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Tut 5 With Solutions

TGA and DSC provide information about thermal transitions in materials. The first transition of calcium oxalate monohydrate shows a 15% weight loss, corresponding to the loss of one water molecule. The second transition would show approximately a 44% weight loss, associated with the decomposition of calcium carbonate into calcium oxide and carbon dioxide. X-ray diffraction determines crystal structure by detecting interference patterns from coherent scattering of x-rays off the periodic atomic arrangement in crystals.

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Londeka Buthelezi
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91 views3 pages

Tut 5 With Solutions

TGA and DSC provide information about thermal transitions in materials. The first transition of calcium oxalate monohydrate shows a 15% weight loss, corresponding to the loss of one water molecule. The second transition would show approximately a 44% weight loss, associated with the decomposition of calcium carbonate into calcium oxide and carbon dioxide. X-ray diffraction determines crystal structure by detecting interference patterns from coherent scattering of x-rays off the periodic atomic arrangement in crystals.

Uploaded by

Londeka Buthelezi
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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Tut 5 – Solid state analysis

1. What information about a sample is derived from TGA and DSC?

TGA – mass loss as a function of temperature or time

DSC – Endothermic and exothermic transitions during isothermal or adiabatic temperature change

2. Show by equations what happens to calcium oxalate monohydrate during a typical TGA
experiment.

3.

3.1 If the first transition has a weight loss of approximately 15wt%, what reaction is occurring?

First calculate the mass of CaCO3.H2O = 40.078+12.011+3(15.999)+2(1.008)+15.999 = 118.101g/mol

Next = calculate what the 15% weight loss amounts to = 15/100 *118.101 = 17.8 ≈18g/mol

which suggests loss of water

CaCO3.H2O → CaCO3 + H2O

3.2 What will the approximate weight loss of the second transition amount to?

CaCO3 → CaO + CO2


Mass of CaCO3 = 100 g/mol

Mass of CO2 which will be lost = 44.009g/mol

44.009/100 *100% = 44%

3.3 What will be chemical transformation associated with the second transition?

CaCO3 → CaO + CO2

4. Explain briefly the principle of X-ray diffraction.

Diffraction occurs when each object in a periodic array scatters radiation coherently, producing

concerted constructive interference at specific angles. In this case X-ray radiation . The electrons

in an atom coherently scatter light and interact with the oscillating electric field of the light wave

(√). Atoms in a crystal are arranged in a periodic array and can thus diffract the x-rays to give

constructive interference. The wavelength of X rays are similar to the distance between atoms.

Diffraction from different planes of atoms produces a diffraction pattern, which contains

information about the atomic arrangement within the crystal. X Rays are also reflected, scattered

incoherently, absorbed, refracted, and transmitted when they interact with matter.

5. Show with the aid of a diagram how the Bragg equation can be derived.

Diagram in the notes

nλ = BC +CD

but BC = d sin θ

since BC = CD

Sub into (1)

we have nλ = 2BC

Using (2), we get

nλ = 2d sin θ
6. The figure shows the first two peaks of the X-ray diffraction pattern for copper, which has an FCC
crystal structure; monochromatic X-ray radiation having a wavelength of 0.1542 nm was used.
Determine the interplanar spacing for the 111 peak which occurs at 43.8 ° 2.

nλ = 2dsin(θ)
d = n x λ / 2sin(θ)
= (1)(0.1542nm)/2 sin (43.8°/2)
= 0.2067 nm or 0.21 nm

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