Curing of EVA. In the DSC experiment, T g is manifested by a sudden increase in the base line, indicating an increase in the heat capacity of the polymer (Fig.4). Normally, identification tasks are outsourced to a lab equipped with an infrared spectrophotometer (FT-IR). �ϼ�||�LX�0t�|�@(̇ޟV:��c�="�ܨ����|8��b���u���x����]+-��G�MH�'wc���O�j���'��m��̄i®�i�c� ����yW\�^��O4�����Ԟ�C���O{�Zy��lj�(${��� ܫ�nV^�ڴ:g������� ��P�@�"b"�z���fr>3�].N��rUA[$�}+�Pێ ����&�|�� �G8���1 �G9kXM�ׄ�ߍ׹��P6��q[1�fS��C��+�������|[��׿Z>���c��x��Y/7���s�l�{�3������IB �����ü�J�5H���]�F�$�9�v�X�ιC}!w�q(�� :,:He�c���/F����]�Zݗ﫱�BS�S�:��߄�@E����3 An example DSC case study compared two different lots of poly(tetrafluoroethylene) (“PTFE”), which is a semi-crystalline polymer. TGA provides compli-mentary and supplementary characterization information to the most commonly used thermal Identification of polymers by means of DSC, TG, STA and computer-assisted database search Abstract. The rate at which the sample can be heated and cooled is controlled and often set to 10 °C per minute. ASTM E1356. CASE STUDY I: IDENTIFICATION OF UNKNOWN POLYMER USING DSC. Crystallization of semi-crystalline polymer into microcrystals is exothermic. 2) The Tg was consistent with a material that has a completely amorphous (non-crystalline) structure. Modulated temperature DSC is a special technique that can offer increased resolution to the measurement capabilities of DSC. However, there are several different types of polyamides commercially available, and the IR information did not reveal which one was in the part. It also provides essential information for troubleshooting when the material does not perform as expected, or when something in the product or process needs to be changed, such as raw materials. Figure 3 Conventional DSC and Modulated DSC (MDSC) of Petrolatum Sample. For example, heating the polymer, it will undergo … Monitoring the heat-capacity related signal as a function of the applied experimental conditions (such as a heating ramp) can determine how the heat capacity of the sample changes as it undergoes a phase change or a chemical reaction. This part showed low hydrolytic stability, resulting in deformation when used under hot, humid conditions. In addition, for the polymer industry, LINSEIS offers other high-quality measuring instruments such as heating microscopes , optical dilatometers , Light Flash … DSC analysis is a technique used to determine what happens to polymers when heated. The DSC plot, shown in Figure 7, revealed a small glass transition temperature (Tg) at 188°C. Temperature (°C) Heat Flow (mW) 126.96°C 191.7J/g 156.59°C 28.74J/g 131.12°C 156.85°C. DTA Thermogram of a Polymer Analysis of a polymer shows several features due to physical and chemical changes, including: Glass transition: glassy, amorphous polymer becomes flexible, H = 0, but change in C p. Often Tg ~ 2/3 Tm. A good reference to DSC and the other thermal analysis techniques described in later posts is Thermal Analysis of Polymers: Fundamentals and Applications, (JD Menczel and RB Prime, eds), Wiley, 2009. The DSC set-up is composed of a measurement chamber and a computer. Knowledge of the thermal properties of polymers is essential for developing the best methods for processing the materials into useful products and predicting performance during product lifetimes. This is indicative of an exothermic event because the temperature registered by the sample sensor is higher than that sensed for the reference. Differential scanning calorimetry (DSC) offers a quick and easy way to determine the purity of crystalline substances. Differential Scanning Calorimetry (DSC) is commonly used for polymer characterization with a focus on three typical applications. Di erential scanning calorimetry (DSC) is a technique used to investigate the response of polymers to heating. It is also available for a wide range of elastomers and plastics. Determination of Polymer Crystallinity by DSC Roger L. Blaine, Ph.D. TA Instruments, 109 Lukens Drive, New Castle DE 19720, USA ABSTACT Perhaps no fundamental property affects the physical properties of a polymer in so general a way as the degree of crystallinity. Figure 6 shows a plot of the Cp of aluminum oxide at the temperatures 6°C, 16°C, 26°C and 36°C, labeled with the steady-state “end point” Cp values. Identification of an unknown polymer is often needed, such as when plastic parts have been purchased from a supply chain not directly affiliated with the manufacturer. From polymer identification to flammability characterization to flexural