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FTIR과 XRD를 이용한 α-Quartz 분석법 비교

Comparison of Analytical Methods for α-Quartz by FTIR and XRD

  • 발행 : 2009.04.30

초록

This study compared FTIR with XRD method for the analysis of quartz by % recovery, coefficient of variation (CV) and influence of the interference. the results were as the following. 1. In FTIR method, the coefficient of determination ($r^2$) was 0.9998 in a calibration curve of $695\;cm^{-1}$, and the limit of detection was $4.9{\mu}g/sample$. 2. The highest recovery was $799\;cm^{-1}$ (98.2%). 3. The CVpooled of the FTIR method was approximately 10% in three wave numbers. 4. The analysis of qualitative and quantitative for quartz is difficult with mixed cristobalite and iron oxide. 5. In XRD method with rotating sample holder and LynxEye detector, the coefficient of determination was 0.9996 in a calibration curve, and the limit of detection was $5.9{\mu}g/sample$. 6. The recovery and CV pooled were 104.3%, and 11 %, respectively. 7. In muffle furnace ashing, the quartz weight decreased to 34% when the maximum weight of the iron oxide was more than eight times. In conclusion, the accuracy (% recovery) and precision (CV) of FTIR and XRD method for analyzing $\alpha$-quartz were similar. FTIR method was a disadvantage for sample matrix because it indicates possibility of interference. However, XRD method distinguished specific crystalline forms of silica, and the majority of silicate minerals. In addition, XRD method recommend filter dissolution to pretreatment method.

