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Journal of the Optical Society of America

Journal of the Optical Society of America

  • Vol. 42, Iss. 3 — Mar. 1, 1952
  • pp: 149–159

Notes on the Practice of Infrared Spectroscopy

R. C. LORD, R. S. McDONALD, and FOIL A. MILLER  »View Author Affiliations


JOSA, Vol. 42, Issue 3, pp. 149-159 (1952)
http://dx.doi.org/10.1364/JOSA.42.000149


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Abstract

Miscellaneous techniques for infrared prism spectroscopy are described in detail. These include: techniques for cleaving, cutting, and polishing alkali halide crystals for absorption cell windows; construction of absorption cells for liquids and gases, including some suitable for high and low temperatures and one of long path; the measurement of cell thickness; removal of atmospheric absorption; techniques useful for wavelengths above twenty-five microns; formulas for recording inks. A modified source-optical system and a method of calibration adjustment for Perkin-Elmer Model 12 instruments are also discussed.

Citation
R. C. LORD, R. S. McDONALD, and FOIL A. MILLER, "Notes on the Practice of Infrared Spectroscopy," J. Opt. Soc. Am. 42, 149-159 (1952)
http://www.opticsinfobase.org/josa/abstract.cfm?URI=josa-42-3-149


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References

  1. V. Z. Williams, Rev. Sci. Instr. 19, 135–178 (1948).
  2. Faraday Soc. Symposium, Trans. Faraday Soc. 41, 171 (1945).
  3. Instruction Manual, Model 12C Infrared Spectrometer, Perkin-Elmer Corporation, Norwalk, Connecticut (1949).
  4. Harrison, Lord, and Loofbourow, Practical Spectroscopy (Prentice-Hall, Inc., New York, 1948).
  5. A brief bibliography appears on p. 165 of reference 1. References to special cells for high and low temperatures will be given later in the present article.
  6. From Harshaw Chemical Company, 1945 E. 97th Street, Cleveland 6, Ohio; or Optovac Company, 59 Summer Street, North Brookfield, Massachusetts.
  7. Obtainable from the Century Glove Corporation, 165 Vanderpool St., Newark 5, New Jersey (lintless polishing cloths).
  8. Obtainable from the Fisher Scientific Company, Pittsburgh, Pennsylvania, as "levigated alumina for dry polishing," or from the Carborundum Company, Niagara Falls, New York, as "Aloxite Brand" Aluminum Oxide Optical Finishing Powder (available in several grades).
  9. This is a mixture of rare earth oxides. It is obtainable from the W. F. and John Barnes Company, 415 South Water Street, Rockford, Illinois. The authors are indebted to John Unertl, Jr., of the Unertl Optical Company for drawing this to their attention.
  10. See H. W. Thompson and D. H. Whiffen, Trans. Faraday Soc. 41, 180 (1945).
  11. Polishing pitch can be obtained from American Optical Company, Southbridge, Massachusetts, whose "Black Jack M405S" pitch is suitable for polishing alkali halides, and from Universal Shellac and Supply Company, 425 Morgan Avenue, Brooklyn 22, New York. In laboratories whose temperature varies seasonally, the pitch used for summer work should be stiffer than for cooler seasons.
  12. The suspension is applied freshly shaken from a bottle with a short glass tube through the stopper.
  13. The authors learned of this from Dr. R. J. Meltzer of the Bausch and Lomb Optical Company.
  14. J. J. McGovern and R. A. Friedel, J. Opt. Soc. Am. 37, 660 (1947).
  15. N. D. Coggeshall, Rev. Sci. Instr. 17, 343 (1946); see also reference 5.
  16. These cells can be conveniently stored in a standard large chemical dessicator. The plate in such dessicators can be used unchanged, or can be replaced by a floor equipped with rows of slotted posts so spaced that the cells slide into them as they do into the spectrometer cell holder. Twenty or more holders of this type will fit into a 14-inch dessicator.
