X-Ray Emission Spectroscopy Tutorial Sheet

1. Compare and contrast between FAAS and ICP technique.

FAAS is an analytical technique used to measure a wide range of elements
concentration in samples, where the free atoms of the sprayed element solution
absorbed the radiation of the Hollow Cathode Lamp of the analyzed element.
Whereas ICP is a multi-element analysis technique that will dissociate a sample into
its constituent atoms and ions and exciting them to a higher energy level using plasma
where there is a temperature up to 10000K.

2. What is the short-wavelength limit of the continuous spectrum produced by an x-

ray having a silver target and operated at 80 kV?

λo=12,398/V
= 12397/ 80 x103
= 0.155Ao

3. The mass absorption coefficient for Ni, measured with the Cu Kαline, is 42.2 cm2/g.
Calculate the thickness of the nickel foil that was found to transmit 36.1% of the
incident power of a beam of Cu Kα radiation. Assume the density of Ni is 8.9 g/cm 3
For this problem,
Po
In 𝑃 = µmρx
100
In = (42.2) (8.9) x
36.1

X = 2.71 x 10-3
4. Calculate the necessary angles to enable you to make a scale diagram showing
constructive interference that produce the first and second order diffraction of x-
rays incident beams of wavelength 154.2 nm from a crystal plane with a spacing of
250 nm.
n λ = 2d sin Ɵ
1(154.2) = 2(250) sin Ɵ
Sin Ɵ = 0.3084
Ɵ = 17.960
Thus 2nd Ɵ = 38.080

5. Derive the Braggs equation (nƟ = 2d sinƟ) from the given diagram

The two X-ray beams of wavelength λ, arrive in phase onto the respective imaginary
planes, with an angle of incidence θ, and form a wave front (first green line on the
left).

In order to obtain a cooperative effect, after reflection both X-ray beams should still
be in phase (last green line on the right), a situation that will only happen if the path
difference traveled by the wave fronts OF and OH (wave fronts before and after
reflection) is an integer number of wavelengths.

This condition is equivalent to say that the sum of the FG and GH segments
corresponds to an integer (n) times the wavelength (λ):

FG + GH = n. λ (1)

but FG = GH and sin θ = FG / d that is: FG = d sin θ

and therefore expression (1) becomes: 2 d sin θ = n. λ
6. A sample consisting of two metallic elements is irradiated in an x-ray
spectrometer. The spectrometer is equipped with a PET crystal for which the d-
spacing is 4.375 nm. Strong emission lines were observed at 2 values of 25.57,
25.62, 30.34 and 30.39 degrees.

i. Calculate the wavelength corresponding to each observed emission line

(The spectrum may be assumed to be in the first order)
Use 2d sin θ = n. λ to calculate the wavelength of each emission line below

ii. using the information given below, determine which elements are present
in the sample

Element Emission Lines (nm)

Kα1 Kα2
V 2.50348 2.50730
Cr 2.28962 2.29351
Mn 2.10175 2.10568
Fe 1.93597 1.93991

Ɵ λ Corresponding
Emission lines
12.785 1.936 Fe Kα1
12.81 1.94 Fe Kα2
15.17 2.2897 Cr Kα1
15.195 2.2934 Cr Kα2

Elements present are Fe and Cr

7. For Mo Kα radiation (0.711 Å), the mass absorption coefficients for K,I, H, and O
are 16.7, 39.2, 0.0, 1.50 cm2/g, respectively:

a) Calculate the mass absorption coefficient for a solution prepared by mixing 8.0 g of
KI with 92 g of water.
Mass absorption coefficient are additive function of the weight fractions of elements
contained in a sample. Thus
µM = WAµA + WBµB + WCµC ……
µM =[((39.0983/166.0038)x 8)/100)x 6.7] + [96.1158/100) x 39.2] + [(81.77/100) x1.5]
µM = 3.94 cm2

b) The density of the solution described in (a) is 1.05 g/cm3. What fraction of
radiation from a Mo Kα source would be transmitted by a 0.50 cm layer of the
solution?
Po
In 𝑃 = µmρx
1
In = (3.93) x 1.05 x 0.050
𝑃

= 0.126
Thus 0.126 x 100 = 12.6%

8. Use the following data to determine which of the following radiation would
produce x-ray fluorescence in Fe
Cr Kα : λ = 2.2897Å
Cu Kα : λ = 1.5418Å
K absorption edge of Fe = 1.743Å
Cu Kα with λ = 1.5418Å has sufficiently high energy to bring about the ejection of
electrons in K shell of Fe. Subsequent rearrangement of electrons within the atom
will produce x-ray fluorescence

9. If the Cr Kβ1 (λ = 2.085 Å) x-ray radiation from the output of a Cr – x-ray tube was
to be removed, which of the two metals below would you select for the job? Give
explanation to the answer of your choice.
i. K (potassium), K absorption edge: λ = 3.742 Å
ii. Rb, K absorption edge: λ = 0.926 Å
K (potassium), K absorption edge: λ = 3.742 Å since beyond this wavelength
the energy is insufficient to remove any further K electrons.