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Determination of Amorphous Phase in Quartz Powder by X-Ray Powder Diffractometry

Published online by Cambridge University Press:  10 January 2013

Toshihiro Nakamura ,
Katsumi Sameshima ,
Kiyoyuki Okunaga ,
Yoshitaka Sugiura  and
Jun Sato
Toshihiro Nakamura
Affiliation:
Department of Industrial Chemistry, Faculty of Engineering, Meiji University, Higashimita, Tama-ku, Kawasaki, 214, Japan
Katsumi Sameshima
Affiliation:
Department of Industrial Chemistry, Faculty of Engineering, Meiji University, Higashimita, Tama-ku, Kawasaki, 214, Japan
Kiyoyuki Okunaga
Affiliation:
Department of Industrial Chemistry, Faculty of Engineering, Meiji University, Higashimita, Tama-ku, Kawasaki, 214, Japan
Yoshitaka Sugiura
Affiliation:
Department of Industrial Chemistry, Faculty of Engineering, Meiji University, Higashimita, Tama-ku, Kawasaki, 214, Japan
Jun Sato
Affiliation:
Department of Industrial Chemistry, Faculty of Engineering, Meiji University, Higashimita, Tama-ku, Kawasaki, 214, Japan
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Abstract

A powder diffraction method was applied to the quantitative analysis of amorphous silica in several quartz powders. Two calibration methods, i.e., direct analysis and the standard addition method were examined. Calibration mixtures were made by mixing a standard silica gel powder ground to under 5 μm particle size with a matrix quartz powder which was ground to 10 to 40 μm particle size and treated with NaOH solution to remove the amorphous phase caused by grinding. Intensity of the amorphous halo was measured at 23.0° 2θ, and the background intensity at 53.0° 2θ was subtracted. Linear calibration curves were obtained over the ranges of 0 to 50 wt% by direct analysis and 0 to 20 wt% by standard addition methods, respectively. The analytical results obtained by the two calibration methods were in good agreement with each other. The relative standard deviations for 4.3 wt% of amorphous silica were 4.6% by the direct analysis and 5.4% by the standard addition method. These methods were successfully applied to a correction of reference intensity ratios (RIR) for several quartz powders containing amorphous silica. After the correction for amorphous content, the relative standard deviations of the RIR values for quartz powders became smaller.

Type
Research Article
Information
Powder Diffraction , Volume 4 , Issue 1 , March 1989 , pp. 9 - 13
Copyright
Copyright © Cambridge University Press 1989

