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Thermogravimetric Analyzer (TGA) - A329

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Thermogravimetric Analyzer (TGA)
TGA TADiscovery5500-h2RaR0Z4iUch.jpg
Thermogravimetric Analyzer, TA Instruments, Discovery 5500
Document Type Article
Document Identifier 329
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Equipment

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Factory Cells

Introduction[edit | edit source]

Thermogravimetric Analysis (TGA) is a method that monitors the mass of a sample as the temperature is varied. It can be used to determine the fraction of volatiles and the thermal stability of a material.[1][2] Mass is monitored as a function of temperature or time in a controlled temperature and atmosphere program.[1]

The TGA instrument can heat samples up to temperatures of around 1200°C, depending on the make and model. It can also cool samples to around -40°C by using nitrogen fed into the chamber, which may vary on make and model of equipment. The typical sample size is between 2 and 50 mg.[1]

Features[edit | edit source]

The TGA consists of a sample pan, which is supported by a highly precise scale, and a furnace chamber that can be heated or cooled during the experiment. The mass of the sample is carefully monitored and logged during the temperature changes. The environment of the chamber is controlled by injecting a gas into the chamber during the experiment, the gas may be reactive, like air or oxygen, or inert, like argon or helium, depending on the desired outcomes of the test.[1][2][3]

Uses and Test Types[edit | edit source]

The TGA instruments can be used for polymers to quantify loss of water, solvent and other volatiles as well as characterizing pyrolysis, decomposition and oxidation to name a few.[1] Mass loss due to volatiles such as moisture or residual solvents occurs in general between ambient and 300°C. Reaction products generally happen between 100°C and 250°C, forming products such as water and formaldehyde. Degradation tends to occur between temperatures of 200°C and 800°C.[3]

There are three variations of tests generally performed in a TGA instrument. Firstly, a constant temperature increase from a specified temperature to a target temperature. This will show the temperature ranges at which gases are removed from the sample and the onset of thermal degradation. Secondly, a static test, where the temperature is held at a certain setpoint. This is usually used to monitor degradation over time at a specified temperature. Lastly, a stepwise increase in the temperature, where a sample is held at certain temperatures until the mass is stabilized. This may be used to monitor how decomposition occurs.[3]

Analysis of Results[edit | edit source]

Example graph from a TGA experiment with polystyrene. Showing % weight loss and first derivative of weight loss.

A typical TGA graph consist of the mass or percentage change in mass on the y-axis and the temperature or time on the x-axis. We can then see a drop in the mass at certain temperature ranges, indicating that a change in the compound has happened[1]. The graph can be used do determine how much of a certain component has been lost and what remains. For example the graph shown here displays the degradation of a polystyrene sample during a ramp of 4°C/min up to 500°C.

By using the first derivative of the TGA curve (DTG), it becomes clearer where there are events taking place in the mass loss curve and may aid in separating out different processes taking place.[3] This is through the DTG curve providing local maxima to indicate areas of maximum mass loss. In the example shown, the derivative curve clearly shows the temperature range where the maximum weight loss occurs and can assist in indicating where the weight loss is starting to occur.

Combining Instruments[edit | edit source]

The TGA gives information on the temperatures and times the mass of a sample changes, however it does not indicate the types of substances that are coming off the sample. A TGA may be combined with other instruments that can analyze the gasses coming off in a process usually referred to as evolved gas analysis (EGA). This is where the off gasses are transferred out of the TGA into a separate piece of equipment, usually a Fourier transform infrared spectroscopy (FTIR) or a mass spectroscopy (MS) device.[4] A TGA may also be combined with a differential scanning calorimeter (DSC) in order to provide energetic information of the sample as it proceeds through the temperature ramp. This will provide information on the enthalpy changes occurring and detect changes and reactions not apparent through mass observations. All these combinations are used to prevent ambiguities when performing tests on different samples, temperatures and atmospheric conditions, by simply performing all of the analyses at once.[3]


