endobj In this case of calcium carbonate we know: • CaCO 3 is an irritant! Interpretation of DSC Curve: DSC curve of a pure compound is a fingerprint of in which compound in the context of transition temperature as well as heat needed for that transition. hެVmo�H�++ݗT�t��k�T!M��B���C|p`�Ʀ�I����,���&��xdz3���>;FH�gBr��H �)�i�2m����)�L@���z �A`I�LD�0�b(�4ͤ�!����8q� fL�1c��É�l�O�l�j��i�����D�^��䒸tRG���nq��t��ˋ�p�R�mw��]��뿈��C��e-�g�!�\���/�$� 2 DSC Training Course 2900 Series DSC’s DSC 2010 DSC 2910 DSC 2920 DSC Training Course Q1000 Q100 Q10 First Generation Q Series™ DSCs. 89 Use of heat flows from DSC curve for calculation of specific heat of the solid materials E. Morîntale1, A. Harabor1, C. Constantinescu2, P. Rotaru1 1University of Craiova, Faculty of Physics, 13 A.I. Polyethylene terephthalate or PETE, is a commonly used plastic in food packaging, including beverage bottles: PETE is a semi-crystalline polymer. because DSC is easy-to-use, DSC has become the most commonly used thermal analysis technique. h�bbd```b``�".�HF��"Y��L�`v3X�$�T �� ��L6�E��Un�D�Șb��lr*��Q�ˀ$���R{H��T[q-��9g�b+��؊ ���#�����D*�I5��~�1012�Ȃ}��H���ߚ� ��� 3.1 Heat Flux DSC In a heat ux DSC system the sample and reference are heated at the same rate from a single heating source as shown in Figure 6. Simultaneous measurement of … … Ease-of-use in this case refers to sample preparation and experimental setup, as well as interpretation of the results. DSC Interpretation Notes 1 of 4 Cooper/Glasgow 25/04/01 DSC Interpretation Notes-- Alan Cooper (Glasgow) These notes are intended to help in the interpretation, avoiding over-interpretation, of biomolecular DSC data (mainly for proteins). DSC measures the enthalpy (H) of unfolding that results from heat-induced denaturation. The higher the thermal transition midpoint (Tm), the more stable the molecule. For example, ... • The bottom right frame shows a live graph of your data once the test has started. 1215 0 obj <>stream A sample of known mass is heated or cooled and the changes in its heat capacity are tracked as changes in the heat flow. The peak temperature is an important experimental value in DSC measurements. Interpretation of Undesirable Events in DSC Data Applications. obscure the main message of the table or graph. 9. Common materials include foods, pharmaceuticals, electronic materials, polymers, ceramics, organic and inorganic compounds, even biological organisms… DSC analysis is used to measure melting temperature, heat of fusion, latent heat of melting, reaction energy and temperature, glass transition temperature, crystalline phase transition temperature and energy, precipitation energy and temperature, denaturization temperatures, oxidation induction times, and specific heat or heat capacity. 1.5 DSC Differential Scanning Calorimetry. The output from a DTA is temperature … Differential scanning calorimetry (DSC) measures the energy absorbed (endotherm) or produced ... curing peak on the DSC curve. %PDF-1.6 %���� 4 0 obj 5 Q What can we learn from this TGA Thermal Curve? Data Interpretation: The output of a DSC is a plot of heat flux (rate) versus temperature at a specified temperature ramp rate. They should be read in conjunction with more comprehensive treatments, some of which are listed at the end. x��UQo�0~���G�Vc�A�*am�DMS5E}�)��:�1WS��lHP���F��qw>�w��ֲ|�WNO�P�|��x���m�wv��-�E�.�\���N��6]�CQ��A4�ᗁ&� (\�ԅ�n?Ae�(3���s! 2 0 obj 3 DSC Training Course Second Generation Q-Series™ DSCs Q2000 Q200 AutoQ20 Introduction Epoxy adhesives are often used as adhesives and fillers for materials such as metal, glass, ceramic, and plastic. The article explains the reasons for these differences and discusses the possibilities for … G�YecJ0�[:&ႉ�zq6s>Xl����%J�_S���F��,R�"��? The DSC graph showing "ACV-1" is for a pure drug while "PM-1" is the graph of a physical mixture of that drug along with two other polymers. This is a … A We must first list all pertinent information we know about the sample before we can analyze the data. This work is about the identification of polymers by means of differential scanning calorimetry (DSC), thermogravimetry (TG) and simultaneous thermal analysis (STA) involving computer-assisted database search. 