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References

Alexander, L. E. & Klug, H. P. (1948). Anal. Chem. 20, 886–889.CrossRefGoogle Scholar
Altree-Williams, S., Byrnes, J. G. & Jordan, B. (1981). Analyst 106, 69–75.CrossRefGoogle Scholar
Calvert, L. D., Sirianni, A. F., Gainsford, C. R. & Hubbard, C. R. (1983). In Adv. X-Ray Anal. 26, 105–110. New York: Plenum.Google Scholar
Chung, F. H. & Scott, R. W. (1973). J. Appl. Crystallogr. 6, 225–236.CrossRefGoogle Scholar
Chung, F. H. (1974a). J. Appl. Crystallogr. 7, 519–525.CrossRefGoogle Scholar
Chung, F. H. (1974b). J. Appl. Crystallogr. 7, 526–531.CrossRefGoogle Scholar
Chung, F. H. (1974c). In Adv. X-Ray Anal. 17, 106–115. New York: Plenum.Google Scholar
Clark, N. H. & Preston, R. J. (1974). X-Ray Spectrom. 3, 21–25.CrossRefGoogle Scholar
Copeland, L. E. & Bragg, R. H. (1958). Anal. Chem. 30, 196–201.CrossRefGoogle Scholar
Corba, J. (1972). Silikaty (Prague) 4, 325–329.Google Scholar
Flörke, O. W. & Saalfeld, H. (1955). Z. Kristallogr., Kristallgeom., Kristallphys., Kristallchem. 106, 460–466.Google Scholar
Fukasawa, T., Iwatsuki, M. & Kawakubo, S. (1978). Bunseki Kagaku 27, 90–95.CrossRefGoogle Scholar
Fukasawa, T., Iwatsuki, M. & Pajapakse, L. (1984). Anal. Chim. Acta 185, 247–256.CrossRefGoogle Scholar
Hubbard, C.R., Evans, E.H. & Smith, D.K. (1976). J. Appl. Crystallogr. 9, 167–174.Google Scholar
Itoh, H., Sasuga, H., Nakamura, T. & Sato, J. (1981). Anal. Chim. Acta 128, 269–272.CrossRefGoogle Scholar
Johnson, D. J. (1981). In Adv. X-Ray Anal. 24, 25–36. New York: Plenum.Google Scholar
Klug, H. P. & Alexander, L. E. (1974). X-Ray Diffraction Procedures for Polycrystalline and Amorphous Materials, 2nd ed., 356–368. New York: John Wiley and Sons.Google Scholar
Knudsen, T. (1976). X-Ray Spectrom. 5, 197–199.CrossRefGoogle Scholar
Krimm, S. & Tobolsky, A. V. (1951). J. Polym. Sci. 7, 57–76.CrossRefGoogle Scholar
Kubo, T. (1978). Mechanochemistry Gairon, 2nd ed., 203–205. Tokyo: Tokyo Kagakudojin.Google Scholar
Leroux, J.Lennox, D. H. & Kay, K. (1953). Anal. Chem. 25, 740–743.CrossRefGoogle Scholar
Nakamura, T. & Sasuga, H. (1979). Mem. Inst. Sci. Tech. Meiji Univ. 18, 12–1 to 12–8.Google Scholar
Nakamura, T. & Sasuga, H. (1980). Bunseki Kagaku, 29, 467–471.CrossRefGoogle Scholar
Nakamura, T. (1987). Adv. X-Ray Chem. Anal. Jpn. 18, 93–103.Google Scholar
Nash, D.B. (1964). In Adv. X-Ray Anal. 7, 209–228. New York: Plenum.Google Scholar
NBS-SRM 1878. McKenzie, R. L. and Hubbard, C.R. (1983). Certificate SRM1878. Respirable Alpha Quarta: Quantitative X-Ray Powder Diffraction Standard. Office of Standard Reference Materials, Natl. Bur. Standards, Gaithersburg, MD 20899.Google Scholar
Niskanen, E. (1964). Am. Mineral. 49, 705–714.Google Scholar
Okamoto, T., Kimura, M. & Nakajuma, K. (1973). J. Sci. Instrum. 3, 414–417.CrossRefGoogle Scholar
Parrish, W. & Huang, T. C. (1983). In Adv. X-Ray Anal. 26, 321–330. New York: Plenum.Google Scholar
Patzak, I. & Konopicky, K. (1966). Ber. Dtsch. Keram. Ges. 43, 632–639.Google Scholar
Redmond, J. C. (1947). Ind. Eng. Chem. Anal. Ed. 19, 773–777.Google Scholar
Sahores, J. J. (1972). In Adv. X-Ray Anal. 16, 186–197. New York: Plenum.Google Scholar
Silva, P., Bliss, M. & Scheetz, E. (1985). In Adv. X-Ray Anal. 28, 321–330. New York: Plenum.Google Scholar
Smith, S. T., Snyder, R. L. & Brownel, W. E. (1979). In Adv. X-Ray Anal. 22, 77–87. New York: Plenum.Google Scholar
Statton, W. O. (1963). J. Appl. Polymer Sci. 7, 803–815.CrossRefGoogle Scholar
Swanson, H. E., Morris, M. C. & Evans, E. H. (1966). Natl. Bur. Stand. (U.S.) Monogr. 25(4), 1. Available as microfiche or photocopy from the National Technical Information Service, 5285 Port Royal Rd., Springfield, VA 22161.Google Scholar
Torii, K., Hotta, M. & Asaka, M. (1979). J. Jpn. Assoc. Mineral. Petrol. Econ. Geol. 74, 251–264.CrossRefGoogle Scholar