X ray

Author:

Md. Waliullah Wali

Dept. of pharmacy

Southeast University

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Outline

X-ray diffraction

Limitations of XRD

Principles of XRD

XRD Techniques

Applications of XRD

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Advantages & Limitations of XRF

Principles of XRF

XRF Techniques

Applications of XRF

X-Ray Fluorescence

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XRD

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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Principles of XRD

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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XRD Techniques

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XRD Techniques

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2

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Applications of XRD

Determine crystal

structures Determine of modal amounts

of minerals

Make textural measurements

-Characterization of

crystalline materials

-Identification of fine-

grained minerals

-Determination of unit cell

dimensions

-Measurement of sample

purity

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Limitations of XRD

Homogeneous and

single phase

material is best

For mixed

materials,

detection limit

is ~ 2% of

sample Peak overlay may

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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XRF

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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Principles of XRF

The XRF method depends on fundamental principles that are common to several other instrumental methods involving interactions between electron beams and X-rays with samples, including, X-ray spectroscopy (e.g. SEM – EDS), X-ray diffraction (XRD) and wavelength dispersive spectroscopy (microprobe WDS).

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XRF Techniques

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Applications of XRF

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

-Research in igneous,

sedimentary, and metamorphic

petrology

-Soil surveys

-mining

-Cement production

-Ceramic and glass

manufacturing

-Environmental studies

-Petroleum industry

-Field analysis

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Advantages of XRF

Minimal

preparation Non-

destructive

Fast

Easy to

use

Cost-

effective

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Limitation of XRF

0 Relatively large

samples, typically >

1 gram

Materials that can be

prepared in powder form

and effectively

homogenized

Materials for which

compositionally similar,

well-characterized

standards are available Materials containing high

abundances of elements for which

absorption and fluorescence effects

are reasonably well understood

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References

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, 466-

470.

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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Thank All of you!

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