  17. Metal foils in various thicknesses can be obtained from Standard Rolling Mills, 196 Diamond Street, Brooklyn 22, New York.
  18. This technique was learned from the Physics Division, Stamford Research Laboratories, American Cyanamid Company.
  19. D. C. Smith and E. C. Miller, J. Opt. Soc. Am. 34, 130 (1944).
  20. G. B. B. M. Sutherland and H. A. Willis, Trans. Faraday Soc. 41, 181 (1945).
  21. High temperature cells: L. G. Smith, Rev. Sci. Instr. 13, 65 (1942) (gases, -100 to +200°C); R. E. Richards and H. W. Thompson, Trans. Faraday Soc. 41, 183 (1945) (solids and liquids, up to 200°C); G. L. Simard and J. E. Steger, Rev. Sci. Instr. 17, 156 (1946) (gases, up to 550°C but cooling below +150°C fractures the cell); H. J. Bernstein, J. Chem. Phys. 17, 258 (1949) (gases, close control of temperatures (±1°C) up to 150°C); H. S. Gutowsky and C. J. Hoffman, J. Am. Chem. Soc. 72, 5751 (1950) (gases, up to 250°C 1 meter path); L. Brown and P. Holliday, J. Sci. Instr. 28, 27 (1951) (liquids, up to 270°C). Low temperature cells: J. Zunino, Z. Physik 100, 335 (1936) (reflection type with nonuniform film condensed on mirror); Conn, Lee, and Sutherland, Proc. Roy. Soc. (London) A176, 484 (1940) (similar in principle to above); W. H. Avery and C. F. Ellis, J. Chem. Phys. 10, 10 (1942) (similar in principle to above); McMahon, Hainer, and King, J. Opt. Soc. Am. 39, 786 (1949) (transmission type of excellent design for range 4°-300°K); Holden, Taylor, and Johnston, J. Opt. Soc. Am. 40, 757 (1950) (transmission type, variable thickness, 35°-300°K); J. Powling and H. J. Bernstein, J. Am. Chem. Soc. 73, 1815 (1951) (transmission type for liquids, from about -75° to +25°C).
  22. F. A. Miller and S. D. Koch, J. Am. Chem. Soc. 70, 1890 (1948).
  23. See L. P. Salter, Bachelor's thesis, Department of Chemistry, Massachusetts Institute of Technology, September, 1948, for a detailed account. A similar cell has been described briefly by Wagner and Hornig, J. Chem. Phys. 18, 296 (1950); see also Axford and Rank, ibid. 18, 51 (1950); Walsh and Willis, ibid. 18, 550 (1950); Bovey, J. Opt. Soc. Am. 41, 381 (1951).
  24. Certain aspects of this technique were communicated to us by Professor L. Harris and Dr. C. M. Cobb.
  25. These seals are purchasable from the Commercial Service Section, Tube Division, General Electric Company, Schenectady, New York.
  26. Some recent references are: J. U. White, J. Opt. Soc. Am. 32, 285 (1942); Perkin-Elmer Instruction Manual (reference 3), p. 34
  27. See White (reference 26) for details.
  28. A drawing of this device for transmitting motion into an evacuated housing is shown on p. 37 of Bomke, Vakuumspektroskopie (Johann Ambrosius Barth, Leipzig, Germany, 1937). Bomke credits the device to J. J. Hopfield.
  29. J. U. White, J. Opt. Soc. Am. 37, 713 (1947).
  30. N. B. Colthup, Perkin-Elmer Instrument News 2, No. 4, 6 (1951).
  31. These crystals may be purchased from the firms cited in reference 6 and also from Pilot Chemicals, Inc., 47 Felton St., Waltham, Massachusetts.
  32. E. K. Plyler and F. P. Phelps, J. Opt. Soc. Am. 41, 209 (1951).
  33. Appendix (dated 1950) to Perkin-Elmer manual (reference 3); see also E. K. Plyler, Bur. Standards J. Research 41, 125 (1948).
  34. Brown Instrument Company, Philadelphia 44, Pennsylvania, Part B-15266.
  35. Obtainable from Eastman Kodak Company, Organic Chemical Sales Division, Rochester 4, New York (E. K. No. 1751); the use of Orange G and Malachite green was learned from Dr. D. H. Anderson of the Eastman Kodak Company.
  36. Obtainable from Eastman Kodak Company (E. K. No. 1264), or from Fisher Scientific Company, Pittsburgh, Pennsylvania.

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