키워드

참고문헌

  1. Choi, B. S. : The current status and measures of pneumoconiosis in Korea. Journal of Korean Medical Association, 40(5), 609-615, 1997 (Translated by Kim, B. W., Korean)
  2. Kim, H. W. : Silica. Report. Ministry of Labor. 37, 2005 (Translated by Kim, B. W., Korean)
  3. Korea Occupational Safety & Health Agency : Crystalline Silica. No. 2007-10-222, 2007 (Translated by Kim, B. W., Korean)
  4. Cannichael. R. S. : Practical Handbook of Physical Properties of Rocks and Minerals, Boca Roton, FL, CRC Press, 1989
  5. Klein, C. : Rocks, minerals, and a dusty world. In: Guthrie, G. D. and Mossman, B. T., eds, Reviews in Mineralogy, Vol. 28, Health Effects of Mineral Dusts, Mineralogical Society of America, Chelsea, MI, Brook Crafters, 8-59, 1993
  6. Klein, C. and Hurlbut, C. S.,Jr : Manual of Mineralogy, 21 st Ed., New York, John Wiley & Sons, 527, 1993
  7. International Agency for Reserarch on Cancer World Hcalth Organization : IARC Monographs on the Evaluation of Carcinogenic Risks to Humans: Silica, Some Silicates, Coal Dust and Para-Aramid Fibrils. Vol. 68. Lyon, France: World Health Organization. IARC, 46, 1997
  8. Ministry of Labor: Threshold limit Values for Chemical Substances and Physical Agents exposure indices. No. 2007-25, 2007 (Tnmslated by Kim, B. W., Korean)
  9. American Conference of Governmental Industrial Hygienists. Threshold Limit Values for Chemical Substances and Physical Agents and Biological Exposure Indices, ACGIH, 2006
  10. Madson, F. A., Rose, M. C. and Cee, R. : Review of quartz analytical methodologies - Present and Future Needs. Applied Occupational and Environmental Hygiene, 10(12), 991-1001. 1995 https://doi.org/10.1080/1047322X.1995.10389086
  11. National Institute for Occupational Safety and Health : NIOSH Manual of Analytical Method, 4ed., Method 7500, DHHSINIOSH Pub. 94-113. 1994 - Revised by Rosa Key-Schwartz et al. NIOSHIDART, 2003
  12. National Institute for Occupational Safety and Health on Centers for Disease Control and Prevention : NIOSH Hazard Review, Health Effects of Occupational Exposure to Respirable Crystalline Silica, pp5, 2002
  13. Occupatioanl Safety and Health Administration Analitical Laboratory : OSHA Manual of Analytical Method, OSHA Method No. 10-142, Salt Lake City, Utah. 1981 Revised, 1996
  14. Choi, H. C., Cheon, Y. H., Kim, H. J. and Lee, J. J. : Quantitative analysis of Quartz, Mica, and Feldspar in respirable coalmine dust in Taebaek area by Fransform Infrared Spectrophotometry. Korean Journal of Preventive Medicine, 21(2), 271-283, 1988
  15. Oh, S. M., Shin, Y. C., Park. D. W., Lee, N. R., Park, S. H., Yi, K. Y. and Moon, Y. H. : A study of Worker's Exposure to Dust, Crystalline Free Silica and Lead in Ceramic Industry. Journal of Korean Society of Occupational and Environmental Hygiene, 4(2), 168-179, 1994
  16. Phee, Y. G., Poh, Y. M., Lee, K. M., Kim, H. A., Kim, Y. W., Won, J. I. and Kim, H. W. : Analysis of Quartz Content and Particle Size Distribution of Airborne Dust from Selected Foundry Operations. Journal of Korean Society of Occupational and Environmental Hygiene, 7(2), 196-208, 1997
  17. Kim, H. J., Phee, Y. G., Roh, Y. M. and Kim, H. W. : Study on the field-pplication of FTIR-direct on filter method for the analysis of quartz in respirable dust samples. Journal of Korean Society of Occupational and Environmental Hygiene, 12(2), 73-78, 2002
  18. Shin, Y. C., Choi, B. S., Lee, B. K., Yi, G. Y., Lee, J. T., Lee, 1. S., Lee, K. O., Kim, K. W., Go, K. S., Kim, T. K. and lung, H. K. : Exposure Assessment of Air Contaminants by Type of Mine in Korea -Focused on Carcinogenic Substances. Journal of Korean Society of Occupational and Environmental Hygiene, 12(2), 95-105, 2002
  19. Shin, Y. C., Choi, B. S., Lee, B. K., Lee, G. Y., Lee, J. T., Lee, J. S., Lee, J. O., Kim, T. K., Go, K. S., Kim, K. W. and Jung, H. K. : Evaluation of Workers Exposure to Total Dust, Respirable Dust, and Crystalline Free Silica by Job in Korea Coal Mines. Journal of Korean Society of Occupational and Environmental Hygiene, 12(3), 146-154, 2002
  20. Ko, W. K., Phee, Y. G., Poh, Y. M. and Kim, H. W.: Performances of the Direct-on-filter and Transfer methods for the analysis of Crystalline silica with FTIR. Journal of Korean Society of Occupational and Environmental Hygiene, 12(3), 155-161,2002
  21. Park, Y. S., Roh, Y. M., K, H. W., Han, J. G., An, Y. S., Kang, S. G. and Kim, J. M. : A Study of Respirable Dust Concentrations and Quartz Contents in Foundry. Journal of Korean Society of Occupational and Environmental Hygiene, 13(1), 90-97, 2003
  22. Cheong, H. K., Kim, J. Y., Cheong, H. K. and Lim, H. S. : A study on evalucatioll of worker exposure to diatomaceous earth dust and engineering control in a diatomite factory. Journal of Korean Society of Occupational and Environmental Hygiene, 4(1), 81-95, 1994