3 0 obj <>/Metadata 650 0 R/ViewerPreferences 651 0 R>> endobj The heat flux can be converted to CP by dividing by the constant rate of temperature change. Both the sample and reference are maintained at nearly the same temperature throughout the experiment. Differential scanning calorimetry (DSC) is a physical characterization method used to study thermal behavior of neat polymers, copolymers, polymer blends and composites. These thermosetting adhesives are mainly created from epoxy resins and curing agents. This paper will provide an overview of DSC. Glass Transition Temperature by DMA 150.49°C 156.10°C 151.64°C Polycarbonate 1Hz, 15µm amplitude 3°C/min 0.0 0.5 1.0 1.5 Tan Delta 0.1 1 10 100 1 Systematic differences in this quantity can occur depending on the measurement conditions and the origin of the peak. Interpreting DSC curves Part 1: Dynamic measurements The art of interpreting curves has yet to be integrated into commercially available com-puter programs. H33�m�� d�0����(g�0 �}� A Differential Scanning Calorimetry, or DSC, is a thermal analysis technique that looks at how a material’s heat capacity (Cp) is changed by temperature. A biomolecule in solution is in equilibrium between its native (folded) and denatured (unfolded) conformations. The measurement signal is the energy absorbed by or released by the sample in milliwatts. endstream endobj 1166 0 obj <>/Metadata 66 0 R/OpenAction 1167 0 R/PageLayout/SinglePage/Pages 1163 0 R/StructTreeRoot 93 0 R/Type/Catalog/ViewerPreferences<>>> endobj 1167 0 obj <> endobj 1168 0 obj <>/ExtGState<>/Font<>/ProcSet[/PDF/Text/ImageC]/Properties<>>>/XObject<>>>/Rotate 0/StructParents 3/TrimBox[0.0 0.0 594.0 792.0]/Type/Page>> endobj 1169 0 obj <>stream %%EOF Plots showing differences in heat flow between a sample and reference, as a function of time Thus, DSC curve could be used to infer about the presence of a particular compounds and its thermal behaviour. 1 0 obj The curve should now be cut into DSC allows you to detect endothermic In DSC, the heat flow to and from a sam-ple and a reference material is measured as a function of temperature as the sam-ple is heated, cooled or held at constant temperature. 3 DSC Instructions Two types of DSC instruments are widely used: the heat ux DSC (eg. For example, tables do not need to be boxed in with lines surrounding each value. Determination of the melting temperature, heat of fusion, and purity analysis of different samples of zidovudine (AZT) using DSC 39 F- fraction of sample melted at T m, R- gas constant, 8.314 J mol-1 deg. stream Differential Scanning Calorimetry (DSC) – provides information about thermal changes that do not involve a change in sample mass11 – more commonly used technique than TGA – Two basic types of DSC instruments: heat-flux and power compensation 1Haines, P. J. <> It requires a considerable amount of experience in thermal 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 DSC Analysis Technique. TA DSC and Mettler DSC) and the power compensated DSC (Perkin-Elmer system). %PDF-1.7 Conveying information efficiently goes along with frugal use of "non-data ink". Interpreting DSC Data 3 Splitting a Curve into Segments To cut a measurement curve into segments users will need to left-click on their curve of interest, causing it to turn white. One of the tools proven to address these needs is differential scanning calorimetry (DSC). Then, users will right click on the same curve to display a menu. <>/ExtGState<>/ProcSet[/PDF/Text/ImageB/ImageC/ImageI] >>/MediaBox[ 0 0 612 792] /Contents 4 0 R/Group<>/Tabs/S/StructParents 0>> The current field of thermal analysis is both diverse and dynamic. From this menu select the “Split Into Segments” option. 8. Similarly, "perspective" should not be added to two-dimensional charts and graphs, as it impedes quick and correct interpretation. DSC Data Analysis in Origin ... other objects in a graph window that reside in the gray area of the page are not visible in Window View mode. Differential scanning calorimetry (DSC) 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. One general limitation depicted is the possibility of multiple interpretations of a single measurement signal which sometimes makes definite identification difficult. Among those guidelines are the pre-treatment and sample preparation, amount of sample used, heating protocol, gas flow rate, and interpretation of DSC thermograms. h�b```b``�g`c`�� ̀ ��@Q������ln|:5qe��F�m^00�)2h>x��TH��^��K�b�U�.