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Questions and Answers
What is the significance of placing the sample relative to the balance and furnace in TGA, and how many possibilities are there?
What is the significance of placing the sample relative to the balance and furnace in TGA, and how many possibilities are there?
The sample holder and furnace must not be in contact. There are 3 main possibilities to place the sample relative to the balance and furnace.
What is the role of a PC in modern TGA instruments, and what features does it provide?
What is the role of a PC in modern TGA instruments, and what features does it provide?
The PC is incorporated into most commercially available instruments to control heating and cooling cycles, store data, and handle data. It also helps resolve overlapping thermal reactions.
What is the purpose of the 1st derivative of the Dm vs.T (DTG) curve in TGA, and when is it used?
What is the purpose of the 1st derivative of the Dm vs.T (DTG) curve in TGA, and when is it used?
The 1st derivative of the Dm vs.T (DTG) curve is used to resolve overlapping thermal reactions. It is used when there are multiple thermal reactions occurring simultaneously.
What are the different types of water that can be expelled during TGA, and how are they differentiated?
What are the different types of water that can be expelled during TGA, and how are they differentiated?
How is the water/moisture content calculated in TGA, and what is the formula used?
How is the water/moisture content calculated in TGA, and what is the formula used?
What is the DTG curve a measure of in thermogravimetry?
What is the DTG curve a measure of in thermogravimetry?
What is the significance of the maximum (or minimum) of the DTG curve in relation to the TG curve?
What is the significance of the maximum (or minimum) of the DTG curve in relation to the TG curve?
What is the advantage of using DTG in thermogravimetry?
What is the advantage of using DTG in thermogravimetry?
In the analysis of Copper Sulfate Penta Hydrate (CuSO4·5H2O), what is the significance of the three endothermic processes?
In the analysis of Copper Sulfate Penta Hydrate (CuSO4·5H2O), what is the significance of the three endothermic processes?
What is the significance of the area under the DTG curve?
What is the significance of the area under the DTG curve?
What is the primary purpose of initially heating the coal sample in an inert atmosphere during a thermogravimetry analysis?
What is the primary purpose of initially heating the coal sample in an inert atmosphere during a thermogravimetry analysis?
What is the purpose of switching the atmosphere from inert to oxidizing during a thermogravimetry analysis of coal?
What is the purpose of switching the atmosphere from inert to oxidizing during a thermogravimetry analysis of coal?
What is the advantage of using a sample robot in thermogravimetry analysis?
What is the advantage of using a sample robot in thermogravimetry analysis?
What is evolved gas analysis (EGA) used for in thermogravimetry?
What is evolved gas analysis (EGA) used for in thermogravimetry?
Why is it important to minimize the exposure of thermogravimetry samples to air?
Why is it important to minimize the exposure of thermogravimetry samples to air?
What is the primary purpose of Evolved Gas Analysis (EGA) in Thermogravimetry (TGA), and how does it correlate with TGA data?
What is the primary purpose of Evolved Gas Analysis (EGA) in Thermogravimetry (TGA), and how does it correlate with TGA data?
In Derivative Thermogravimetry (DTG), what does the peak of the DTG curve represent, and what information does it provide?
In Derivative Thermogravimetry (DTG), what does the peak of the DTG curve represent, and what information does it provide?
What is the significance of water content analysis in TGA, and how is it affected by heating rates?
What is the significance of water content analysis in TGA, and how is it affected by heating rates?
What is the principle behind Thermogravimetry (TGA), and what type of information does it provide?
What is the principle behind Thermogravimetry (TGA), and what type of information does it provide?
What is the significance of the DTG curve in relation to the TG curve in Thermogravimetry, and what information does it provide?
What is the significance of the DTG curve in relation to the TG curve in Thermogravimetry, and what information does it provide?
What is the purpose of hermetically sealing samples in thermogravimetry?
What is the purpose of hermetically sealing samples in thermogravimetry?
What type of variations in mass can occur in thermogravimetry?
What type of variations in mass can occur in thermogravimetry?
What is the significance of evolved gas analysis (EGA) in thermogravimetry?
What is the significance of evolved gas analysis (EGA) in thermogravimetry?
What are the primary components of a thermogravimetry instrument?
What are the primary components of a thermogravimetry instrument?
What is the advantage of using a simultaneous TG-MS-EGA instrument?
What is the advantage of using a simultaneous TG-MS-EGA instrument?
What is the purpose of thermogravimetry in determining the purity of a sample?
What is the purpose of thermogravimetry in determining the purity of a sample?
What is evolved gas analysis used for in thermogravimetry?
What is evolved gas analysis used for in thermogravimetry?
What is the role of derivative thermogravimetry (DTG) in thermogravimetry?
What is the role of derivative thermogravimetry (DTG) in thermogravimetry?
