{"id":252,"date":"2024-05-18T19:45:29","date_gmt":"2024-05-18T18:45:29","guid":{"rendered":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/chapter\/2-thermogravimetry\/"},"modified":"2024-05-19T19:26:10","modified_gmt":"2024-05-19T18:26:10","slug":"2-thermogravimetry","status":"publish","type":"chapter","link":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/chapter\/2-thermogravimetry\/","title":{"raw":"2. Thermogravimetry","rendered":"2. Thermogravimetry"},"content":{"raw":"<div>\r\n<div class=\"textbox textbox--learning-objectives\"><header class=\"textbox__header\">\r\n<p class=\"textbox__title\"><strong><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image1-7.png\" width=\"34.6666666666667px\" height=\"34.6666666666667px\" alt=\"image\" \/>Learning Objectives<\/strong><\/p>\r\n\r\n<\/header>\r\n<div class=\"textbox__content\">\r\n\r\nAfter completing this section, you should be able to:\r\n<ul>\r\n \t<li class=\"import-Normal\" style=\"text-align: justify\">Describe the effect of heat on materials.<\/li>\r\n \t<li class=\"import-Normal\" style=\"text-align: justify\">Identify physical and chemical transitions.<\/li>\r\n \t<li class=\"import-Normal\" style=\"text-align: justify\">Describe the essential features of a thermobalance.<\/li>\r\n \t<li class=\"import-Normal\" style=\"text-align: justify\">Draw and interpret thermogravimetric and derivative thermogravimetric curve for a known system.<\/li>\r\n \t<li class=\"import-Normal\" style=\"text-align: justify\">Illustrate the range of applications of thermogravimetry.<\/li>\r\n \t<li class=\"import-Normal\" style=\"text-align: justify\">Calculate % weight loss at every stage of decomposition and predict stoichiometry.<\/li>\r\n<\/ul>\r\n<\/div>\r\n<\/div>\r\n<\/div>\r\n<div class=\"2.-thermogravimetry\">\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-align: justify\">Thermogravimetry is a technique used to detect any physical or chemical transitions which are accompanied by a weight loss or weight gain as the sample is heated in a controlled manner.<\/p>\r\n<strong>2.1 Effect of heat on matter:<\/strong>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">We need to first understand the effects of heat on matter. And For further explanation please see Introductory Chemistry in <em>Libretexts<\/em><\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image2-11.png\" width=\"38px\" height=\"28.6666666666667px\" alt=\"image\" \/><a class=\"rId9\" href=\"https:\/\/chem.libretexts.org\/Bookshelves\/Introductory_Chemistry\/Introduction_to_General_Chemistry_(Malik)\/01%3A_Matter_energy_and_their_measurements\/1.09%3A_Heat_and_changes_in_physical_states_of_matter\">https:\/\/chem.libretexts.org\/Bookshelves\/Introductory_Chemistry\/Introduction_to_General_Chemistry_(Malik)\/01%3A_Matter_energy_and_their_measurements\/1.09%3A_Heat_and_changes_in_physical_states_of_matter<\/a><\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-align: justify\">Now, we have understood the effects of heat on matter and also able to identify the processes involving change in weight on heating through Activity 1D. It is important to keep in mind that the change in weight could be due to physical or chemical transitions. To be able to distinguish between physical and chemical transition, let us go through the next sub-topic.<\/p>\r\n<strong>2.2 Changes in matter: Physical and Chemical Changes<\/strong>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">For further explanation please see Introductory Chemistry in <em>Libretexts<\/em><\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image2-12.png\" width=\"38px\" height=\"28.6666666666667px\" alt=\"image\" \/><a class=\"rId10\" href=\"https:\/\/chem.libretexts.org\/Bookshelves\/Introductory_Chemistry\/Introductory_Chemistry\/03%3A_Matter_and_Energy\/3.06%3A_Changes_in_Matter_-_Physical_and_Chemical_Changes\">https:\/\/chem.libretexts.org\/Bookshelves\/Introductory_Chemistry\/Introductory_Chemistry\/03%3A_Matter_and_Energy\/3.06%3A_Changes_in_Matter_-_Physical_and_Chemical_Changes#:~:text=3.6%3A%20Changes%20in%20Matter%20%20Physical%20and%20Chemical,4%20Summary%20...%205%20Contributions%20%26%20Attributions%20<\/a><\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><strong><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-20.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/>Activity 2A:<\/strong> Can you assign which of these transitions will be physical or chemical transitions? ( <strong>please indicate by writing 'Y' in appropriate column<\/strong>)<\/p>\r\n\r\n<table style=\"width: 493px;height: 310px\">\r\n<tbody>\r\n<tr class=\"a-R\" style=\"height: 16.7pt\">\r\n<td class=\"a-C\" style=\"background-color: #5b9bd5;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\r\n<p class=\"import-Normal\"><strong>Phenomenon<\/strong><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #5b9bd5;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\r\n<p class=\"import-Normal\"><strong>Physical<\/strong><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #5b9bd5;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\r\n<p class=\"import-Normal\"><strong>Chemical <\/strong><\/p>\r\n<\/td>\r\n<\/tr>\r\n<tr class=\"a-R\" style=\"height: 16.7pt\">\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\r\n<p class=\"import-Normal\">Adsorption<\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<\/tr>\r\n<tr class=\"a-R\" style=\"height: 19.05pt\">\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\r\n<p class=\"import-Normal\">Dehydration<\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<\/tr>\r\n<tr class=\"a-R\" style=\"height: 19.05pt\">\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\r\n<p class=\"import-Normal\">Desorption<\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<\/tr>\r\n<tr class=\"a-R\" style=\"height: 16.7pt\">\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\r\n<p class=\"import-Normal\">Fusion (melting)<\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<\/tr>\r\n<tr class=\"a-R\" style=\"height: 16.7pt\">\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\r\n<p class=\"import-Normal\">Chemisorption<\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<\/tr>\r\n<tr