Surname and Initials: Majajabothata J

Student number: 201828135

Date: 16 September 2021
SPHA032 ACTIVITY 3: X-Ray Diffraction analysis
INTRODUCTION
What is x-ray diffraction?

X-ray diffraction (XRD) is a non-destructive technique for analyzing the structure of

materials, primarily at the atomic or molecular level. It works best for materials that are
crystalline or partially crystalline (i.e., that have periodic structural order) but is also used
to study non-crystalline materials.

XRD relies on the fact that X-rays are a form of light, with wavelengths on the order
of nanometers. When X-rays scatter from a substance with structure at that length
scale, interference can take place, resulting in a pattern of higher and lower intensities.
This is qualitatively similar to the colorful patterns produced by soap bubbles, in which
different colors are viewed in different directions.

XRD is quite different from X-ray radiography, or tomography. Tomography relies on the

fact that the X-rays are absorbed more strongly by some materials than others--for
example, bone or tumors absorb more than muscle or fat. Therefore, the transmitted
image provides a direct image of the structure inside the body or object (typically a length
scales of a millimeter or above), making it an invaluable tool for doctors. (X-ray
tomography is also widely used in other fields such as materials science and metallurgy.)
In contrast, the XRD produces a diffraction pattern, which does not superficially resemble
the underlying structure, and provides information about the internal structure on length
scales from 0.1 to 100 nm.

In its most simplified form, a generic X-ray scattering measurement is shown below.

A beam of X-rays is directed towards a sample, and the scattered intensity is measured as
a function of outgoing direction. By convention, the angle between the incoming and
outgoing beam directions is called 2θ. For the simplest possible sample, consisting of
sheets of charge separated by a distance d, constructive interference (greater scattered
intensity) is observed when Bragg's Law is satisfied:

n λ = 2 d sin θ
Here n is an integer (1, 2, 3, ...), λ is the wavelength of the x-ray beam, and θ is half the
scattering angle 2 θ shown above.

Real materials are more complicated, of course, but the general result holds that there is a
relationship between interparticle distances within the sample and the angles at which the
scattered intensity is the highest, with larger distances d corresponding
to smaller scattering angles 2θ.
THEORY

Bragg law, in material science, the connection between the dispersing of nuclear planes in
precious stones and the points of frequency at which these planes create the foremost
seriously reflections of electromagnetic radiations, such as X beams and gamma beams,
and molecule waves, such as those related with electrons and neutrons.

N𝜆=2dsin𝜃

The d-spacing of each peak is then obtained by solution of the Bragg equation for the
appropriate value of λ. Once all d-spacings have been determined, automated
search/match routines compare the ds of the unknown to those of known materials.
Because each mineral has a unique set of d-spacings, matching these d-spacings
provides an identification of the unknown sample. A systematic procedure is used by
ordering the d- spacings in terms of their intensity beginning with the most intense peak.
Files of d-spacings for hundreds of thousands of inorganic compounds are available from
the International Centre for Diffraction Data as the Powder Diffraction File (PDF). Many
other sites contain d- spacings of minerals such as the American Mineralogist Crystal
Structure Database.

Commonly this information is an integral portion of the software that comes with the
instrumentation.

A Grid point is the position within the unit cell or in a precious stone where the likelihood of
finding an iota or an particle is the most elevated. In other words, the particles or particles
involve the cross section focuses in a crystalline strong. The grid positions possessed by
the constituent particles are shown as focuses within the open structure of the unit cell.

d = √h2+k2+l2
The percentage difference is: The difference between two values divided by the average
of the two values. Shown as a percentage. Difference means to subtract one value from
another: Average is the value halfway between

% difference

% different = x1–x2 x 100

(x1+x2)/
2
APPARATUS

a) DIFRACTION DATA

b) Mineral data

c) CALCULATOR

d) COMPUTER RUNNING EXCEL

METHOD

1. An XRD raw data was given to be examined and the sample name was
recorded.
2. The wavelength of 1.540589 A0 was used and the intensity vs 2𝜃 graph was
plotted using the excel.
3. The 7 strongest peaks were chosen on the graph.
4. The d-spacing and relative intensities were calculated and the lattice points.
RESULTS AND DISCUSSION
1. Sample identification #a06u
2. K-Alpha1 wavelength 1.540598A
K-Alpha2 wavelength 1.544426A
3.

