This document provides an overview of X-ray diffraction (XRD) and X-ray fluorescence (XRF) techniques. It discusses the principles, methods, applications, advantages, and limitations of both XRD and XRF. XRD is described as a technique that uses X-ray scattering from crystalline materials to determine their atomic structure, while XRF involves bombarding a material with X-rays and analyzing the characteristic secondary X-rays emitted to determine its elemental composition. A variety of applications are outlined for each technique in fields such as materials science, geology, and chemistry.
4. XRD
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X-ray diffraction (XRD) is an analytical technique
looking at X-ray scattering from crystalline
materials. Each material produces a unique X-ray
"fingerprint" of X-ray intensity versus scattering
angle that is characteristic of it's crystalline atomic
structure.
X-ray diffraction procedures
apply only to crystalline
Materials.
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5. Principles of XRD
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X-ray diffraction is based on constructive
interference of monochromatic X-rays and a
crystalline sample.
The interaction of the incident rays with the sample
produces constructive interference (and a diffracted
ray) when conditions satisfy Bragg's Law (nλ=2d sin
θ).
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12. Applications of XRD
Determine crystal
structures
-Characterization of
crystalline materials
-Identification of finegrained minerals
-Determination of unit cell
dimensions
-Measurement of sample
purity
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Determine of modal amounts
of minerals
Make textural measurements
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13. Limitations of XRD
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Homogeneous and
single phase
material is best
For mixed
materials,
detection limit
is ~ 2% of
Peak overlay may
sample
occur and worsens
for high angle
'reflections'
Requires tenths of a
gram of material
which must be
ground into a powder
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14. XRF
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X-Ray Fluorescence is defined as “The emission of
characteristic "secondary" (or fluorescent) X-rays
from a material that has been excited by
bombarding with high-energy X-rays. The
phenomenon is widely used for elemental analysis.”
X-ray fluorescence procedures
applied to the material
in any physical state,
solid, liquid and gas.
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19. Applications of XRF
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-Research in igneous,
sedimentary, and metamorphic
petrology
-Soil surveys
-mining
-Cement production
-Ceramic and glass
manufacturing
-Environmental studies
-Petroleum industry
-Field analysis
Bulk chemical analyses of major elements
(Si, Ti, Al, Fe, Mn, Mg, Ca, Na, K, P) in
rock and sediment
Bulk chemical analyses of trace elements
(in abundances >1 ppm; Ba, Ce, Co, Cr,
Cu, Ga, La, Nb, Ni, Rb, Sc, Sr, Rh, U, V,
Y, Zr, Zn) in rock and sediment
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21. Limitation of XRF
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0
Relatively large
samples, typically >
1 gram
Materials that can be
prepared in powder form
and effectively
homogenized
Materials containing high
abundances of elements for which
absorption and fluorescence effects
are reasonably well understood
Materials for which
compositionally similar,
well-characterized
standards are available
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22. References
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1. Elements of physical chemistry by S Glasstone
2. Atkins physical chemistry
3. Pharmaceutical chemistry by LG Chattem
4. Brady, John B., and Boardman, Shelby J., 1995, Introducing
Mineralogy Students to X-ray Diffraction Through Optical
Diffraction Experiments Using Lasers. Jour. Geol. Education, v.
43 #5, 471-476.
5. Brady, John B., Newton, Robert M., and Boardman, Shelby J.,
1995, New Uses for Powder X-ray Diffraction Experiments in the
Undergraduate Curriculum. Jour. Geol. Education, v. 43 #5, 466470.
6. Buhrke, V. E., Jenkins, R., Smith, D. K., A Practical Guide for
the Preparation of Specimens for XRF and XRD Analysis, Wiley,
1998.
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