class=\"a-R\" style=\"height: 16.7pt\">\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\r\n<p class=\"import-Normal\">Vaporization<\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<\/tr>\r\n<tr class=\"a-R\" style=\"height: 16.7pt\">\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\r\n<p class=\"import-Normal\">Decomposition<\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<\/tr>\r\n<tr class=\"a-R\" style=\"height: 16.7pt\">\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\r\n<p class=\"import-Normal\">Redox reactions<\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<\/tr>\r\n<tr class=\"a-R\" style=\"height: 16.7pt\">\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\r\n<p class=\"import-Normal\">Reduction in gaseous atmosphere<\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\r\n<p class=\"import-Normal\"><\/p>\r\n<\/td>\r\n<\/tr>\r\n<tr style=\"height: 10px\">\r\n<td style=\"width: 237.594px;height: 10px\"><\/td>\r\n<td style=\"width: 102.031px;height: 10px\"><\/td>\r\n<td style=\"width: 112.5px;height: 10px\"><\/td>\r\n<\/tr>\r\n<\/tbody>\r\n<\/table>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 (<span style=\"color: #ff6600\">Dodd &amp; Tonge, 2008<\/span>)<\/p>\r\n<p class=\"import-Normal\"><strong>2.3 Principle and Instrumentation of TGA:<\/strong><\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">The instrument used to carry out thermogravimetric analysis is known as \u201cthermobalance\u201d.<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image4-2.jpg\" width=\"470.798530183727px\" height=\"223.037270341207px\" alt=\"image\" \/><\/p>\r\n<p class=\"import-Normal\" style=\"text-indent: 36pt\"><strong>Figure 2.3<\/strong> Block diagram of a thermobalance<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-indent: 36pt\">(Source: <a class=\"rId13\" href=\"https:\/\/images.app.goo.gl\/uyRxxbkVNkxLF3nT7\">https:\/\/images.app.goo.gl\/uyRxxbkVNkxLF3nT7<\/a>)<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><strong>Working:<\/strong> Please go through the <em>Chemlibre<\/em> link to understand the principle and working of a thermobalance.<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image2-13.png\" width=\"38px\" height=\"28.6666666666667px\" alt=\"image\" \/><a class=\"rId14\" href=\"https:\/\/chem.libretexts.org\/Bookshelves\/Analytical_Chemistry\/Instrumental_Analysis_(LibreTexts)\/31%3A_Thermal_Methods\/31.01%3A_Thermogravimetric_Methods\">https:\/\/chem.libretexts.org\/Bookshelves\/Analytical_Chemistry\/Instrumental_Analysis_(LibreTexts)\/31%3A_Thermal_Methods\/31.01%3A_Thermogravimetric_Methods<\/a><\/p>\r\n<strong>2.4 Interpretation of thermogravimetric curve:<\/strong>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-align: justify\">The graphical information obtained from thermogravimetric analysis is known as thermogram\/pyrolysis curve. The TG curve is a plot of weight (W) decreasing downwards on the y-axis (ordinate), and temperature (T) increasing to the right on the x-axis (abscissa). A typical thermogram for a single step decomposition is shown in Fig. 2.4.<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-align: justify\">The plateau \u2018AB\u2019 indicates no change in weight or the temperature range over which the sample is thermally stable. At point \u2018B\u2019 the sample starts decomposing which is indicated by an inflexion.<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-align: justify\">Please read the following text explaining the interpretation of thermogram and then attempt Activity 2B.<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image2-14.png\" width=\"38px\" height=\"28.6666666666667px\" alt=\"image\" \/><a class=\"rId15\" href=\"https:\/\/chem.libretexts.org\/Courses\/Franklin_and_Marshall_College\/Introduction_to_Materials_Characterization__CHM_412_Collaborative_Text\/Thermal_Analysis\/Thermogravimetric_analysis_(TGA)\">https:\/\/chem.libretexts.org\/Courses\/Franklin_and_Marshall_College\/Introduction_to_Materials_Characterization__CHM_412_Collaborative_Text\/Thermal_Analysis\/Thermogravimetric_analysis_(TGA)<\/a><\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-21.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/> <strong>Activity 2B: <\/strong>A typical thermogram is shown below, observe and fill in the\u00a0 blanks by choosing the most appropriate answer. (Hint: Initial mass at \u2018A\u2019 is considered as 100%)<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-indent: 36pt\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image5-5.png\" width=\"300px\" height=\"214.112965879265px\" alt=\"image\" \/><\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><strong>Figure 2.4<\/strong> Typical TG curve<\/p>\r\n\r\n<ol>\r\n \t<li class=\"import-Normal\">The part of the TG curve where the mass is essentially constant______________<\/li>\r\n \t<li class=\"import-Normal\">The temperature at which cumulative mass change reaches a magnitude that the thermobalance can detect ________________<\/li>\r\n \t<li class=\"import-Normal\">The temperature at which the cumulative mass change reaches a maximum_______________<\/li>\r\n<\/ol>\r\n<p class=\"import-Normal\" style=\"text-indent: 36pt\"><strong>Choose from the following options.<\/strong><\/p>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 i. the initial temperature (B)<\/p>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 ii. the record of weight from temperature B to C<\/p>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 iii. the final temperature C<\/p>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 iv. the plateau (AB)<\/p>\r\n<p class=\"import-Normal\">(<span style=\"color: #ff6600\">Dodd &amp; Tonge, 2008<\/span>)<\/p>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-22.png\" width=\"31.3333333333333px\" height=\"32.6666666666667px\" alt=\"image\" class=\"\" \/><strong> Activity 2C: <\/strong>For the processes given in the table, predict the nature of thermogram (Type- X\/Type-Y\/None of theses)<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image6-4.png\" width=\"298\" height=\"308\" alt=\"image\" class=\"\" \/><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image7-2.png\" width=\"197.103727034121px\" height=\"329.2px\" alt=\"image\" \/><\/p>\r\n<strong style=\"font-size: 1em\">2.5 Need for Derivative Thermogravimetry (DTG):<\/strong>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">In the above example (Fig.2.4a.), we have considered the thermogravimetric curve which represents a single stage decomposition.