THERMOGRAVIMETRIC ANALYSIS

PURUSHOTH ABIRAMI ASHIQ ARUL

What is TGA ?
Process which measures the weight loss(or weight gain) of a sample material as a function of temperature

PRINCIPLE
As materials are heated they loose weight from a simple process such as drying or from chemical reactions that liberate gases .

TGA-Principle of Operation
A sample of the test material is placed into a platinum cup that is supported on, or suspended from an analytical balance located outside the furnace chamber.

The balance is zeroed, and the sample cup is heated according to a predetermined thermal cycle.

TGA-Principle of Operation
The balance sends the weight signal to the computer for storage, along with the sample temperature and the elapsed time.

The TGA curve plots the TGA signal, converted to percent weight change on the Y-axis against the reference material temperature on the X-axis.

METHODOLOGY

TGA-Basic Diagram

Methodology
The analyzer usually consists of a high-precision balance with a pan (generally platinum) loaded with the sample. The pan is placed in a small electrically heated oven with a thermocouple to accurately measure the temperature. The atmosphere may be purged with an inert gas to prevent oxidation or other undesired reactions. A computer is used to control the instrument.

Methodology
Analysis is carried out by raising the temperature gradually and plotting weight against temperature. The temperature in many testing methods routinely reaches 1000C or greater, but the oven is greatly insulated.

After the data is obtained, curve smoothing and other operations may be done such as to find the exact points of inflection.

Methodology
A method known as hi-res TGA is often employed to obtain greater accuracy in areas where the derivative curve peaks. In this method, temperature increase slows as weight loss increases. This is done so that the exact temperature at which a peak occurs can be more accurately identified.

Methodology
Several modern TGA devices can vent burnoff to a fourier-transform infrared spectrophotometer to analyze composition. Fourier transform infrared (FTIR) spectroscopy is a measurement technique for collecting infrared spectra.

Instead of recording the amount of energy absorbed when the frequency of the infra-red light is varied , the IR light is guided through an interferometer.

Methodology
After passing through the sample, the measured signal is the interferogram. Performing a Fourier transform on this signal data results in a spectrum identical to that from conventional (dispersive) infrared spectroscopy.

Processes Requiring TGA

Drying Structural Water Release Structural Decomposition Carbonate Decomposition Gas Evolution Sulphur Oxidation Fluoride Oxidation Re-hydration

Temperature Ranges
Room Temperature to 1,200C Kanthal wire wound heating element Room Temperature to 1,600C Platinum alloy wire wound heating element Silicon Carbide heating element Room Temperature to 1,700C Molybdenum Disilicide heating elements

Areas of Application
TGA is commonly employed in Research and Testing Characteristics of materials such as polymers, Degradation temperatures, Absorbed moisture content of materials, Level of inorganic and organic components in materials, Decomposition points of explosives,and solvent residues. Corrosion kinetics in high temperature oxidation.

Examples of TGA-Report

Precipitated Zr5O8(SO4)2*15 H2O

Analysis of Filtrate from Precipitation

Precipitation 5ZrOCl2 + 2H2SO4 + xH2O Zr5O8(SO4)2*15 H2O (s) + 10 HCl Decomposition
Zr5O8(SO4)2*15 H2O (s) Zr5O8(SO4)2*14 H2O (s) + H2O (v) Zr5O8(SO4)2 5 ZrO2 (s) +2 SO2 (v)
SO2 15 H2O Water Loss 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1 2 Wt. Loss 18.0152 36.0304 54.0456 72.0608 90.076 108.0912 126.1064 144.1216 162.1368 180.152 198.1672 216.1824 234.1976 252.2128 270.228 64.0588 128.1176 % loss 1.721573 3.443146 5.164719 6.886292 8.607865 10.32944 12.05101 13.77258 15.49416 17.21573 18.9373 20.65887 22.38045 24.10202 25.82359 31.9452 38.0668

TGA in Black & White

REFERENCES
Brochure of Orton . Lecture notes of Terry A. Ring, Chemical Engineering, University of Utah. HKUST Wikipedia. Advt. of TA Instruments in youtube.com

THANK
YOU