  23. Kim, H. W., Phee, Y. G., Poh, Y. M., Won, J. I. and Kim, Y. W. : Analysis of Quartz Contents by XRD and FTIR in Respirable Dust from Various Manufacturing Industries, Part I-Foundry. Journal of Korean Society of Occupational and Environmental Hygiene, 8(1), 50-66, 1998
  24. Kim, H. W. Phee, Y. G., Poh, Y. M. and Won, J. I : Analysis of quartz contents by XRD and Fl'IR in respirable dust from various manufacturing industries. Journal of Korean Society of Occupational and Environmental Hygiene, 9(1), 99-111, 1999
  25. Kenney, E. R., Fischbach, T. J., Song, R., Eller, P. E. and Shulman, S. A. : Guideline for Air Sampling and AnalyticaJ Method Development and Evaluation, HHS NIOSH) Publication No. 95-117, NationaJ Institute for OccupationaJ Safety and Health, Cincinnati, OH,1995
  26. Kenney, E. R., Fischbach, T. J., Song, R., Eller, P. E. and Shulman, S. A. : Summary of the NIOSH guidelines for air sampling and analyticaJ method development and evaluation. The Analyst, 121, 1163-1169, 1996 https://doi.org/10.1039/an9962101163
  27. Taylor, J. K. : QuaJity Assurance of Chemical Measurement, Chelsea, MI, Lewis Publishers Inc., 20-24, 1987
  28. Kohyaman, N. ; A new X-ray diffraction method for the quantitave anaJysis anaJysis of free silica in the airborne dust in working environment. Industrial Health, 23, 221-234, 1985 https://doi.org/10.2486/indhealth.23.221
  29. Hogan, TJ. Particulates. In. : Fundamentals of Industrials Hygiene, 4ed, by B.A. Plog, Itasca, Illinois, National Safety Council, 1995
  30. Kim, B. W., Choi, B. S., Lee, J. S., Kim, E. S., Jung, J. E., Won, J. Y. and Park, S. Y. : Workers' Exposure to Crysta1line silica and HexavaJent chromium in the cement dust. Proceedings of the 41th Korean Society of OccupationaJ and EnvironmentaJ Medicine. BEXCO, Busan, 91-97, 2008 (Translated by Kim, B. W., Korean)
  31. Shulman, S. A., Groff, J. H. and Abell, M. T. : Performance of Laboratories Measuring Silica in the Proficiency AnalyticaJ Testing Program. American Industrial Hygiene Association Journal, 53(1), 49-56, 1992 https://doi.org/10.1080/15298669291359294
  32. Phee, Y. G. and Kim, H. W. ; The preliminary study on the quantitave analysis of quartz by fourier transform infrared spectrophotometric direct on filter (FfIR-DOF) method. Journal of Korean Society of Occupational and Environmental Hygiene, 15(1), 1-7, 2005
  33. Phee, Y. G., Poh, Y. M. and Kim, H. W. ; The effect of cristobalite on quantitative analysis of quartz in respirable dust by FTJR direct-on-iilter method. Journal of Korean Society of Occupational and Environmental Hygiene, 17(1), 21-30, 2007
  34. Bye, E. : Quantitative determination of silica mixtures by multivatiate calibration applied to infrared spectroscopy. Chemometrics and Intelligent Laboratory Systems, 14, 413-417, 1992 https://doi.org/10.1016/0169-7439(92)80122-K
  35. Dollberg, D. D., Abell, M. T. and Lange, B. A.: Occupational health analytical chemistry : Quantitation using X-ray powder diffraction. ACS Symposium Series, 120, 43, 1980 https://doi.org/10.1021/bk-1980-0120.ch003
  36. Suryanarayana, C. and Norton, M. : X-ray Diffraction. A Practical Approach. Springer. led. 67-71, 1998
  37. Smith, D. K. : Evalution of the Detectability and Quantification of Respirable Crystalline Silica by Xray Powder Diffraction Method. Presented at the Crystalline silica Analytical Method Workshop of the Chemical Manufacturers Association, Arlington (VA): November, 12-13, 1991
  38. Klug, H. P. and Alexander, L. E. : X-Ray Diffraction Procedures, 2ed. John Wiley & Sons, New York, 1974
  39. Chung, F. H. and Smith, D. K. : Industrial Applications of X-Ray Diffraction. CRC Press, 441-465, 1999
  40. Bhaskar, R., Ki, J. and Xu, L. : A comparative study of particle size dependency of IR and XRD methods for quartz analysis. American Industrial Hygiene Association Journal, 55(7), 605-609, 1994 https://doi.org/10.1080/15428119491018682
  41. Verma, D. K., Johnson, D. M. and Tombe, K. D. : A Method for Determining Crystalline Silica in Bulk Samples by Fourier Transform Infrared Spectrophotometry. Annals of Occupupatioal Hygiene, 46(7), 609-615, 2002 https://doi.org/10.1093/annhyg/mef077
  42. Culity, B. D. and Stock, S. R. : Elements of X-ray Diffraction, 3ed. Prentice-Hall, Inc., Copyright, 2001
  43. Peter, S., Barry, T., Delphine, B. and Russell, A. : The performance of laboratories analysing a-quartz in the workplace anaJysis scheme for proficiency (WASP). Annals of Occupational Hygiene, 47(4), 269-277, 2003 https://doi.org/10.1093/annhyg/meg026
  44. Stepan, R., Raisa, S., Derek, H. and Peter, P. : Factor affecting the accuracy of airborne quartz determination. Journal of Occupational and Environmental Hygiene, 4, 80-86, 2007 https://doi.org/10.1080/15459620601115743