How is the water content of a sample determined using thermogravimetry?
How is the water content of a sample determined using thermogravimetry?
What is the derivative thermogravimetry (DTG) curve a measure of in thermogravimetry?
What is the derivative thermogravimetry (DTG) curve a measure of in thermogravimetry?
What is the primary principle of thermogravimetry, and how is it used to analyze materials?
What is the primary principle of thermogravimetry, and how is it used to analyze materials?
What type of information can be obtained from the derivative thermogravimetry (DTG) curve?
What type of information can be obtained from the derivative thermogravimetry (DTG) curve?
What is evolved gas analysis, and how is it used in thermogravimetry?
What is evolved gas analysis, and how is it used in thermogravimetry?
What is the significance of moisture content in materials, and how is it analyzed using thermogravimetry?
What is the significance of moisture content in materials, and how is it analyzed using thermogravimetry?
What are some typical applications of thermogravimetry in materials science and industry?
What are some typical applications of thermogravimetry in materials science and industry?
How does the atmosphere affect the results of a thermogravimetric analysis?
How does the atmosphere affect the results of a thermogravimetric analysis?
What is the significance of the temperature range in thermogravimetry, and how is it selected?
What is the significance of the temperature range in thermogravimetry, and how is it selected?
What is the advantage of using thermogravimetry for materials characterization?
What is the advantage of using thermogravimetry for materials characterization?
How does thermogravimetry differ from other thermal analysis techniques, such as differential scanning calorimetry (DSC)?
How does thermogravimetry differ from other thermal analysis techniques, such as differential scanning calorimetry (DSC)?
What is the importance of sample preparation in thermogravimetry, and how can it affect the results?
What is the importance of sample preparation in thermogravimetry, and how can it affect the results?
What is the primary difference between thermogravimetry and other thermal analysis techniques?
What is the primary difference between thermogravimetry and other thermal analysis techniques?
What is the significance of simultaneous measurements in thermoanalytical techniques?
What is the significance of simultaneous measurements in thermoanalytical techniques?
What is the role of the atmosphere in thermogravimetric analysis?
What is the role of the atmosphere in thermogravimetric analysis?
What is the primary advantage of computer-controlled instruments in thermoanalytics?
What is the primary advantage of computer-controlled instruments in thermoanalytics?
What is the significance of thermogravimetry in determining sample purity?
What is the significance of thermogravimetry in determining sample purity?
What is the relationship between thermogravimetry and thermal analysis?
What is the relationship between thermogravimetry and thermal analysis?
What is the role of thermal analysis in materials science and industry?
What is the role of thermal analysis in materials science and industry?
What is the primary principle behind thermogravimetric analysis?
What is the primary principle behind thermogravimetric analysis?
What is the significance of the temperature program in thermogravimetric analysis?
What is the significance of the temperature program in thermogravimetric analysis?
What is the role of evolved gas analysis in thermogravimetry?
What is the role of evolved gas analysis in thermogravimetry?
What is the primary function of the furnace in a thermogravimetry instrument?
What is the primary function of the furnace in a thermogravimetry instrument?
What is the significance of the sample chamber in a thermogravimetry instrument?
What is the significance of the sample chamber in a thermogravimetry instrument?
How does the type of pan used in the instrument affect the results of a thermogravimetry analysis?
How does the type of pan used in the instrument affect the results of a thermogravimetry analysis?
What is the purpose of the null-point weighing balance in a thermogravimetry instrument?
What is the purpose of the null-point weighing balance in a thermogravimetry instrument?
What is the advantage of using an isothermal or quasi-isothermal technique in thermogravimetry?
What is the advantage of using an isothermal or quasi-isothermal technique in thermogravimetry?
What is the significance of the derivative thermogravimetry (DTG) curve in thermogravimetry?
What is the significance of the derivative thermogravimetry (DTG) curve in thermogravimetry?
What is the purpose of the ceramic crucibles in sample handling for TGA and DSC?
What is the purpose of the ceramic crucibles in sample handling for TGA and DSC?
What is the significance of minimizing the exposure of thermogravimetry samples to air?
What is the significance of minimizing the exposure of thermogravimetry samples to air?
What is the role of the PC in modern TGA instruments?
What is the role of the PC in modern TGA instruments?
What is the significance of electrostatic effects in thermogravimetry?
What is the significance of electrostatic effects in thermogravimetry?
What is the purpose of using a reference sample in Differential Scanning Calorimetry (DSC)?
What is the purpose of using a reference sample in Differential Scanning Calorimetry (DSC)?
What is the difference between Thermodilometry (TD) and Thermomechanical Analysis (TMA)?
What is the difference between Thermodilometry (TD) and Thermomechanical Analysis (TMA)?
What is the significance of measuring the storage modulus (E') in Dynamic Mechanical Analysis (DMA)?