<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">Figures \u20182.5a\u2019 and \u20182.5b\u2019 show two-step and three-step decompositions respectively. In both these figures there is an overlay of TGA and DTG thermogram, clearly depicting advantages of DTG over TGA thermogram in locating the exact decomposition temperature.<\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 72pt;text-indent: 36pt\"><strong><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image8-3.png\" width=\"391.713910761155px\" height=\"184.335958005249px\" alt=\"image\" \/><\/strong><\/p>\r\n<p class=\"import-Normal\"><strong>Figure 2.5a. <\/strong>Thermogravimetric (TG) and Derivative thermogravimetry (DTG)<\/p>\r\n<p class=\"import-Normal\">curves for PVP at a heating rate of 10\u00b0C\/min. (<span style=\"color: #ff6600\">Source: Al-Hada et al., 2014<\/span>)<\/p>\r\n<p class=\"import-Normal\"><a class=\"rId20\" href=\"https:\/\/images.app.goo.gl\/fWChwNJi9uxfHZAJ7\">https:\/\/images.app.goo.gl\/fWChwNJi9uxfHZAJ7<\/a><\/p>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0<img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image9-2.png\" width=\"495.402939632546px\" height=\"223.379317585302px\" alt=\"image\" class=\"\" \/><\/p>\r\n<p class=\"import-Normal\" style=\"text-indent: 36pt\"><strong>Figure 2.5b. <\/strong>TGA test result of calcium oxalate <span style=\"text-align: initial;text-indent: 36pt;font-size: 1em\">monohydrate (<\/span><span style=\"color: #ff6600\">Source: Chegg.com<\/span><span style=\"text-align: initial;text-indent: 36pt;font-size: 1em\">) <\/span><a class=\"rId22\" href=\"https:\/\/images.app.goo.gl\/1Hbp2vSV2rBjeFc4A\" style=\"text-align: initial;text-indent: 36pt;font-size: 1em\">https:\/\/images.app.goo.gl\/1Hbp2vSV2rBjeFc4A<\/a><\/p>\r\n<p class=\"import-Normal\" style=\"text-align: justify\">Figure \u20182.5b\u2019 is for the decomposition of calcium oxalate monohydrate, the weight loss commences just above 100 \u1d52C and continues up to 200 \u1d52C. Between about 400 \u1d52C and 500 \u1d52C further decomposition occurs, to give a product which is stable up to 700 \u1d52C before decomposing to give another stable compound at 800\u1d52C. Every process of decomposition continues over a range of temperature hence the DTG curve is useful in providing information regarding precise decomposition temperature at every stage.<\/p>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-23.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2D:<\/strong> ( <span style=\"color: #ff6600\">James &amp; Tonge, 2008<\/span>)<\/p>\r\n<p class=\"import-Normal\" style=\"text-indent: 18pt\">Indicate by circling either T for true or F for false,<\/p>\r\n\r\n<ol>\r\n \t<li class=\"import-Normal\">A derivative thermogravimetric (DTG) curve represents a plot of mass of sample, as a function of temperature. T\/F<\/li>\r\n \t<li class=\"import-Normal\">A point of inflection on a thermogravimetric (TG) curve will correspond to a minimum on the DTG curve for a given chemical decomposition.T\/F<\/li>\r\n \t<li class=\"import-Normal\">A \u2018plateau\u2019 on a TG curve will not necessarily correspond to a zero ordinate value of the DTG curve.T\/F<\/li>\r\n \t<li class=\"import-Normal\">Thermal decompositions which overlap are often indicated more clearly by DTG curves than by the corresponding TG curves.T\/F<\/li>\r\n<\/ol>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-24.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2E: <\/strong>Complete the following reaction for the decomposition of calcium carbonate. Identify the volatile and stable compound\/s remaining in the crucible post decomposition and indicate these on the thermogram.<\/p>\r\n<p class=\"import-NormalWeb\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image10.jpeg\" width=\"496px\" height=\"187.333333333333px\" alt=\"image\" \/><\/p>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-25.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2F: <\/strong>Observe the image given below for the decomposition of magnesium oxalate monohydrate and complete the activity.<\/p>\r\n\r\n<ul>\r\n \t<li class=\"import-Normal\">Identify the volatile product and the residue remaining in the crucible at each stage of decomposition.<\/li>\r\n \t<li class=\"import-Normal\">Write the decomposition reaction taking place at each stage.<\/li>\r\n \t<li class=\"import-Normal\">Draw a thermogram for the decomposition of magnesium oxalate monohydrate.<\/li>\r\n<\/ul>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0<img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image11-2.png\" width=\"438.582677165354px\" height=\"232px\" alt=\"image\" \/><\/p>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-26.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2G: <\/strong>Observe the image given below for the decomposition of ammonium nitrate and complete the activity.<\/p>\r\n\r\n<ul>\r\n \t<li class=\"import-Normal\">Identify the volatile product\/s and the residue remaining in the crucible at each stage of decomposition.<\/li>\r\n \t<li class=\"import-Normal\">Write the decomposition reaction at each stage.<\/li>\r\n \t<li class=\"import-Normal\">Draw a thermogram for the decomposition of ammonium nitrate<\/li>\r\n \t<li class=\"import-Normal\">Compare the thermogram with calcium carbonate thermogram for post decomposition pattern. Can you suggest why the thermogram shows zero mass after decomposition for ammonium nitrate?<\/li>\r\n<\/ul>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0<img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image12-2.png\" width=\"396.055223097113px\" height=\"163.022782152231px\" alt=\"image\" \/><\/p>\r\n<p class=\"import-Normal\"><strong>2.7 Applications of Thermogravimetric analysis<\/strong><\/p>\r\n<p class=\"import-Normal\"><strong>I. Thermogravimetric analysis of a binary mixture of calcium and magnesium oxalates:<\/strong><\/p>\r\n<p class=\"import-Normal\">Following thermogram shows the decomposition curve for a mixture of oxalates.