Abstract

The infrared spectra of water sorbed on several synthetic zeolites is discussed in terms of the molecular species present. Three different sets of bands are observed for water as the water content on the zeolite is varied. Evidence for surface OH groups for synthetic zeolites is presented. A technique for reducing the scattered light of zeolite powders by wetting them is suggested. It is possible to study surface OH groups by this technique using D2O as the wetting agent. A mechanism whereby surface OH groups can form in sodium and ammonium zeolites is given. The results obtained for water sorbed on sodium zeolites differs to some extent from those reported previously.

© 1960 Optical Society of America

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References

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  1. J. E. Mapes and R. P. Eischens, J. Phys. Chem. 58, 1059 (1954).
    [CrossRef]
  2. G. J. C. Frohnsdorff and G. L. Kington, Proc. Roy. Soc. (London) A247, 469 (1958).
  3. R. P. Eischens, J. Chem. Educ. 35, 385 (1958).
    [CrossRef]
  4. R. S. McDonald, J. Am. Chem. Soc. 79, 850 (1957).
    [CrossRef]
  5. Advances in Catalysis,  10, 41 (1958).
  6. H. A. Szymanski, R. Povinelli, D. Stamires, and G. Lynch, Anal. Chem. 31, 2110 (1959).
    [CrossRef]
  7. R. M. Barrer, F. W. Bultitude, and T. W. Sutherland, Trans. Faraday Soc. 53, 1111 (1957).
    [CrossRef]
  8. D. W. Breck, E. M. Flanigen, R. M. Milton, and T. B. Reed, meeting of the American Chemical Society, September, 1958, Chicago, Illinois, abstract 134.
  9. R. M. Barrer, Proceedings of the 10th Symposium of the Colston Research Society, March 24–27, 1958.
  10. D. W. Breck, W. G. Eversale, R. M. Milton, T. B. Reed, and T. L. Thomas, J. Am. Chem. Soc. 78, 5963 (1956).
    [CrossRef]
  11. R. M. Barrer, Nature 164, 112 (1949).
    [CrossRef]
  12. A. N. Terenin, Mikrochim. Acta 2, 467 (1955).
    [CrossRef]
  13. H. A. Benesi and A. C. Jones, J. Phys. Chem. 63, 179 (1959).
    [CrossRef]
  14. A. M. Buswell, K. Krebs, and W. H. Rodebush, J. Am. Chem. Soc. 59, 2603 (1937).
    [CrossRef]
  15. G. C. Pimental, C. W. Garland, and G. Jura, J. Am. Chem. Soc. 75, 803 (1953).
    [CrossRef]
  16. J. T. Brqumholtz, G. E. Hall, F. C. Mann, and N. Sheppard, J. Chem. Soc.1959, 868.
  17. A. N. Terenin, Gordon Research Conference on Infrared Spectroscopy, August, 1957.
  18. T. H. Milliken and G. A. Mills, Discussions Faraday Soc. No. 8,  279 (1950).
  19. M. Falk and P. A. Giguere, Can. J. Chem. 35, 1195 (1957).
    [CrossRef]

1959 (2)

H. A. Szymanski, R. Povinelli, D. Stamires, and G. Lynch, Anal. Chem. 31, 2110 (1959).
[CrossRef]

H. A. Benesi and A. C. Jones, J. Phys. Chem. 63, 179 (1959).
[CrossRef]

1958 (3)

G. J. C. Frohnsdorff and G. L. Kington, Proc. Roy. Soc. (London) A247, 469 (1958).

R. P. Eischens, J. Chem. Educ. 35, 385 (1958).
[CrossRef]

Advances in Catalysis,  10, 41 (1958).