What is the significance of measuring the storage modulus (E') in Dynamic Mechanical Analysis (DMA)?
What is the purpose of adding a plasticizer to a polymer in DSC?
What is the purpose of adding a plasticizer to a polymer in DSC?
What is the unit of energy measurement in Differential Scanning Calorimetry (DSC)?
What is the unit of energy measurement in Differential Scanning Calorimetry (DSC)?
What is the main difference between Thermomechanical Analysis (TMA) and Dynamic Mechanical Analysis (DMA)?
What is the main difference between Thermomechanical Analysis (TMA) and Dynamic Mechanical Analysis (DMA)?
What is the purpose of using alumina or silicon carbide as a reference sample in DSC?
What is the purpose of using alumina or silicon carbide as a reference sample in DSC?
What is the advantage of using Dynamic Mechanical Analysis (DMA)?
What is the advantage of using Dynamic Mechanical Analysis (DMA)?
What is the significance of the heat flow in Differential Scanning Calorimetry (DSC)?
What is the significance of the heat flow in Differential Scanning Calorimetry (DSC)?
What is the purpose of clamping the sample in Dynamic Mechanical Analysis (DMA)?
What is the purpose of clamping the sample in Dynamic Mechanical Analysis (DMA)?
What is the effect of adding a plasticizer to a polymer?
What is the effect of adding a plasticizer to a polymer?
What happens to the glass transition temperature of a polymer as the plasticizer content increases?
What happens to the glass transition temperature of a polymer as the plasticizer content increases?
What is the state of a material above its glass transition temperature?
What is the state of a material above its glass transition temperature?
What is the purpose of using Hyper DSC?
What is the purpose of using Hyper DSC?
What is the temperature range of the cooling system in Hyper DSC?
What is the temperature range of the cooling system in Hyper DSC?
What is the advantage of using low-mass furnaces in Hyper DSC?
What is the advantage of using low-mass furnaces in Hyper DSC?
What is the purpose of closed-loop operation in Hyper DSC?
What is the purpose of closed-loop operation in Hyper DSC?
What is the significance of calorimetry in Hyper DSC?
What is the significance of calorimetry in Hyper DSC?
What is the effect of losing plasticizer on the glass transition temperature of a material?
What is the effect of losing plasticizer on the glass transition temperature of a material?
What is the purpose of optimizing materials using plasticizers?
What is the purpose of optimizing materials using plasticizers?
What factors affect the mass and temperature measurements in thermogravimetry?
What factors affect the mass and temperature measurements in thermogravimetry?
How are samples typically handled in thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC)?
How are samples typically handled in thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC)?
What is the primary difference between differential thermal analysis (DTA) and differential scanning calorimetry (DSC)?
What is the primary difference between differential thermal analysis (DTA) and differential scanning calorimetry (DSC)?
What does thermomechanical analysis (TMA) measure?
What does thermomechanical analysis (TMA) measure?
What are the two moduli measured in dynamic mechanical analysis (DMA)?
What are the two moduli measured in dynamic mechanical analysis (DMA)?
What is the purpose of adding plasticizers to polymers?
What is the purpose of adding plasticizers to polymers?
What is the advantage of using hyper DSC over conventional DSC systems?
What is the advantage of using hyper DSC over conventional DSC systems?
What is the role of evolved gas analysis (EGA) in thermogravimetry?
What is the role of evolved gas analysis (EGA) in thermogravimetry?
How do plasticizers affect the glass transition temperature of a material?
How do plasticizers affect the glass transition temperature of a material?
What is the primary advantage of dynamic mechanical analysis (DMA)?
What is the primary advantage of dynamic mechanical analysis (DMA)?
What is thermal analysis, and what is the main variable being monitored in this process?
What is thermal analysis, and what is the main variable being monitored in this process?
What are the types of properties that can be monitored during thermal analysis?
What are the types of properties that can be monitored during thermal analysis?
What is the significance of thermogravimetry (TG) in thermal analysis?
What is the significance of thermogravimetry (TG) in thermal analysis?
What are the essential components of a thermogravimetry (TG) instrument?
What are the essential components of a thermogravimetry (TG) instrument?
What is the primary purpose of thermogravimetry (TG) analysis?
What is the primary purpose of thermogravimetry (TG) analysis?
What is the significance of Differential Scanning Calorimetry (DSC) in thermal analysis?
What is the significance of Differential Scanning Calorimetry (DSC) in thermal analysis?
What types of thermal analysis techniques are used to monitor the properties of a sample?
What types of thermal analysis techniques are used to monitor the properties of a sample?
What is the significance of Evolved Gas Analysis (EGA) in thermogravimetry?
What is the significance of Evolved Gas Analysis (EGA) in thermogravimetry?