strength testing, you can check our wider array of polymer testing services here. The ability of the MDSC to separate overlapping events, such as Tg and curing, into two distinct plots makes this a very powerful tool for analyzing complex materials and mixtures containing multiple components. Especially the Chip-DSC is a powerful tool to identify and evaluate polymers. Examples of these changes are melting point, glass transition temperature, specific heat capacity and heat of … Characterization of Polymers using Differential Scanning Calorimetry (DSC), Determining best processing temperatures (cure, injection molding, extrusion, heat welding), Comparing quality (failure analysis, new material evaluation), Determining phase separation (polymer blend, copolymer), Determining thermal stability (oxidation induction time), Determining effects of additives (blends, fillers, plasticizers, process aids), Measuring residual cure and Tg as a function of cure temperature/time, Setting specifications (verify material meets expectations, set limits for end-use conditions), Designing devices (evaluating performance under operating temperatures, choosing materials for specific applications), Estimating upper use temperature from Tg or melting point, Analyzing cure or crystallization kinetics. Only one measurement with a few milligrams of sample is needed. Once the PCM has been cooled below the freezing point, and is reheated, the magnitude of the Cp increase is identical. 10 Thermal Analysis of Polymers METTLER TOLEDO Selected Applications 2.1 Introduction This chapter describes how DSC is used to analyze a thermoplastic, PET (polyeth- ylene terephthalate), as comprehensively as possible. When the analysis is conducted using conventional DSC, the Tg and ΔHR overlap. A special application of the HPer DSC is the study of kinetic processes related to the thermal activity of polymers. Not only were the results obtainable in a timely manner, DSC analysis did not require large samples, numerous controls or extensive method development. Composition analysis is especially key for quality control of a polymer based material. DSC analysis in accordance with ISO 11357 provides the following valuable information for the development and quality control of polymers: Photo-DSC 204 F1 Phoenix® with UV coupling and ASC for up to 192 samples Product Identification and An illustration of the higher resolution that can be achieved using MDSC is presented in Figure 3. DSC can reveal several important thermal transitions in these materials. The endothermic step change (glass transition) occurs first in the scan, followed by an exothermic peak due to “cold” crystallization, which is then followed by the endothermic peak due to melting. Characterization of Polymers Using TGA W.J. The technique can analyze materials that exhibit either mass loss or gain due to decomposition, oxidation or loss of volatiles (such as moisture). The sample was heated from room temperature to 300 °C at a rate of 10°C/min. DSC testing was performed on a small slice taken from the part. Thermal analysis is a very useful tool for the analysis of various compounds. Polymer crystallinity can be determined with DSC by quantifying the heat associated with melting (fusion) of the polymer. Properties that respond to the cyclic heating rate are separated into the reversing signal, which include polymer transitions that significantly affect molecular mobility. Ethylene-Propylene-Diene-Rubber-Mixture (EPDM) UV curing. The percent crystallinity of each lot was determined by normalizing the measured heat of fusion to the literature value of 100% crystalline PTFE. Long term storage of polymers below Tg typically results in a gradual process of molecular relaxation. Polymer Identification Using the PerkinElmer Mid-Infrared Polymer Analysis System. Two pans are heated in the measurement chamber. Figure 6 MDSC Quasi-isothermal Results: Heat Capacity of Aluminum Oxide at Four Temperatures. Figure 7 DSC Plot for an Unknown Plastic Part, CASE STUDY II: THERMAL AND MORPHOLOGICAL VARIATIONS OF DIFFERENT LOTS OF MATERIAL. How to Perform a Differential Scanning Calorimetry Analysis of a Polymer Step 1: Preliminaries. Differential scanning calorimetry is a thermoanalytical technique in which the difference in the amount of heat required to increase the temperature of a sample and reference is measured as a function of temperature. Monitoring the Cp signal over time will show that the initial drop in the curve reaches a plateau, which marks the stage when the crosslinking reaction rate has