<\/p>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 <img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image13-2.png\" width=\"298.266666666667px\" height=\"316.2px\" alt=\"image\" \/><\/p>\r\n<p class=\"import-Normal\"><strong>Figure 2.7a<\/strong>. Decomposition curve for a mixture of calcium and magnesium oxalate dihydrate.<\/p>\r\n\r\n<ul>\r\n \t<li class=\"import-Normal\">There is a significant loss which occurs before 210\u00b0C- due to loss of water from the sample.<\/li>\r\n \t<li class=\"import-Normal\">The mixture of anhydrous carbonate then shows some weight loss by about 480 \u00b0C owing to the reaction given below.<\/li>\r\n<\/ul>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0MgCO<sub>3<\/sub><sub>(s)<\/sub> \u2192 MgO <sub>(s)<\/sub> + CO<sub>2 <\/sub><sub>(g)<\/sub><\/p>\r\n\r\n<ul>\r\n \t<li class=\"import-Normal\">No further weight loss occurs before 600 \u00b0C. (EF)<\/li>\r\n \t<li class=\"import-Normal\">CaCO<sub>3 <\/sub>decomposes between about 600 \u00b0C and 900 \u00b0C. (FG)<\/li>\r\n<\/ul>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">CaCO<sub>3<\/sub> <sub>(s)<\/sub> \u2192 CaO <sub>(s)<\/sub> + CO<sub>2 <\/sub><sub>(g)<\/sub><\/p>\r\n\r\n<ul>\r\n \t<li class=\"import-Normal\">Thus, EF represents a mixture of MgO and CaCO<sub>3<\/sub><\/li>\r\n \t<li class=\"import-Normal\">The plateau GH represents the residue of MgO and CaO<\/li>\r\n<\/ul>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-27.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2H: <\/strong>Will you be able to construct separate decomposition curves for calcium oxalate dihydrate and magnesium oxalate dihydrate based on the above application.<\/p>\r\n<p class=\"import-Normal\"><strong>II. Thermogravimetric analysis of plaster for safety screening:<\/strong><\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 40.5pt\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image14-1.jpg\" width=\"556\" height=\"237\" alt=\"image\" class=\"\" \/><\/p>\r\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-indent: 36pt\"><strong>Figure 2.7b.<\/strong> TG curve for plaster<\/p>\r\n<p class=\"import-Normal\">Plaster contains following ingredients,<\/p>\r\n<p class=\"import-Normal\" style=\"text-indent: 36pt\">Gypsum--- CaSO<sub>4<\/sub>.2H<sub>2<\/sub>O<\/p>\r\n<p class=\"import-Normal\" style=\"text-indent: 36pt\">Lime--- Ca(OH)<sub>2<\/sub><\/p>\r\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0Chalk--- CaCO<sub>3<\/sub><\/p>\r\n<p class=\"import-Normal\" style=\"text-align: justify\">From the weight loss at each step on the curve, the quantity of each ingredient can be determined in the original sample. In the manufacture of Portland cement, 5% gypsum is added to reduce the rate of setting. The gypsum is added to the fused clinker during processing, and the two components are subsequently milled to obtain uniform mixing and the required particle size. During milling, the thermal energy generated may cause partial dehydration of gypsum to hemihydrate CaSO<sub>4<\/sub><span style=\"font-size: 12pt;color: #;text-decoration: none\">1\/2.<\/span>H<sub>2<\/sub>O which adversely affects (increases) the rate of setting of the cement. Hence it is important to monitor the presence of each hydrate in the final cement. In order to provide quantitation at the required levels, this problem can be solved by TGA and DTA\/DSC.<\/p>\r\n<p class=\"import-Normal\" style=\"text-align: justify\">The dehydration of gypsum occurs as a two-stage endothermic process.<\/p>\r\n<p class=\"import-Normal\" style=\"text-align: justify\">CaSO<sub>4<\/sub>.2H<sub>2<\/sub>O\u00a0 <span style=\"font-size: 12pt;color: #;text-decoration: none\">\u2192 <\/span>CaSO<sub>4<\/sub><span style=\"font-size: 12pt;color: #;text-decoration: none\">1\/2. <\/span>H<sub>2<\/sub>O <span style=\"font-size: 12pt;color: #;text-decoration: none\">\u2192 <\/span>CaSO<sub>4<\/sub><\/p>\r\n<p class=\"import-Normal\" style=\"text-align: justify\">So, if there is conversion of gypsum to hemihydrate, the TG curve in Fig. 2.7b will show two step decomposition for gypsum instead of one.<\/p>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-28.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2I: <\/strong>(<span style=\"color: #ff6600\">James &amp; Tonge, 2008)<\/span><\/p>\r\n<p class=\"import-Normal\">A manufacturer wishes to incorporate a plastic coating on the inside of a utensil. One factor to be evaluated is the stability of the following polymer.<\/p>\r\n<p class=\"import-Normal\">a. Polyethylene<\/p>\r\n<p class=\"import-Normal\">b. Polypropylene<\/p>\r\n<p class=\"import-Normal\">c. PVC<\/p>\r\n<p class=\"import-Normal\">d. Polytetrafluoroethylene<\/p>\r\n<p class=\"import-Normal\">Figure below gives TG curves for the above polymers.<\/p>\r\n\r\n<\/div>\r\n<img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image15-4.png\" width=\"289\" height=\"239\" alt=\"image\" class=\"\" \/>\r\n<div class=\"2.-thermogravimetry\">\r\n<ol>\r\n \t<li class=\"import-Normal\">Which polymer is the least stable?<\/li>\r\n \t<li class=\"import-Normal\">Which polymer decomposes at the slowest rate?<\/li>\r\n \t<li class=\"import-Normal\">Which polymer shows no decomposition below 450<sup>o<\/sup>C ?<\/li>\r\n \t<li class=\"import-Normal\">Which polymer gives rise to more than one type of thermal decomposition?<\/li>\r\n<\/ol>\r\n<p class=\"import-Normal\">So far, we have discussed qualitative applications of TGA. Let us see some quantitative applications of thermogravimetric measurement.<\/p>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-29.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2J: Numerical Problems <\/strong><\/p>\r\n<p class=\"import-Normal\" style=\"text-align: justify\">1) Calculate the percent weight changes W% for each of the following reactions which occur on heating the parent material. Can you predict the nature of TG curve in each case?