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Definition and review of instrument Balance, furnace and heat exchanger review Mass and temperature calibration Purge as consideration Baseline considration Sample prepration and pan selection
WHAT IS TGA?
TGA measures the amount and rate of change in the weight of a material as a function of temperature or time in a controlled atmosphere. Measurement are used primarily to determine the composition of
INSTRUMENT CONSIST
Instrument has main parts:
Thermo balance Furnace Pure gas system Data collection system
THERMO BALANCE
Sample holder + cup housed inside furnace Platinum 40-500 L
FURNACE
House sample holder and cup Temperatures up to 1600C at max rate 200C/min Typical rates from .1C /min-100C /min
Thermally isolated Due to high temperature reached by the furnace the rest has to be thermally isolated from the rest of instrument from damage
STANDARD FURNACE
TGA BALANCE
The balance operates on a null-balance principle. At the zero, or null position equal amounts of light shines on the 2 photodiodes. If the balance moves out of the null position an unequal amount of light shines on the 2 photodiodes. Current is then applied to the meter movement to return the balance to null position. The amount of current applied is proportional to the weight loss
or gain.
BALANCE
THE THERMOGRAM
Y-axis: mass in mg weight percent X-axis: temperature or time Curve always being at top as sample is intact and drops to 0 Plateau desirable Temperature ramp must be linear
EXAMPLE
CaC2O4(s)+H2O(g)
calcium oxalate
TGA PERFORMANCE
TGA performance is primarily a function of balance sensitivity and baseline stability Balance sensitivity is optimized through design and construction
techniques
Baseline stability is a function of instrument design.as well as purge gases control TGA resolution is primarily a function of heating rate, but can be
E R RO R S I N T H E R M O G R AV I M E T R I C A N A LY S I S
Heating rate:
No standard heating rate Using gas can accelerate or slower down the acceleration of sample Mass of air can cause a small sample to decompose as faster than large samples Decomposition of analysis is endothermic or exothermic if the mass of samples is too large it can affect the require temperature of samples
Gases used:
QUALITATIVE APPLICATIONS
Composition analysis Method modification Material characterization identification
QUANTITATIVE APPLICATIONS
Decomposition profiles
Thermal stability polymers Thermogravimetrymass spectrometry Using a Simple capillary Interface High resolution TGA Kinetics Determination of Carbon Black Pigment in Nylon 66 Evaluation of Zeolite catalysts Clarification of inorganic decomposition by TG-MS Characterization of polyurethane by TGA
THANK YOU
Presented by: AMAN ARORA PIYUSH PALIWAL ANUP KUMAR JHODE PAVAN GAUTAM