25 X-RAY POWDER DIFFRACTOMETRY Division of Forensic Science TRACE EVIDENCE TRAINING MANUAL

25.1 Introduction to X-radiation, Diffraction, and the X-ray Diffractometer 25.1 Objectives

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25 X-RAY POWDER DIFFRACTOMETRY (XRD)

25.2

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The characteristics and properties of x-rays; The general understanding of crystalline states; Principles of diffraction; The theory and basic design of the instrument; The capabilities and limitations of the instrument; Sample preparation techniques; The interpretation of results; QA/QC procedures; and, Safety issues. Required Readings 25.2.1 25.2.2 25.2.3 25.2.4 25.2.5 25.2.6 25.2.7

Through completion of this module the trainee will have developed and demonstrated theoretical knowledge and/or practical skills to:

Gobel, H. E., "Identification of Crystalline Phases and Phase Kinetics of Solid Body Reactions Through Powder X-Ray Diffraction," Siemens Analytical Systems, Vol. 4, 1985, pp. 167-176. Jenkins, R., ed., "Sample Preparation Methods in X-Ray Powder Diffraction," Powder Diffraction, Vol. 1, 1986, pp. 51-63. Jenkins, R., and deVries, J. L., An Introduction to X-Ray Diffractometry, N. V. Philips, Gloeilampenfabrieken, Eindhoven, Germany.

McCarthy, Gregory J., Hubbard, Camden R., and Foris, Catherine M., PDF Workbook - Use of the XRay Powder Diffraction File, JCPDS, International Centre For Difffraction Data. Skoog, Douglas A., and West, Donald M., Principles of Instrumental Analysis, 2nd edition, Saunders College, Philadelphia, PA, 1980, pp. 427-457. Thacher, P. J. and Briner, G. P., "The Application of X-Ray Powder Diffraction to Forensic Science," Powder Diffraction, Vol. 1, 1986, pp. 320-324.

25.3

Questions

The trainee will provide written answers to the following questions:

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Willard, H. H., Merritt, L. L., and Dean, J. A., Instrumental Methods of Analysis, 5th edition, D. Van Norstrand Company, New York, NY, 1974, pp. 258-301.

What are x-rays and how are they formed? What determines the wavelength and intensity of an x-ray? What is a crystalline compound? Define Braggs Law and how it relates to x-ray diffraction. What is the wavelength of Copper K radiation? How does the wavelength of Cu K radiation relate to (typical) intermolecular distances in crystals. Name the basic components of the XRD and their function. What detector do we use? Explain how it works.

25 X-RAY POWDER DIFFRACTOMETRY Division of Forensic Science TRACE EVIDENCE TRAINING MANUAL

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25.4

25.5

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Practical Exercises 25.4.1 The trainer will demonstrate the operation of the instrument to the trainee. 25.4.2 25.4.3 25.4.4 The trainee will be given 10 unknown samples to analyze by XRD. Evaluation 25.5.1 The trainer will review the written answers to the questions with the trainee. 25.5.2 25.5.3 25.5.4 Review of practical exercises. The trainee will be quizzed orally upon the subject matter.

How can K radiation be removed from the pattern? In a simple mixture, what approximate minimum percentage of a compound must be present for detection? How are samples prepared for analysis by XRD? What are the advantages/disadvantages of the XRD?

The trainee will prepare, examine, and perform database searches on 10 different known powders provided by the trainer. The results will be compared with library standards. The trainee will prepare, examine, and perform database searches on 10 different known powder mixtures provided by the trainer. The exercise will include using a variety of sample holders, including the zero background plate.

The trainer and the trainee will review and discuss the pertinent points of each of the required readings.

25.2

Competency Evaluation and Mock Trial The trainee will use x-ray powder diffraction when completing their subdiscipline competency test and will defend their results as a part of their mock trial in that subdiscipline.

25.3

Reading List 25.3.1 25.3.2 25.3.3 25.3.4 25.3.5 25.3.6 25.3.7 Gobel, H. E., "Identification of Crystalline Phases and Phase Kinetics of Solid Body Reactions Through Powder X-Ray Diffraction," Siemens Analytical Systems, Vol. 4, 1985. Jenkins, R., ed., "Sample Preparation Methods in X-Ray Powder Diffraction," Powder Diffraction, Vol. 1, 1986, pp. 51-63. Jenkins, R., and deVries, J. L., An Introduction to X-Ray Diffractometry, N. V. Philips Gloeilampenfabrieken, Eindhoven, Germany. Jenkins, R. and deVries, J. L., Worked Examples in X-Ray Analysis, The Macmillan Press Limited, New York, NY, 1974. McCarthy, Gregory J., Hubbard, Camden R., and Foris, Catherine M., PDF Workbook - Use of the X-Ray Powder Diffraction File, JCPDS, International Centre For Difffraction Data. Skoog, Douglas A., and West, Donald M., Principles of Instrumental Analysis, 2nd edition, Saunders College, Philadelphia, PA, 1980. Thacher, P. J. and Briner, G. P., "The Application of X-Ray Powder Diffraction to Forensic Science," Powder Diffraction, Vol. 1, 1986, pp. 320-324.

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25 X-RAY POWDER DIFFRACTOMETRY Division of Forensic Science TRACE EVIDENCE TRAINING MANUAL
25.3.8

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Willard, H. H., Merritt, L. L., and Dean, J. A., Instrumental Methods of Analysis, 5th edition, D. Van Norstrand Company, New York, NY, 1974. End

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