<\/p>\r\n<p class=\"import-Normal\">a) Ca(OH)<sub>2(s)<\/sub> \u2192CaO <sub>(S) <\/sub> +H<sub>2<\/sub>O<sub>(g)<\/sub><\/p>\r\n<p class=\"import-Normal\">b) 6PbO<sub>(s)<\/sub> + O<sub>2(g)<\/sub> \u2192 2Pb<sub>3<\/sub>O<sub>4(S)<\/sub><\/p>\r\n<p class=\"import-Normal\">[Ca=40.1, H=1.0, O=16.0, Pb=207.2]<\/p>\r\n<p class=\"import-Normal\" style=\"text-align: justify\">2) A mixture of calcium oxide and calcium carbonate is analysed by thermogravimetry. The resultant curve indicates one decomposition only between 600-900<sup>0 <\/sup>C during which the weight of the sample decreases from 250.6 mg to 190.8 mg. What is the percentage of calcium carbonate in a mixture by weight?<\/p>\r\n<p class=\"import-Normal\">[Atomic mass: H=1.0, Pb=207.2, C=12.0, O=16.0, Ca= 40.1]<\/p>\r\n<p class=\"import-Normal\" style=\"text-align: justify\">3) The thermogram given below shows the mass of a sample of calcium oxalate monohydrate, CaC<sub>2<\/sub>O<sub>4<\/sub>.H<sub>2<\/sub>O, as a function of temperature. The original sample of 17.61 mg was heated from room temperature to 1000<sup>o<\/sup>C at a rate of 20<sup>o<\/sup>C per minute. For each step in the thermogram.<\/p>\r\n<p class=\"import-Normal\" style=\"text-align: justify;text-indent: 36pt\">i. Identify the volatilization product and the solid residue that remains.<\/p>\r\n<p class=\"import-Normal\" style=\"text-align: justify;text-indent: 36pt\">ii. Calculate the % weight loss at each step.<\/p>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image16-2.png\" width=\"419.513910761155px\" height=\"278.904461942257px\" alt=\"image\" \/><\/p>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-30.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2K: Puzzle <\/strong><\/p>\r\n<p class=\"import-Normal\"><img src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image2-15.png\" width=\"38px\" height=\"28.6666666666667px\" alt=\"image\" \/><a class=\"rId30\" href=\"https:\/\/thewordsearch.com\/puzzle\/6923734\/thermal-analysis\/\">https:\/\/thewordsearch.com\/puzzle\/6923734\/thermal-analysis\/<\/a><\/p>\r\n<p class=\"import-Normal\"><\/p>\r\n\r\n<\/div>","rendered":"<div>\n<div class=\"textbox textbox--learning-objectives\">\n<header class=\"textbox__header\">\n<p class=\"textbox__title\"><strong><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image1-7.png\" width=\"34.6666666666667px\" height=\"34.6666666666667px\" alt=\"image\" \/>Learning Objectives<\/strong><\/p>\n<\/header>\n<div class=\"textbox__content\">\n<p>After completing this section, you should be able to:<\/p>\n<ul>\n<li class=\"import-Normal\" style=\"text-align: justify\">Describe the effect of heat on materials.<\/li>\n<li class=\"import-Normal\" style=\"text-align: justify\">Identify physical and chemical transitions.<\/li>\n<li class=\"import-Normal\" style=\"text-align: justify\">Describe the essential features of a thermobalance.<\/li>\n<li class=\"import-Normal\" style=\"text-align: justify\">Draw and interpret thermogravimetric and derivative thermogravimetric curve for a known system.<\/li>\n<li class=\"import-Normal\" style=\"text-align: justify\">Illustrate the range of applications of thermogravimetry.<\/li>\n<li class=\"import-Normal\" style=\"text-align: justify\">Calculate % weight loss at every stage of decomposition and predict stoichiometry.<\/li>\n<\/ul>\n<\/div>\n<\/div>\n<\/div>\n<div class=\"2.-thermogravimetry\">\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-align: justify\">Thermogravimetry is a technique used to detect any physical or chemical transitions which are accompanied by a weight loss or weight gain as the sample is heated in a controlled manner.<\/p>\n<p><strong>2.1 Effect of heat on matter:<\/strong><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">We need to first understand the effects of heat on matter. And For further explanation please see Introductory Chemistry in <em>Libretexts<\/em><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image2-11.png\" width=\"38px\" height=\"28.6666666666667px\" alt=\"image\" \/><a class=\"rId9\" href=\"https:\/\/chem.libretexts.org\/Bookshelves\/Introductory_Chemistry\/Introduction_to_General_Chemistry_(Malik)\/01%3A_Matter_energy_and_their_measurements\/1.09%3A_Heat_and_changes_in_physical_states_of_matter\">https:\/\/chem.libretexts.org\/Bookshelves\/Introductory_Chemistry\/Introduction_to_General_Chemistry_(Malik)\/01%3A_Matter_energy_and_their_measurements\/1.09%3A_Heat_and_changes_in_physical_states_of_matter<\/a><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-align: justify\">Now, we have understood the effects of heat on matter and also able to identify the processes involving change in weight on heating through Activity 1D. It is important to keep in mind that the change in weight could be due to physical or chemical transitions. To be able to distinguish between physical and chemical transition, let us go through the next sub-topic.<\/p>\n<p><strong>2.2 Changes in matter: Physical and Chemical Changes<\/strong><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">For further explanation please see Introductory Chemistry in <em>Libretexts<\/em><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image2-12.png\" width=\"38px\" height=\"28.6666666666667px\" alt=\"image\" \/><a class=\"rId10\" href=\"https:\/\/chem.libretexts.org\/Bookshelves\/Introductory_Chemistry\/Introductory_Chemistry\/03%3A_Matter_and_Energy\/3.06%3A_Changes_in_Matter_-_Physical_and_Chemical_Changes\">https:\/\/chem.libretexts.org\/Bookshelves\/Introductory_Chemistry\/Introductory_Chemistry\/03%3A_Matter_and_Energy\/3.06%3A_Changes_in_Matter_-_Physical_and_Chemical_Changes#:~:text=3.6%3A%20Changes%20in%20Matter%20%20Physical%20and%20Chemical,4%20Summary%20&#8230;%205%20Contributions%20%26%20Attributions%20<\/a><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><strong><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-20.