A G E N DA : T G A T H E O RY, O P E R A T I O N A N D CALLIBRATION

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

material and to predict their thermal stability at temperatures up to

1000c. The technique can characterize materials that exhibit weight loss or gain due to decomposition, oxidation, or dehydration.

Mass of sample is plotted against time

WHAT TGA CAN TELL

Thermal stability of materials Oxidative stability of materials Composition of Multi-component system Estimated lifetime of a product Decomposition kinetics of materials The effect of reactive or corrosive atmospheres on materials

Moisture and volatiles content of materials

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

It is good to use Auto sampler, most TGA instruments are completely

automated Increases temperature linearly Most samples 1-100mg

Can detect changes up to .1 g

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

Fast cooling through use of forced air Temperature monitored by:

Thermocouple- close to but not touching the sample, typical precision of .1C

STANDARD FURNACE

PURGE GAS SYSTEM

Ar or N2 to prevent unwanted oxidation 02 can be used but it depends on the purpose of analysis

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

HOW DOES IT WORKS?

Measures loss of mass over time or temperature Change in mass causes deflection of beam Photodiode amplifies current

Current pulsing through magnetic coil between poles of the permanent

magnet causes a magnetic field to restore the balance beam to the original position Same current amplified by photodiode is converted to mass-loss information and plotted against temperature or time to cerate a Thermo gram

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

CALCIUM OXALATE DECOMPOSITION

CALCIUM OXALATE DECOMPOSITION

1st Step CaC2O4*H2O(s)
calcium oxalate Monohydrate

CaC2O4(s)+H2O(g)
calcium oxalate

2nd Step CaC2O4(s)

calcium oxalate

CaCO3 + CO2 (g)

calcium carbonate

3rd Step CaCO3 (s)

calcium carbonate

Cao(s) + CO2 (g)

calcium oxide

TGA CURVES ARE NOT FINGERPRINT CURVE

Because most event that occur in a TGA are Kinetic in nature (meaning they are dependent on absolute temperature and time spent at that temperature), any experimental parameter that can effect the reaction rate will change the shape /

transition temperatures of the curve. These thing include:

Pan material, shape and size Ramp rate Purge gas

Sample mass, volume/form and morphology

TGA PERFORMANCE CRITERIA

Baseline -drift Affected by TGA construction, balance quality, and buoyancy effect
Sensitivity Affected by TGA balance quality Reproducibility Affected by balance quality, temperature control, and construction quality Temperature accuracy Affected by thermocouple placement, calibration stability, pure gas interaction

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

optimized using Hi-res TGA

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:

Mass of the sample

Differences between sample temperature and

temperature inside the furnace

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