significantly slowed. Though FT-IR data can reveal the chemical “family” of the material, the identification of the subclass of the polymer often calls for additional analytical methods. The following evidence led to the most likely assignment of the main type of polyamide in the plastic part: 1) The unknown plastic did not show a crystalline melting peak. Figure 1 shows a DSC plot for a polyethylene terephthalate (PET) sample, which had been cooled from the melt at an extremely high rate. The peak area represents the heat of fusion per gram of material for the PCM. about lamella-distribtuion, recrystallization etc. The conventional DSC plot does not have a well-defined peak shape. /Length 1342 DSC is a useful tool for studying this phenomenon known as “physical aging”. Initially, FT-IR analysis had shown the plastic to be consistent with a polyamide (nylon). Sichina, Marketing Manager Introduction Thermogravimetric analysis (TGA) is one of the members of the family of thermal analysis techniques used to characterize a wide variety of materials. The HPer DSC technique allows for the analysis of the metastability of polymers,. DSC is highly useful in its ability to deliver precise readings on a material’s specific heat capacity. The quality of plastic products depends on the quality of the polymers or polymer blends used during … Intertek provides Differential Scanning Calorimeter (DSC) thermal analysis for polymer and plastic research and development (R&D), quality control, product and process … Relaxation is a phenomenon that occurs when amorphous polymer chains form abnormally denser regions. This peak is referred to as the “enthalpy of relaxation” or “enthalpic recovery” (ΔHR). Oxidation peak would be absent in N 2 The upper portion of the Figure shows conventional DSC (non-modulated) data for a petrolatum sample (scanned at 10°C/minute), and the lower part shows MDSC data obtained for the same sample (scanned at 3°C/minute). This is done by dividing the signal by the measured heating rate, which converts it into a heat capacity signal. Especially the Chip-DSC is a powerful tool to identify and evaluate polymers. The “end point” of this steady-state condition is considered to be the heat capacity of the sample at that particular temperature. Non-vulcanized Natural Rubber — Evolded Gas Analysis (TG-GC-MS) Paints — Evolved Gas Analysis (FT-IR) Quality Control of Polymers by means of DSC - Thermal Behavior of Thermoplastic Polyurethane. 4 0 obj << The MDSC data in Figure 5 demonstrates the effective separation of these transitions: Tg is separated into the reversing heat flow plot, and the ΔHR is separated into the non-reversing heat flow plot. Glass transition temperature (T g ) of conjugated polymers (CPs) cannot be readily measured from conventional DSC with simple heat and cool scans.Herein, the authors measured heat capacity change at T g (Δc p ) for a series of conventional and donor–acceptor (D–A) CPs and compared them to polystyrene.Results show a more than one order of magnitude decrease in Δc p as the material … Generally, the temperature program for a DSC analysis is designed such that the sample holder temperature increases linearly as a function of time. Heating to Tg allows polymer chains move to a more relaxed condition; that is, the chains spring back to normal (pre-aging) volume and density conditions. Curing of EVA. This information is useful when comparing a series of different isothermal curing temperatures to narrow down the best curing conditions for achieving maximum cure with the highest throughput. IMPORTANCE OF CHARACTERIZING THERMAL BEHAVIORS OF POLYMERS. DSC can reveal several important thermal transitions in these materials. Table 1 compares the melting point data and the heat of fusion (calculated from the area of the melting peak). An example case in which DSC pinpointed the polymer subclass involved a molded part designed for use in hot humid conditions. In TGA the mass loss during heating is monitored under controlled temperature which provides information about thermal stability and changes in the composition of the … A good reference to DSC and the other thermal analysis techniques described in later posts is Thermal Analysis of Polymers: Fundamentals and Applications, (JD Menczel and RB Prime, eds), Wiley, 2009. Figure 1 DSC Scan of Polyethylene Terephthalate: Heat Flow versus Temperature. Before testing, each lot was thermally treated under identical conditions to impart the same thermal history to the crystalline phase. This work is about the identification of polymers by means of differential scanning calorimetry (DSC),... Introduction. It includes thermoplastics and thermoset, rubbers, or elastomer based … Cross contamination of a resin with another polymer can occur in melt processing equipment. Applications Include: ∑ Polymers o Identification o Melt Point o Glass Transition Point o Degree of Crystallization o Cross-Linking Characterization Ethylene-Propylene-Diene-Rubber-Mixture (EPDM) UV curing. The initial DSC heating scan of physically aged polymers commonly reveals an endothermic peak near the trailing edge of the Tg step-change. This paper will provide an overview of DSC. To find out more, please see our privacy policy. 