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/>Activity 2A:<\/strong> Can you assign which of these transitions will be physical or chemical transitions? ( <strong>please indicate by writing &#8216;Y&#8217; in appropriate column<\/strong>)<\/p>\n<table style=\"width: 493px;height: 310px\">\n<tbody>\n<tr class=\"a-R\" style=\"height: 16.7pt\">\n<td class=\"a-C\" style=\"background-color: #5b9bd5;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\n<p class=\"import-Normal\"><strong>Phenomenon<\/strong><\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #5b9bd5;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\n<p class=\"import-Normal\"><strong>Physical<\/strong><\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #5b9bd5;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\n<p class=\"import-Normal\"><strong>Chemical <\/strong><\/p>\n<\/td>\n<\/tr>\n<tr class=\"a-R\" style=\"height: 16.7pt\">\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\n<p class=\"import-Normal\">Adsorption<\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<\/tr>\n<tr class=\"a-R\" style=\"height: 19.05pt\">\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\n<p class=\"import-Normal\">Dehydration<\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<\/tr>\n<tr class=\"a-R\" style=\"height: 19.05pt\">\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\n<p class=\"import-Normal\">Desorption<\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<\/tr>\n<tr class=\"a-R\" style=\"height: 16.7pt\">\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\n<p class=\"import-Normal\">Fusion (melting)<\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<\/tr>\n<tr class=\"a-R\" style=\"height: 16.7pt\">\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\n<p class=\"import-Normal\">Chemisorption<\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<\/tr>\n<tr class=\"a-R\" style=\"height: 16.7pt\">\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\n<p class=\"import-Normal\">Vaporization<\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<td class=\"a-C\" style=\"background-color: #eaeff7;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<\/tr>\n<tr class=\"a-R\" style=\"height: 16.7pt\">\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\n<p class=\"import-Normal\">Decomposition<\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<\/tr>\n<tr class=\"a-R\" style=\"height: 16.7pt\">\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\n<p class=\"import-Normal\">Redox reactions<\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<\/tr>\n<tr class=\"a-R\" style=\"height: 16.7pt\">\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 230.365px;height: 30px\">\n<p class=\"import-Normal\">Reduction in gaseous atmosphere<\/p>\n<\/td>\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 94.4688px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<td class=\"a-C\" style=\"background-color: #d2deef;padding: 3.6pt 7.2pt;border: 1pt solid #000000;width: 105.271px;height: 30px\">\n<p class=\"import-Normal\">\n<\/td>\n<\/tr>\n<tr style=\"height: 10px\">\n<td style=\"width: 237.594px;height: 10px\"><\/td>\n<td style=\"width: 102.031px;height: 10px\"><\/td>\n<td style=\"width: 112.5px;height: 10px\"><\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<p class=\"import-Normal\">\u00a0 \u00a0 (<span style=\"color: #ff6600\">Dodd &amp; Tonge, 2008<\/span>)<\/p>\n<p class=\"import-Normal\"><strong>2.3 Principle and Instrumentation of TGA:<\/strong><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">The instrument used to carry out thermogravimetric analysis is known as \u201cthermobalance\u201d.<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image4-2.jpg\" width=\"470.798530183727px\" height=\"223.037270341207px\" alt=\"image\" \/><\/p>\n<p class=\"import-Normal\" style=\"text-indent: 36pt\"><strong>Figure 2.3<\/strong> Block diagram of a thermobalance<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-indent: 36pt\">(Source: <a class=\"rId13\" href=\"https:\/\/images.app.goo.gl\/uyRxxbkVNkxLF3nT7\">https:\/\/images.app.goo.gl\/uyRxxbkVNkxLF3nT7<\/a>)<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><strong>Working:<\/strong> Please go through the <em>Chemlibre<\/em> link to understand the principle and working of a thermobalance.<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image2-13.png\" width=\"38px\" height=\"28.6666666666667px\" alt=\"image\" \/><a class=\"rId14\" href=\"https:\/\/chem.libretexts.org\/Bookshelves\/Analytical_Chemistry\/Instrumental_Analysis_(LibreTexts)\/31%3A_Thermal_Methods\/31.01%3A_Thermogravimetric_Methods\">https:\/\/chem.libretexts.org\/Bookshelves\/Analytical_Chemistry\/Instrumental_Analysis_(LibreTexts)\/31%3A_Thermal_Methods\/31.01%3A_Thermogravimetric_Methods<\/a><\/p>\n<p><strong>2.4 Interpretation of thermogravimetric curve:<\/strong><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-align: justify\">The graphical information obtained from thermogravimetric analysis is known as thermogram\/pyrolysis curve. The TG curve is a plot of weight (W) decreasing downwards on the y-axis (ordinate), and temperature (T) increasing to the right on the x-axis (abscissa). A typical thermogram for a single step decomposition is shown in Fig. 2.4.<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-align: justify\">The plateau \u2018AB\u2019 indicates no change in weight or the temperature range over which the sample is thermally stable. At point \u2018B\u2019 the sample starts decomposing which is indicated by an inflexion.<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-align: justify\">Please read the following text explaining the interpretation of thermogram and then attempt Activity 2B.<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image2-14.png\" width=\"38px\" height=\"28.6666666666667px\" alt=\"image\" \/><a class=\"rId15\" href=\"https:\/\/chem.libretexts.org\/Courses\/Franklin_and_Marshall_College\/Introduction_to_Materials_Characterization__CHM_412_Collaborative_Text\/Thermal_Analysis\/Thermogravimetric_analysis_(TGA)\">https:\/\/chem.libretexts.org\/Courses\/Franklin_and_Marshall_College\/Introduction_to_Materials_Characterization__CHM_412_Collaborative_Text\/Thermal_Analysis\/Thermogravimetric_analysis_(TGA)<\/a><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-21.