1957 (3)

R. S. McDonald, J. Am. Chem. Soc. 79, 850 (1957).
[CrossRef]

R. M. Barrer, F. W. Bultitude, and T. W. Sutherland, Trans. Faraday Soc. 53, 1111 (1957).
[CrossRef]

M. Falk and P. A. Giguere, Can. J. Chem. 35, 1195 (1957).
[CrossRef]

1956 (1)

D. W. Breck, W. G. Eversale, R. M. Milton, T. B. Reed, and T. L. Thomas, J. Am. Chem. Soc. 78, 5963 (1956).
[CrossRef]

1955 (1)

A. N. Terenin, Mikrochim. Acta 2, 467 (1955).
[CrossRef]

1954 (1)

J. E. Mapes and R. P. Eischens, J. Phys. Chem. 58, 1059 (1954).
[CrossRef]

1953 (1)

G. C. Pimental, C. W. Garland, and G. Jura, J. Am. Chem. Soc. 75, 803 (1953).
[CrossRef]

1950 (1)

T. H. Milliken and G. A. Mills, Discussions Faraday Soc. No. 8,  279 (1950).

1949 (1)

R. M. Barrer, Nature 164, 112 (1949).
[CrossRef]

1937 (1)

A. M. Buswell, K. Krebs, and W. H. Rodebush, J. Am. Chem. Soc. 59, 2603 (1937).
[CrossRef]

Barrer, R. M.

R. M. Barrer, F. W. Bultitude, and T. W. Sutherland, Trans. Faraday Soc. 53, 1111 (1957).
[CrossRef]

R. M. Barrer, Nature 164, 112 (1949).
[CrossRef]

R. M. Barrer, Proceedings of the 10th Symposium of the Colston Research Society, March 24–27, 1958.

Benesi, H. A.

H. A. Benesi and A. C. Jones, J. Phys. Chem. 63, 179 (1959).
[CrossRef]

Breck, D. W.

D. W. Breck, W. G. Eversale, R. M. Milton, T. B. Reed, and T. L. Thomas, J. Am. Chem. Soc. 78, 5963 (1956).
[CrossRef]

D. W. Breck, E. M. Flanigen, R. M. Milton, and T. B. Reed, meeting of the American Chemical Society, September, 1958, Chicago, Illinois, abstract 134.

Brqumholtz, J. T.

J. T. Brqumholtz, G. E. Hall, F. C. Mann, and N. Sheppard, J. Chem. Soc.1959, 868.

Bultitude, F. W.

R. M. Barrer, F. W. Bultitude, and T. W. Sutherland, Trans. Faraday Soc. 53, 1111 (1957).
[CrossRef]

Buswell, A. M.

A. M. Buswell, K. Krebs, and W. H. Rodebush, J. Am. Chem. Soc. 59, 2603 (1937).
[CrossRef]

Eischens, R. P.

R. P. Eischens, J. Chem. Educ. 35, 385 (1958).
[CrossRef]

J. E. Mapes and R. P. Eischens, J. Phys. Chem. 58, 1059 (1954).
[CrossRef]

Eversale, W. G.

D. W. Breck, W. G. Eversale, R. M. Milton, T. B. Reed, and T. L. Thomas, J. Am. Chem. Soc. 78, 5963 (1956).
[CrossRef]

Falk, M.

M. Falk and P. A. Giguere, Can. J. Chem. 35, 1195 (1957).
[CrossRef]

Flanigen, E. M.

D. W. Breck, E. M. Flanigen, R. M. Milton, and T. B. Reed, meeting of the American Chemical Society, September, 1958, Chicago, Illinois, abstract 134.

Frohnsdorff, G. J. C.

G. J. C. Frohnsdorff and G. L. Kington, Proc. Roy. Soc. (London) A247, 469 (1958).

Garland, C. W.

G. C. Pimental, C. W. Garland, and G. Jura, J. Am. Chem. Soc. 75, 803 (1953).
[CrossRef]

Giguere, P. A.

M. Falk and P. A. Giguere, Can. J. Chem. 35, 1195 (1957).
[CrossRef]

Hall, G. E.

J. T. Brqumholtz, G. E. Hall, F. C. Mann, and N. Sheppard, J. Chem. Soc.1959, 868.

Jones, A. C.