Related pages

Page type Links
Introduction to Composites Articles
Foundational Knowledge Articles
Foundational Knowledge Method Documents
Foundational Knowledge Worked Examples
Systems Knowledge Articles
Systems Knowledge Method Documents
Systems Knowledge Worked Examples
Systems Catalogue Articles
Systems Catalogue Objects – Material
Systems Catalogue Objects – Shape
Systems Catalogue Objects – Tooling and consumables
Systems Catalogue Objects – Equipment
Practice Documents
Case Studies
Perspectives Articles

References

  1. 1.0 1.1 1.2 1.3 1.4 1.5 [Ref] PerkinElmer (2015), A Beginner's Guide Thermogravimetric Analysis (TGA) FAQ (PDF), PerkinElmer, retrieved 20 July 2022CS1 maint: uses authors parameter (link) CS1 maint: date and year (link)
  2. 2.0 2.1 [Ref] Rajisha, K.R. et al. (2011). "Thermomechanical and spectroscopic characterization of natural fibre composites". Woodhead Publishing. doi:10.1533/9780857092281.2.241. Cite journal requires |journal= (help); |access-date= requires |url= (help)CS1 maint: extra punctuation (link) CS1 maint: uses authors parameter (link)
  3. 3.0 3.1 3.2 3.3 3.4 [Ref] Menczel, Joseph D.; Prime, R. Bruce (2009). Thermal Analysis of Polymers: Fundamentals and Applications. John Wiley & Sons, Inc.CS1 maint: uses authors parameter (link) CS1 maint: date and year (link)
  4. [Ref] Redshift (2019). [_What_is?_What_Instruments_to_Use?_What_Can_You_Achieve? "Evolved Gas Analysis (EGA), What is? What Instruments to Use? What Can You Achieve?"] Check |url= value (help) (published June 2019). Retrieved 21 July 2022.CS1 maint: uses authors parameter (link) CS1 maint: date and year (link)



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Welcome to the CKN Knowledge in Practice Centre (KPC). The KPC is a resource for learning and applying scientific knowledge to the practice of composites manufacturing. As you navigate around the KPC, refer back to the information on this right-hand pane as a resource for understanding the intricacies of composites processing and why the KPC is laid out in the way that it is. The following video explains the KPC approach:

Understanding Composites Processing

The Knowledge in Practice Centre (KPC) is centered around a structured method of thinking about composite material manufacturing. From the top down, the heirarchy consists of:

The way that the material, shape, tooling & consumables and equipment (abbreviated as MSTE) interact with each other during a process step is critical to the outcome of the manufacturing step, and ultimately critical to the quality of the finished part. The interactions between MSTE during a process step can be numerous and complex, but the Knowledge in Practice Centre aims to make you aware of these interactions, understand how one parameter affects another, and understand how to analyze the problem using a systems based approach. Using this approach, the factory can then be developed with a complete understanding and control of all interactions.

The relationship between material, shape, tooling & consumables and equipment during a process step


Interrelationship of Function, Shape, Material & Process

Design for manufacturing is critical to ensuring the producibility of a part. Trouble arises when it is considered too late or not at all in the design process. Conversely, process design (controlling the interactions between shape, material, tooling & consumables and equipment to achieve a desired outcome) must always consider the shape and material of the part. Ashby has developed and popularized the approach linking design (function) to the choice of material and shape, which influence the process selected and vice versa, as shown below:

The relationship between function, material, shape and process


Within the Knowledge in Practice Centre the same methodology is applied but the process is more fully defined by also explicitly calling out the equipment and tooling & consumables. Note that in common usage, a process which consists of many steps can be arbitrarily defined by just one step, e.g. "spray-up". Though convenient, this can be misleading.

The relationship between function, material, shape and process consisting of Equipment and Tooling and consumables


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The KPC's Practice and Case Study volumes consist of three types of workflows:

  • Development - Analyzing the interactions between MSTE in the process steps to make decisions on processing parameters and understanding how the process steps and factory cells fit within the factory.
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