Intensity Vs Angle 2θ
16000
14000
12000
10000
INTENSITY

8000
6000
4000
2000
0
0 10 20 30 40 50 60 70 80 90 100
ANGLE 2θ

4. Peaks table:
Rank 2θ Intensity d-spacings( Å ¿ I rel
1. 25.375 14969 3.51 100.00
2. 48.167 3523 1.89 23.54
3. 37.875 2888 2.38 19.29
4. 54.025 2094 1.70 13.99
5. 55.207 2010 1.67 13.43
6. 62.796 1649 1.48 11.02
7. 75.139 1037 1.27 6.93

d-spacings:nλ = 2dsinθ
n=1 since we are dealing with first order
λ = 2dsinθ
λ
d 1=
2 sinθ
1.54 4 Å
¿
25.375
2sin ( 2 )
¿ 3.5 1 Å
 λ λ λ
d 2= d 3= d4=
2 sinθ 2 sinθ 2 sinθ
1.544 Å 1.544 Å 1.544 Å
¿ ¿ ¿
48.169 37. 876 5 4.025
2sin
2 ( ) 2sin( 2 ) 2sin( 2 )
¿ 1.89 Å ¿ 2.38 Å ¿ 1.70 Å

λ λ λ
d 5= d6= d 7=
2 sinθ 2 sinθ 2 sinθ
1.544 Å 1.544 Å 1.544 Å
¿ ¿ ¿
55.207 62. 796 75.1 34
2sin
2( ) 2sin( 2 ) 2sin( 2 )
¿ 1.67 Å ¿ 1. 48 Å ¿ 1.27 Å

I
Relative intensity: I rel = ×100
I max
I 14969
I rel = = ×100=100.00
I max 14969

I 3523 I 2888 I 2094

I rel = = ×100=23.54I rel = = ×100=19.29I rel = = ×100=13.99
I max 14969 I max 14969 I max 14969

I 2010 I 1649 I 1037

I rel = = ×100=13.43I rel = = ×100=11.02I rel = = ×100=6.93
I max 14969 I max 14969 I max 14969
5. Reference Data Mineral Name Actinolite
2-THETA INTENSITY D-SPACING HKL Match?
(Yes/No)
33.06 100.00 2.7097 151 no
10.51 80.68 8.4201 110 no
28.57 64.66 3.1210 310 no
35.42 57.70 2.5341 -2 0 2 no
26.32 50.83 3.3856 131 no

Reference Data Mineral Name Anatase

2-THETA INTENSITY D-SPACING HKL Match?
(Yes/No)
25.33 100.00 3.5165 101 yes
48.08 28.85 1.8922 200 no
37.82 20.47 2.3786 004 no
53.93 18.58 1.7001 105 no
55.12 18.21 1.6663 211 no

Reference Data Mineral Name Brookite

2-THETA INTENSITY D-SPACING HKL Match?
(Yes/No)
25.38 100.00 3.5092 210 yes
30.86 99.94 2.8978 211 no
25.73 78.87 3.4619 111 no
55.33 34.76 1.6604 421 no
48.11 34.28 1.8914 321 no

Reference Data Mineral Name Chlorargyrite

2-THETA INTENSITY D-SPACING HKL Match?
(Yes/No)
32.74 100.00 2.7350 200 no
46.98 63.96 1.9339 220 no
28.26 52.01 3.1581 111 no
78.14 21.70 1.2231 420 no
55.74 20.92 1.6493 311 no

Reference Data Mineral Name Quartz

2-THETA INTENSITY D-SPACING HKL Match?
(Yes/No)
26.65 69.90 3.3446 011 no
26.65 30.10 3.3446 101 no
20.87 19.93 4.2574 100 no
50.17 12.58 1.8184 112 no
35.56 7.13 2.4580 110 no
Reference Data Mineral Name Rutile
2-THETA INTENSITY D-SPACING HKL Match?
(Yes/No)
27.50 100.00 3.2435 110 no
54.46 57.99 1.6849 211 no
36.17 46.72 2.4836 101 no
69.18 20.83 1.3579 301 no
41.34 18.28 2.1840 111 no

 Brookite is the one which has the intensity,2-theta and d-spacings that are
very close to that of the peaks table.