H. A. Benesi and A. C. Jones, J. Phys. Chem. 63, 179 (1959).
[CrossRef]

Jura, G.

G. C. Pimental, C. W. Garland, and G. Jura, J. Am. Chem. Soc. 75, 803 (1953).
[CrossRef]

Kington, G. L.

G. J. C. Frohnsdorff and G. L. Kington, Proc. Roy. Soc. (London) A247, 469 (1958).

Krebs, K.

A. M. Buswell, K. Krebs, and W. H. Rodebush, J. Am. Chem. Soc. 59, 2603 (1937).
[CrossRef]

Lynch, G.

H. A. Szymanski, R. Povinelli, D. Stamires, and G. Lynch, Anal. Chem. 31, 2110 (1959).
[CrossRef]

Mann, F. C.

J. T. Brqumholtz, G. E. Hall, F. C. Mann, and N. Sheppard, J. Chem. Soc.1959, 868.

Mapes, J. E.

J. E. Mapes and R. P. Eischens, J. Phys. Chem. 58, 1059 (1954).
[CrossRef]

McDonald, R. S.

R. S. McDonald, J. Am. Chem. Soc. 79, 850 (1957).
[CrossRef]

Milliken, T. H.

T. H. Milliken and G. A. Mills, Discussions Faraday Soc. No. 8,  279 (1950).

Mills, G. A.

T. H. Milliken and G. A. Mills, Discussions Faraday Soc. No. 8,  279 (1950).

Milton, R. M.

D. W. Breck, W. G. Eversale, R. M. Milton, T. B. Reed, and T. L. Thomas, J. Am. Chem. Soc. 78, 5963 (1956).
[CrossRef]

D. W. Breck, E. M. Flanigen, R. M. Milton, and T. B. Reed, meeting of the American Chemical Society, September, 1958, Chicago, Illinois, abstract 134.

Pimental, G. C.

G. C. Pimental, C. W. Garland, and G. Jura, J. Am. Chem. Soc. 75, 803 (1953).
[CrossRef]

Povinelli, R.

H. A. Szymanski, R. Povinelli, D. Stamires, and G. Lynch, Anal. Chem. 31, 2110 (1959).
[CrossRef]

Reed, T. B.

D. W. Breck, W. G. Eversale, R. M. Milton, T. B. Reed, and T. L. Thomas, J. Am. Chem. Soc. 78, 5963 (1956).
[CrossRef]

D. W. Breck, E. M. Flanigen, R. M. Milton, and T. B. Reed, meeting of the American Chemical Society, September, 1958, Chicago, Illinois, abstract 134.

Rodebush, W. H.

A. M. Buswell, K. Krebs, and W. H. Rodebush, J. Am. Chem. Soc. 59, 2603 (1937).
[CrossRef]

Sheppard, N.

J. T. Brqumholtz, G. E. Hall, F. C. Mann, and N. Sheppard, J. Chem. Soc.1959, 868.

Stamires, D.

H. A. Szymanski, R. Povinelli, D. Stamires, and G. Lynch, Anal. Chem. 31, 2110 (1959).
[CrossRef]

Sutherland, T. W.

R. M. Barrer, F. W. Bultitude, and T. W. Sutherland, Trans. Faraday Soc. 53, 1111 (1957).
[CrossRef]

Szymanski, H. A.

H. A. Szymanski, R. Povinelli, D. Stamires, and G. Lynch, Anal. Chem. 31, 2110 (1959).
[CrossRef]

Terenin, A. N.

A. N. Terenin, Mikrochim. Acta 2, 467 (1955).
[CrossRef]

A. N. Terenin, Gordon Research Conference on Infrared Spectroscopy, August, 1957.

Thomas, T. L.

D. W. Breck, W. G. Eversale, R. M. Milton, T. B. Reed, and T. L. Thomas, J. Am. Chem. Soc. 78, 5963 (1956).
[CrossRef]

Advances in Catalysis (1)

Advances in Catalysis,  10, 41 (1958).