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/> <strong>Activity 2B: <\/strong>A typical thermogram is shown below, observe and fill in the\u00a0 blanks by choosing the most appropriate answer. (Hint: Initial mass at \u2018A\u2019 is considered as 100%)<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-indent: 36pt\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image5-5.png\" width=\"300px\" height=\"214.112965879265px\" alt=\"image\" \/><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><strong>Figure 2.4<\/strong> Typical TG curve<\/p>\n<ol>\n<li class=\"import-Normal\">The part of the TG curve where the mass is essentially constant______________<\/li>\n<li class=\"import-Normal\">The temperature at which cumulative mass change reaches a magnitude that the thermobalance can detect ________________<\/li>\n<li class=\"import-Normal\">The temperature at which the cumulative mass change reaches a maximum_______________<\/li>\n<\/ol>\n<p class=\"import-Normal\" style=\"text-indent: 36pt\"><strong>Choose from the following options.<\/strong><\/p>\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 i. the initial temperature (B)<\/p>\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 ii. the record of weight from temperature B to C<\/p>\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 iii. the final temperature C<\/p>\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 iv. the plateau (AB)<\/p>\n<p class=\"import-Normal\">(<span style=\"color: #ff6600\">Dodd &amp; Tonge, 2008<\/span>)<\/p>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-22.png\" width=\"31.3333333333333px\" height=\"32.6666666666667px\" alt=\"image\" class=\"\" \/><strong> Activity 2C: <\/strong>For the processes given in the table, predict the nature of thermogram (Type- X\/Type-Y\/None of theses)<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image6-4.png\" width=\"298\" height=\"308\" alt=\"image\" class=\"\" \/><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image7-2.png\" width=\"197.103727034121px\" height=\"329.2px\" alt=\"image\" \/><\/p>\n<p><strong style=\"font-size: 1em\">2.5 Need for Derivative Thermogravimetry (DTG):<\/strong><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">In the above example (Fig.2.4a.), we have considered the thermogravimetric curve which represents a single stage decomposition.<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">Figures \u20182.5a\u2019 and \u20182.5b\u2019 show two-step and three-step decompositions respectively. In both these figures there is an overlay of TGA and DTG thermogram, clearly depicting advantages of DTG over TGA thermogram in locating the exact decomposition temperature.<\/p>\n<p class=\"import-Normal\" style=\"margin-left: 72pt;text-indent: 36pt\"><strong><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image8-3.png\" width=\"391.713910761155px\" height=\"184.335958005249px\" alt=\"image\" \/><\/strong><\/p>\n<p class=\"import-Normal\"><strong>Figure 2.5a. <\/strong>Thermogravimetric (TG) and Derivative thermogravimetry (DTG)<\/p>\n<p class=\"import-Normal\">curves for PVP at a heating rate of 10\u00b0C\/min. (<span style=\"color: #ff6600\">Source: Al-Hada et al., 2014<\/span>)<\/p>\n<p class=\"import-Normal\"><a class=\"rId20\" href=\"https:\/\/images.app.goo.gl\/fWChwNJi9uxfHZAJ7\">https:\/\/images.app.goo.gl\/fWChwNJi9uxfHZAJ7<\/a><\/p>\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0<img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image9-2.png\" width=\"495.402939632546px\" height=\"223.379317585302px\" alt=\"image\" class=\"\" \/><\/p>\n<p class=\"import-Normal\" style=\"text-indent: 36pt\"><strong>Figure 2.5b. <\/strong>TGA test result of calcium oxalate <span style=\"text-align: initial;text-indent: 36pt;font-size: 1em\">monohydrate (<\/span><span style=\"color: #ff6600\">Source: Chegg.com<\/span><span style=\"text-align: initial;text-indent: 36pt;font-size: 1em\">) <\/span><a class=\"rId22\" href=\"https:\/\/images.app.goo.gl\/1Hbp2vSV2rBjeFc4A\" style=\"text-align: initial;text-indent: 36pt;font-size: 1em\">https:\/\/images.app.goo.gl\/1Hbp2vSV2rBjeFc4A<\/a><\/p>\n<p class=\"import-Normal\" style=\"text-align: justify\">Figure \u20182.5b\u2019 is for the decomposition of calcium oxalate monohydrate, the weight loss commences just above 100 \u1d52C and continues up to 200 \u1d52C. Between about 400 \u1d52C and 500 \u1d52C further decomposition occurs, to give a product which is stable up to 700 \u1d52C before decomposing to give another stable compound at 800\u1d52C. Every process of decomposition continues over a range of temperature hence the DTG curve is useful in providing information regarding precise decomposition temperature at every stage.<\/p>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-23.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2D:<\/strong> ( <span style=\"color: #ff6600\">James &amp; Tonge, 2008<\/span>)<\/p>\n<p class=\"import-Normal\" style=\"text-indent: 18pt\">Indicate by circling either T for true or F for false,<\/p>\n<ol>\n<li class=\"import-Normal\">A derivative thermogravimetric (DTG) curve represents a plot of mass of sample, as a function of temperature. T\/F<\/li>\n<li class=\"import-Normal\">A point of inflection on a thermogravimetric (TG) curve will correspond to a minimum on the DTG curve for a given chemical decomposition.T\/F<\/li>\n<li class=\"import-Normal\">A \u2018plateau\u2019 on a TG curve will not necessarily correspond to a zero ordinate value of the DTG curve.T\/F<\/li>\n<li class=\"import-Normal\">Thermal decompositions which overlap are often indicated more clearly by DTG curves than by the corresponding TG curves.T\/F<\/li>\n<\/ol>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-24.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2E: <\/strong>Complete the following reaction for the decomposition of calcium carbonate. Identify the volatile and stable compound\/s remaining in the crucible post decomposition and indicate these on the thermogram.<\/p>\n<p class=\"import-NormalWeb\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image10.jpeg\" width=\"496px\" height=\"187.333333333333px\" alt=\"image\" \/><\/p>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-25.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2F: <\/strong>Observe the image given below for the decomposition of magnesium oxalate monohydrate and complete the activity.