What is the primary purpose of Thermodilatometry (TD) in thermal analysis?
What is the primary purpose of Thermodilatometry (TD) in thermal analysis?
What is the significance of Dynamic Mechanical Analysis (DMA) in thermal analysis?
What is the significance of Dynamic Mechanical Analysis (DMA) in thermal analysis?
Study Notes
Here are the study notes in markdown format:
Thermogravimetry (TGA)
- Measures the variation in mass of a sample as a function of temperature (or time) in a controlled atmosphere
- Essential components:
- Balance
- Thermobalance
- Furnace
- Sample chamber
- Instrument control/data handling
- Applications:
- Drying/water content determination
- Decomposition behavior
- Chemical kinetics
- Sample purity determination
Evolved Gas Analysis (EGA)
- Studies the gas evolved from a heated sample that undergoes decomposition or desorption
- Can be coupled with Mass Spectrometry (MS), Fourier transform infrared spectroscopy (FTIR), or Gas Chromatography (GC) for evolved gas detection (EGD)
Thermogravimetry (TG) Instrumentation
- TG instruments:
- PerkinElmer, USA
- Mettler Tolledo, Switzerland
- SETARAM Instrumentation, France
- Sample handling:
- Samples are hermetically sealed and lid is pierced just before measurement
- Samples are stored in ceramic crucible and lid is removed just before experiment
TG-EGA
- Simultaneous TG-MS-EGA for Calcium Oxalate CaC2O4.H2O
- Applications:
- Materials' characterization
- Polymers Material analysis
- Pharmaceuticals
- Quality control
- Ceramics
- Process control
- Metals
- Alloys
Derivative Curve (DTG)
- Records the rate of mass change (dm/dt) vs. temperature
- Area under the DTG curve is proportional to the mass change
- Height of DTG peak at any temperature gives the rate of mass change
- Maximum or minimum of DTG curve corresponds to a point of inflection in TG curve
Applications of TG
- Materials:
- Composition
- Content
- Purity
- Effect of moisture
- Storage stability
- Chemical changes:
- Decomposition
- Pyrolysis
- Oxidation
- Stability
- Physical properties:
- Specific heat capacity
- Expansion coefficient and behavior
- Viscoelastic behavior
- Elastic modulus
Copper Sulfate Pentahydrate (CuSO4·5H2O)
- Three endothermic processes:
- 75°C: loss of 2 H2O
- 113°C: loss of 2 H2O
- 250°C: loss of 1 H2O
Handling of Samples
-
Sample robot (for TGA and DSC)
-
Advantages:
- Preparation of set of samples at the same time
- Overnight (weekend) measurements
-
Two ways:
- Automatic loading
- Automatic open### Thermogravimetry (TG)
-
Measures changes in the mass of a sample as a function of temperature or time in a controlled atmosphere
-
Loss of mass indicates vapour emission, while gain of mass indicates gas fixation
-
Essential components of the TG instrument:
- Balance and furnace (thermobalance)
- Sample chamber
- Instrument to control data handling
-
Analytical balance has a sensitivity of 1 microgram and can measure samples from 10 to 50 micrograms
-
Different types of balance mechanisms can be used, including:
- Beam spring
- Cantilever
- Torsion balance
- Null-point weighing balance
- Electromagnetic balance
Furnace
- Temperature range depends on the materials used
- Fused quartz tubes and kanthal-type heating elements can reach up to 1100°C
- Ceramic refractories such as alumina or mullite can reach up to 1500-1700°C
- Temperature reading above 1500°C can indicate material problems with the heating element, furnace construction, or thermocouples
Sample Handling
- Samples are airtight sealed and the lid is pierced just before measurements are taken
- Samples are stored in ceramic crucibles and the lid is removed just before the experiments
- Samples can be stored in sample changers to prevent loss of moisture or absorption of water
Evolved Gas Analysis (EGA)
- Studies the gas evolved from a heated sample undergoing decomposition/desorption
- Often coupled with techniques such as mass spectrometry, gas chromatography, or Fourier transform infrared spectroscopy to identify the gases produced
Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC)
- DTA measures the temperature difference against a reference sample
- DSC measures the difference in heating power needed on a sample
- Both methods measure heat flows and temperatures with transition in materials as functions of time and temperature upon heating and cooling in a controlled atmosphere
Factors Affecting Mass and Temperature Measurements
- Sample size and packing
- Heating rate
- Type of pan used in the instrument
- Gas flow (atmosphere the instrument is in)
- Electrostatic effects
- Condensation and reaction
- Buoyancy
- Sample holder
- Reaction enthalpy
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Description
Review the principles and applications of thermoanalytical methods, including Thermogravimetry (TGA) and Evolved Gas Analysis (EGA). Learn about the different furnace configurations and sample holders used in TGA.