Anal. Chem. (1)

H. A. Szymanski, R. Povinelli, D. Stamires, and G. Lynch, Anal. Chem. 31, 2110 (1959).
[CrossRef]

Can. J. Chem. (1)

M. Falk and P. A. Giguere, Can. J. Chem. 35, 1195 (1957).
[CrossRef]

Discussions Faraday Soc. No. 8 (1)

T. H. Milliken and G. A. Mills, Discussions Faraday Soc. No. 8,  279 (1950).

J. Am. Chem. Soc. (4)

R. S. McDonald, J. Am. Chem. Soc. 79, 850 (1957).
[CrossRef]

D. W. Breck, W. G. Eversale, R. M. Milton, T. B. Reed, and T. L. Thomas, J. Am. Chem. Soc. 78, 5963 (1956).
[CrossRef]

A. M. Buswell, K. Krebs, and W. H. Rodebush, J. Am. Chem. Soc. 59, 2603 (1937).
[CrossRef]

G. C. Pimental, C. W. Garland, and G. Jura, J. Am. Chem. Soc. 75, 803 (1953).
[CrossRef]

J. Chem. Educ. (1)

R. P. Eischens, J. Chem. Educ. 35, 385 (1958).
[CrossRef]

J. Phys. Chem. (2)

J. E. Mapes and R. P. Eischens, J. Phys. Chem. 58, 1059 (1954).
[CrossRef]

H. A. Benesi and A. C. Jones, J. Phys. Chem. 63, 179 (1959).
[CrossRef]

Mikrochim. Acta (1)

A. N. Terenin, Mikrochim. Acta 2, 467 (1955).
[CrossRef]

Nature (1)

R. M. Barrer, Nature 164, 112 (1949).
[CrossRef]

Proc. Roy. Soc. (London) (1)

G. J. C. Frohnsdorff and G. L. Kington, Proc. Roy. Soc. (London) A247, 469 (1958).

Trans. Faraday Soc. (1)

R. M. Barrer, F. W. Bultitude, and T. W. Sutherland, Trans. Faraday Soc. 53, 1111 (1957).
[CrossRef]

Other (4)

D. W. Breck, E. M. Flanigen, R. M. Milton, and T. B. Reed, meeting of the American Chemical Society, September, 1958, Chicago, Illinois, abstract 134.

R. M. Barrer, Proceedings of the 10th Symposium of the Colston Research Society, March 24–27, 1958.

J. T. Brqumholtz, G. E. Hall, F. C. Mann, and N. Sheppard, J. Chem. Soc.1959, 868.

A. N. Terenin, Gordon Research Conference on Infrared Spectroscopy, August, 1957.

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Figures (2)

Fig. 1
Fig. 1

Dashed curve, spectra of a fairly thick sample of nearly anhydrous zeolite; undashed curve, spectra of same zeolite wetted slightly with deuterium oxide.

Fig. 2
Fig. 2

(A) Spectra of NaX zeolite saturated with D2O; (B) spectra of NH4X zeolite saturated with D2O; (C) spectra of anhydrous NaX zeolite used to obtain spectra (A).

Tables (4)

Tables Icon

Table I Infrared frequencies for water sorbed on NaX synthetic zeolite. All samples were in pellet form and rechecked in powder form. Spectra were taken at the temperature indicated.

Tables Icon

Table II Infrared frequencies for water sorbed on NH4X zeolites. All samples were in pellet form and rechecked in powder form. Pressure was maintained constant at 0.03 mm Hg. Spectra were taken at the activation temperature except where indicated.

Tables Icon

Table III Infrared frequencies for NaX, NH4X, and NaA zeolites. All samples were activated at the temperatures listed for several hours and then run at room temperature in Nujol mull.

Tables Icon

Table IV Infrared frequencies of deuterium oxide sorbed on NaX and NH4X zeolites. Samples were run as powders and in Nujol mull.

Equations (1)

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Na 76 + ( H 3 O ) 7 + [ ( AlO 2 ) 83 ( SiO 2 ) 109 ] .