Calculating the percentage difference of 2-theta, intensity and d-spacing

between Brookite and results from peaks table:

|V a −V b|
%diff = ×10 0
V +V
( a b)
2

a) 2-Theta

|25.375−25.38| |48.169−30.86| |37.876−25.73|

%diff = ×10%diff
0 = × 10%diff
0 = ×10 0
25.375+25.38 48.169+30.86 37.876+ 25.73
( ) ( ) ( )
2 2 2
=0.01% =43.80% =38.19%

|54.025−55.33| |55.207−48.11|
%diff = ×10%diff
0 = ×10 0
54.025+55.33 55.207+ 48.11
( ) ( )
2 2
=2.39% =18.74%

b) D-spacing
 |3.510−3.5092| |1.89 0−2.8978| |2.38 0−3.4619|
%diff = ×10%diff
0 = ×10%diff
0 = ×10 0
3.510+3.5092 1.890+2.8978 2.380+ 3.4619
( ) ( ) ( )
2 2 2

=0.02% =42.1% =37.04%

|1.70 0−1.6604| |1.67 0−1.8914|

%diff = × 100
%diff = × 100
1.700+1.6604 1.670+1.8914
( ) ( )
2 2

=2.36% =12.43%

c) Intensity

|100−100| |23.54−99.94| |19.29−78.87|

%diff = ×10 0 %dif f = ×10%diff
0 = ×10 0
100+100 23.54+ 99.94 19.29+78.87
( ) ( ) ( )
2 2 2
=0.0% =123.74% =121.39%

|13.99−34.76| |13.43−34.28|
%diff = ×10 0%diff = ×10 0
13.99+34.76 13.43+34.28
( ) ( )
2 2
=85.21% =87.4%
DISCUSSION

From the given XRD RAW data the graph was drawn I was able to find the 7 strongest
peaks which were 14969,3523,2888,2094,2010,1649 and and the 2𝜃 values of the
strongest peaks were 25.375,48.167,37.875,54.025,55.207,62.796 and 75.139, which
lead me to calculate the d-spacing of the unknown raw data, according to the calculated
data above it has been shown that by the raw data and anatase sample were having the
matching values.the d- spacing were calculated using the braggs equation and were found
to be 3.5215,1.8931,2.3852,1.7079,1.6668,1.4870 and 1.2643. the percentage difference
between the anatase and the raw data it has slightly difference percentage of d-spacing
and angles the relative intensity shows a huge difference on than the other 2 , which
proved that the raw data it is the anatase sample. From the discovered sample I was able
to calculated the lattice parameters which were 4.9802A 0, 3.7862A0,9.5408A0,8.7086A0
and 4.0828A0
CONCLUSION
I was able to analyses the XRD raw data by using the drawn graph data of intensities vs
the 2theta angles, by choosing the 7 strongest peaks that lead me calculate d-spacing and
the relative intensities. those values where matching with the XRD sample of anatase with
the smallest difference between the angles, d-spacing and the relative intensities. And the
lattice parameters were calculated using the bragg law equation.

ACKNOWLEDGES
I would love to give thanks to my lab assistance for showing me on how to continue with
the experiment.

REFERENCES
 Dutrow, Barb, 1997, Better Living Through Minerals X-ray Diffraction of Household
Products, in: Brady, J., Mogk, D., and Perkins D. (eds.) Teaching Mineralogy,
Mineralogical Society of America, p. 349-359.
 Hovis, Guy, L., 1997, Determination of Chemical Composition, State of Order,
Molar Volume, and Density of a Monoclinic Alkali Feldspar Using X-ray Diffraction,
in: Brady, J., Mogk, D., and Perkins D. (eds.) Teaching Mineralogy, Mineralogical
Society of America, p. 107-118.
 Brady, John B., 1997, Making Solid Solutions with Alkali Halides (and Breaking
Them) , in: Brady, J., Mogk, D., and Perkins D. (eds.) Teaching Mineralogy,
Mineralogical Society of America, p. 91-95.
 Perkins, Dexter, III, and Sorensen, Paul, Mineral Synthesis and X-ray Diffraction
Experiments, in: Brady, J., Mogk, D., and Perkins D. (eds.) Teaching Mineralogy,
Mineralogical Society of America, p. 81-90.
 Hollecher, Kurt, A Long-Term Mineralogy Practical Exam, in: Brady, J., Mogk, D.,
and Perkins D. (eds.) Teaching Mineralogy, Mineralogical Society of America, p.
43-46.