+ͪJ�-X2���H�c�U�:/�)'�^�X��6o�OP}WӤ̗&'w5)O�����д�� -l�B�;:��+@��b� �Ł���B|n@Z ���~ad�˨�`��郜�{�6�ë= DSC of PETE 4 The second direct information obtainable from DSC thermograms is the enthalpy associated with first order processes. In Draft View, the page automatically sizes to fill the graph window. DSC Measurements of Epoxy Adhesives 1. DSC-TGA (SDT): The Technique Q600 SDT Simultaneous DSC-TGA: Measures heat flow and weight changes simultaneously Simultaneous DSC-TGA measures both heat flow and weight changes in a material as a function of temperature or time in a controlled atmosphere. This allows the detection of transitions such as melts, The DSC graph showing "ACV-1" is for a pure drug while "PM-1" is the graph of a physical mixture of that drug along with two other polymers. During curing, the epoxy group starts a polymerization reaction, cross-links and DSC can elucidate the factors that contribute to the folding and stability o… 0 Differential scanning calorimetry• This technique is used to study what happens to polymers/samples upon heating• It is used to study thermal transitions of a polymer/sample (the changes that take place on heating) – For example: • The melting of a crystalline polymer • The glass transition • The crystallization 3. After molding, the plastic has crystalline and amorphous regions. There are, however, some common DSC events/ transitions that can be the cause of less than optimum results and/or misinterpretation. endobj 1202 0 obj <>/Filter/FlateDecode/ID[<8396A40228C5ED45AC5751051A60CB23>]/Index[1165 51]/Info 1164 0 R/Length 156/Prev 1324854/Root 1166 0 R/Size 1216/Type/XRef/W[1 3 1]>>stream Interpretation and analysis of DSC data may be difficult for some samples. Generally, the non-isothermal DSC is used for the identification of neat basic polymers as well as the determination of their purity and stability. Theoretically, almost any substance whether solid, semi-solid or liquid can be analyzed and characterized with thermal analytical techniques. Besides providing a wealth of information, Differential Scanning Calorimetry (DSC) is user-friendly in terms of sample preparation, experimental configuration, and interpretation of the results. %���� Differential Scanning Calorimetry (DSC) Differential Scanning Calorimetry (DSC) is an analytical technique which measures the heat flow into or out of a sample as a function of time and/or temperature. Although not a new field, more advanced instrumentation, techniques and applications are constantly appearing on the market and in the literature. DSC Although DSC is a simple, convenient and fast technique to measure lipid oxidation, some recommended guidelines should be considered to obtain reliable and reproducible results. 1165 0 obj <> endobj ; so be careful handling the sample, wear eye protection • It is hygroscopic (it absorbs or attracts moisture from the air). endstream endobj startxref It is also used to determine the change in heat capacity (ΔCp) of denaturation. Draft View has the fastest screen update of the four view modes. To obtain the graph of T m x 1/F from the DSC curve, some points, normally within the region between 10 and 50% of the peak, are evaluated. {4UN(8�X��������������vn��9�dQ['���YV7��d�JT�k��s�:�&�/�����e�Z��$�� 3�8��8﬌`���#�� ����s]�9�{�d��@��c {���p���V0LT��?HTL�A�Z�Y2_\�,�(3��3̵f�ʹ1͎;��t�����,�T�D�|�F����B �B��B��f�b��j��1e���9V ,P tJ�6"���͑��C�o��k{�~ۆh. [�i�u�n��0m�k���4NKG�p��8�V�C_v73��s&��dU�r�?��o�9�J����د���8�q�r�h���_O�k�r첊E��V�. <> Differential scanning calorimetry is a specific type of calorimetry including both a sample substance and a reference substance, residing in separate chambers. I~̝ä$u�a��g��&˃AΙ,�"�lj��3 7�y���!A�@h��m��,`j�{��`���t�?�� ���p���ҌA�Y?�f�m��9���, ���� The interpretation of a DSC measurement curve is therefore still some-thing you have to do yourself. Correct interpretation graph window PETE, is a semi-crystalline polymer it requires considerable. 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