite J.
Chem. Soc, pp. 2475-2485, 1968.
[22] F. Hund, Nitrite, Cyanide und Rhodanid-Sodalite, Z. Anorg. Allg. Chem,
vol. 511, pp. 225-230, 1984.
[23] D. J. Schipper, C.Z. Van Doorn, and P. T. Bolwijn, Preparation of
Cathodochromic Sodalites, J. A. Ceramic. Soc., vol. 55, pp. 256-559,
1972.
[24] G. M. Johnson, P. J. Mead, and M. T. Weller, Synthesis of a range of
anion-containing gallium and germanium sodalites, Micro. and Meso.
Mate, vol. 38, pp. 445-460, 2000.
[25] S. Bachmann and J. C. Buhl, Crystallization, characterization and
structure of nitrite aluminogermanate sodalite Na8(AlGeO4)6(NO2)2,
Micro. and Meso. Mate., vol. 28, pp. 35-47, 1999.
[26] M. E. Fleet, Structures of sodium alumino-germanate sodalites
(Na8(Al6Ge6O24)A2, A = Cl, Br, I), Acta. Cryst, vol. C45, pp. 843-847,
1989.
[27] W. Kiefer, and H. Bernstein, Resonance Raman spectroscopic study on
iodine in various organic solvents: Spectroscopic constants and half
band widths of the I2 vibration J. Appl. Spectro., vol.25, pp. 500-509,
1971.
[28] R. D. Shannon, Revised effective ionic radii and systematic studies of
interatomic distances in halides and chalcogenides, Acta. Crystallgr.,
vol.A32, pp. 751-767, 1976.
[29] P. B. Kempa, G. Engelhardt, J. C. Buhl, et al., X-ray powder diffraction
crystal structure analysis and 29Si, 23Na MAS n.m.r. studies of nitrite
sodalite, Na8(AlSiO4)6 (NO2)2, at 295 K, Zeolites, vol. 11, pp. 558-562, 1991.
[30] G. Engelhardt, S. Luger, J. C. Buhl, et al., 29Si MAS n.m.r. of
aluminosilicate sodalites: Correlations between chemical shifts and
structure parameters, Zeolites, vol. 9, pp. 182-186, 1989.
[31] E. Kundla, A. Samson and E. Lippma, High-resolution NMR of
quadrupolar nuclei in rotating solids, Chem. Phy. Letters, vol.83, pp.
229-232, 1981.
[32] J. C. Buhl, Hydrothermal synthesis and characterization of nitrite
sodalite single crystals, J. Crystal Growth, vol. 108, pp. 143-149, 1991.
[33] J. C. Buhl, F. Stief, M. Fechtelkord, et al., Synthesis, X-ray diffraction
and MAS NMR characteristics of nitrate cancrinite Na7.6(AlSiO4)6(NO3)1.6(H2O)2, J. Alloys and Comp., vol.305, pp. 93-102,
2000.
@article{"International Journal of Chemical, Materials and Biomolecular Sciences:64693", author = "Ashok V. Borhade and Sanjay G. Wakchaure", title = "Synthesis and Characterization of Gallosilicate Sodalite Containing NO2- Ions", abstract = "Pure phase gallosilicate nitrite sodalite has been synthesized in a single step by low temperature (373 oK) hydrothermal technique. The product obtained was characterized using a combination of techniques including X-ray powder diffraction, IR, Raman spectroscopy, SEM, MAS NMR spectroscopy as well as thermogravimetry. Sodalite with an ideal composition was obtained after synthesis at 3730K and seven days duration using alkaline medium. The structural features of the Na8[GaSiO4]6(NO2)2 sodalite were investigated by IR, MAS NMR spectroscopy of 29Si and 23Na nuclei and by Reitveld refinement of X-ray powder diffraction data. The crystal structure of this sodalite has been refined in the space group P 4 3n; with a cell parameter 8.98386Å, V= 726.9 Å, (Rwp= 0.077 and Rp=0.0537) and Si-O-Ga angle is found to be 132.920 . MAS NMR study confirms complete ordering of Si and Ga in the gallosilicate framework. The surface area of single entity with stoichiometry Na8[GaSiO4]6(NO2)2 was found to be 8.083 x10-15 cm2/g.
", keywords = "Gallosilicate, hydrothermal, nitrite, Reitveldrefinement.", volume = "4", number = "1", pages = "126-6", }