100 110 120 130 140 150 160 170 -20 -15 -10 -5 0 5. This analytical technique has found use in addressing a variety of customer needs such as contamination analysis, material verification, R&D, reverse engineering, and failure analysis. DSC analysis provides test data for a wide range of materials, including polymers, plastics, composites, laminates, adhesives, food, coatings, pharmaceuticals, organic materials, rubber, petroleum, chemicals, explosives, biological samples and more. If the sample is held long enough at this particular temperature, and the sample does not undergo any transitions, the plot of Cp versus time will appear linear (flat) at some given time. The aluminum oxide experiment is used to verify DSC accuracy by comparing the Cp data with the literature values at the corresponding temperatures. Many modern DSC instruments have the ability to measure the absolute heat flow. This information narrowed down the classification of the unknown to a possible blend of semi-aromatic polyamide with a reinforcing agent, such as fiberglass. Examples of these changes are melting point, glass transition temperature, specific heat capacity and heat of transition determinations. Thermogravimetric analysis (TGA) of polymers is conducted to measure weight changes as a function of temperature and time. 10 Thermal Analysis of Polymers METTLER TOLEDO Selected Applications 2.1 Introduction This chapter describes how DSC is used to analyze a thermoplastic, PET (polyeth- ylene terephthalate), as comprehensively as possible. The heat flow properties associated with these thermal events are found in the MDSC plots of the non-reversing signal. Case studies will be discussed to demonstrate many of the capabilities of this sensitive analytical instrument. The presenters in the DSC video series recently collaborated to write “Thermal Analysis of Polymers: Fundamentals and Applications,” by Menczel and Prime, editors, Wiley, 2009. “Basic Principles of DSC” by Joseph Menczel, Ph.D. IMPORTANCE OF CHARACTERIZING THERMAL BEHAVIORS OF POLYMERS. For example, the reversing heat flow plot suggests two overlapping melting peaks, which can be integrated to provide melting points of the two suspected types of crystalline fractions in the material. In the simplest terms, Differential Scanning Calorimetry (DSC) is a thermal analysis technique used by material testing labs like ACE Products and Consulting to investigate the response of polymers to heating. Differential scanning calorimetry is a technique we use to study what happens to polymers when they're heated. DSC Analysis. This tool features many powerful techniques for studying polymer thermal properties and provides essential information to the polymer industry and end users of polymer-based products. The control raw materials suspected to be the contaminant can also be analyzed by DSC. Thermal techniques like differential scanning calorimetry (DSC) and modulated temperature DSC (MDSC), thermogravimetric analysis (TGA), thermomechanical analysis (TMA) and dynamic mechanical analysis (DMA) are established techniques for characterizing the structure and morphology of polymers. Polymers — Behavior under Pressure. Differential Scanning Calorimetry (DSC) gives information about phase changes and chemical reactions. TGA provides compli-mentary and supplementary characterization information to the … The reference sample should have It’s a very popular … DSC is highly useful in its ability to deliver precise readings on a material’s specific heat capacity. These were measured using DSC analysis. This is called an endotherm and, in these cases, the temperature sensor measures a lower temperature for the sample compared to the reference. But these properties change with the polymer structure. Differential scanning calorimetry (DSC) is a thermoanalytical technique used to study the thermal properties of the polymer using a differential scanning calorimeter. Differential Scanning Calorimetry (DSC) Standardized Tests. DSC analysis is a technique used to determine what happens to polymers when heated. Different Types of Polyethylene. Curing of EVA. DSC melting curves contain a lot of information, e.g. The polymer analysis required the determination of the glass transition temperature (T g) and melting temperature of the pellet samples. When the sample evolves heat through some thermal process, such as a crosslinking reaction, the DSC plot shows an increase in heat flow. DSC is used to measure enthalpy changes due to changes in the physical and chemical properties of a material as a function of temperature or time. In this case, the heat capacity of the epoxy decreases as it changes from an uncured liquid to a solid network. Differential scanning calorimetry ( DSC) is the most frequently used thermal analysis technique alongside TGA, TMA and DMA. about lamella-distribtuion, recrystallization etc. DSC analysis can also be employed for more specialized applications including oxidative induction time (OIT) measurements and kinetics studies of curing polymers. Non-vulcanized Natural Rubber — Evolded Gas Analysis (TG-GC-MS) Paints — Evolved Gas Analysis (FT-IR) Quality Control of Polymers by means of DSC - Thermal Behavior of Thermoplastic Polyurethane. For example, Figure 2 shows a DSC plot of the heat capacity of a phase change material (PCM) that was measured directly during a temperature scan. This analytical technique has found use in addressing a variety of customer needs such as contamination analysis, material verification, R&D, reverse engineering, and failure analysis. Variations in thermal and morphological properties can affect polymer performance and processability. The melting of a crystalline polymer is one example. The lower crystallinity of Lot 1 could probably decrease the material density. This densification can adversely affect performance by causing embrittlement, dimensional change and/or the development of internal stresses. Table 1 DSC Data Comparison of Different PTFE Lots, CASE STUDY III: POLYMER CONTAMINANT INVESTIGATION BY DSC. Several commercial semi-aromatic polyamides, which contain high levels of benzene rings, are known to be wholly amorphous. For example, polypropylene (PP), polyoxymethylene (POM) and polyamide-6 (PA6) were tested using this method. ASTM E1269. As shown, PTFE Lot 1 was 72% crystalline, which was significantly lower compared to the 82% of Lot 2. Non-vulcanized Natural Rubber — Evolded Gas Analysis (TG-GC-MS) Paints — Evolved Gas Analysis (FT-IR) Quality Control of Polymers by means of DSC - Thermal Behavior of Thermoplastic Polyurethane. Please click Continue to provide your authorization and permanently remove this message. The baseline, which is the heat flow signal of the DSC in the absence of a thermal event, is much flatter and more reproducible using Tzero Technology. The quantity of heat flowing into and out of the DSC sensor is not only dependent on the applied temperature and the properties of the sample, but also on the thermal resistance and capacitance of both sides of the DSC cell (the reference and the sample sides). After verification, the polymer samples of interest can be run using a series of temperatures within the verified performance range. This provides for the identification of weak thermal events and improves the accuracy of heat capacity measurements. Typically 2 to 20 mg of material is placed in an aluminum capsule, shown above left, which is then placed on the sample (s) side of the DSC cell. ABS, the short form of acrylonitrile-butadiene-styrene, is a … Differential scanning calorimetry (DSC) is the most frequently used thermal analysis technique alongside TGA, TMA and DMA. ASTM D3418. For example, when a polymer in the glassy phase is heated to a certain temperature, it can undergo a phase change which induces liquid-like flow. DSC can be used to study the melting of a crystalline polymer or the glass transition. Beyond this time point the reaction will become sluggish, which can necessitate extra processing time or post-baking that will reduce throughput of cured parts. Identification of a polymer’s melting, crystallization, and glass transition temperatures can help us characterize and compare such … To accomplish this, the MDSC signals are plotted two ways: (1) Reversing Heat Flow versus Temperature for analyzing Tg, and, (2) Reversing Heat Capacity versus Temperature to analyze the change in Cp. 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