<\/p>\n<ul>\n<li class=\"import-Normal\">Identify the volatile product and the residue remaining in the crucible at each stage of decomposition.<\/li>\n<li class=\"import-Normal\">Write the decomposition reaction taking place at each stage.<\/li>\n<li class=\"import-Normal\">Draw a thermogram for the decomposition of magnesium oxalate monohydrate.<\/li>\n<\/ul>\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0<img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image11-2.png\" width=\"438.582677165354px\" height=\"232px\" alt=\"image\" \/><\/p>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-26.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2G: <\/strong>Observe the image given below for the decomposition of ammonium nitrate and complete the activity.<\/p>\n<ul>\n<li class=\"import-Normal\">Identify the volatile product\/s and the residue remaining in the crucible at each stage of decomposition.<\/li>\n<li class=\"import-Normal\">Write the decomposition reaction at each stage.<\/li>\n<li class=\"import-Normal\">Draw a thermogram for the decomposition of ammonium nitrate<\/li>\n<li class=\"import-Normal\">Compare the thermogram with calcium carbonate thermogram for post decomposition pattern. Can you suggest why the thermogram shows zero mass after decomposition for ammonium nitrate?<\/li>\n<\/ul>\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0<img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image12-2.png\" width=\"396.055223097113px\" height=\"163.022782152231px\" alt=\"image\" \/><\/p>\n<p class=\"import-Normal\"><strong>2.7 Applications of Thermogravimetric analysis<\/strong><\/p>\n<p class=\"import-Normal\"><strong>I. Thermogravimetric analysis of a binary mixture of calcium and magnesium oxalates:<\/strong><\/p>\n<p class=\"import-Normal\">Following thermogram shows the decomposition curve for a mixture of oxalates.<\/p>\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 <img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image13-2.png\" width=\"298.266666666667px\" height=\"316.2px\" alt=\"image\" \/><\/p>\n<p class=\"import-Normal\"><strong>Figure 2.7a<\/strong>. Decomposition curve for a mixture of calcium and magnesium oxalate dihydrate.<\/p>\n<ul>\n<li class=\"import-Normal\">There is a significant loss which occurs before 210\u00b0C- due to loss of water from the sample.<\/li>\n<li class=\"import-Normal\">The mixture of anhydrous carbonate then shows some weight loss by about 480 \u00b0C owing to the reaction given below.<\/li>\n<\/ul>\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0MgCO<sub>3<\/sub><sub>(s)<\/sub> \u2192 MgO <sub>(s)<\/sub> + CO<sub>2 <\/sub><sub>(g)<\/sub><\/p>\n<ul>\n<li class=\"import-Normal\">No further weight loss occurs before 600 \u00b0C. (EF)<\/li>\n<li class=\"import-Normal\">CaCO<sub>3 <\/sub>decomposes between about 600 \u00b0C and 900 \u00b0C. (FG)<\/li>\n<\/ul>\n<p class=\"import-Normal\" style=\"margin-left: 36pt\">CaCO<sub>3<\/sub> <sub>(s)<\/sub> \u2192 CaO <sub>(s)<\/sub> + CO<sub>2 <\/sub><sub>(g)<\/sub><\/p>\n<ul>\n<li class=\"import-Normal\">Thus, EF represents a mixture of MgO and CaCO<sub>3<\/sub><\/li>\n<li class=\"import-Normal\">The plateau GH represents the residue of MgO and CaO<\/li>\n<\/ul>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-27.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2H: <\/strong>Will you be able to construct separate decomposition curves for calcium oxalate dihydrate and magnesium oxalate dihydrate based on the above application.<\/p>\n<p class=\"import-Normal\"><strong>II. Thermogravimetric analysis of plaster for safety screening:<\/strong><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 40.5pt\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image14-1.jpg\" width=\"556\" height=\"237\" alt=\"image\" class=\"\" \/><\/p>\n<p class=\"import-Normal\" style=\"margin-left: 36pt;text-indent: 36pt\"><strong>Figure 2.7b.<\/strong> TG curve for plaster<\/p>\n<p class=\"import-Normal\">Plaster contains following ingredients,<\/p>\n<p class=\"import-Normal\" style=\"text-indent: 36pt\">Gypsum&#8212; CaSO<sub>4<\/sub>.2H<sub>2<\/sub>O<\/p>\n<p class=\"import-Normal\" style=\"text-indent: 36pt\">Lime&#8212; Ca(OH)<sub>2<\/sub><\/p>\n<p class=\"import-Normal\">\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0Chalk&#8212; CaCO<sub>3<\/sub><\/p>\n<p class=\"import-Normal\" style=\"text-align: justify\">From the weight loss at each step on the curve, the quantity of each ingredient can be determined in the original sample. In the manufacture of Portland cement, 5% gypsum is added to reduce the rate of setting. The gypsum is added to the fused clinker during processing, and the two components are subsequently milled to obtain uniform mixing and the required particle size. During milling, the thermal energy generated may cause partial dehydration of gypsum to hemihydrate CaSO<sub>4<\/sub><span style=\"font-size: 12pt;color: #;text-decoration: none\">1\/2.<\/span>H<sub>2<\/sub>O which adversely affects (increases) the rate of setting of the cement. Hence it is important to monitor the presence of each hydrate in the final cement. In order to provide quantitation at the required levels, this problem can be solved by TGA and DTA\/DSC.<\/p>\n<p class=\"import-Normal\" style=\"text-align: justify\">The dehydration of gypsum occurs as a two-stage endothermic process.<\/p>\n<p class=\"import-Normal\" style=\"text-align: justify\">CaSO<sub>4<\/sub>.2H<sub>2<\/sub>O\u00a0 <span style=\"font-size: 12pt;color: #;text-decoration: none\">\u2192 <\/span>CaSO<sub>4<\/sub><span style=\"font-size: 12pt;color: #;text-decoration: none\">1\/2. <\/span>H<sub>2<\/sub>O <span style=\"font-size: 12pt;color: #;text-decoration: none\">\u2192 <\/span>CaSO<sub>4<\/sub><\/p>\n<p class=\"import-Normal\" style=\"text-align: justify\">So, if there is conversion of gypsum to hemihydrate, the TG curve in Fig. 2.7b will show two step decomposition for gypsum instead of one.<\/p>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-28.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2I: <\/strong>(<span style=\"color: #ff6600\">James &amp; Tonge, 2008)<\/span><\/p>\n<p class=\"import-Normal\">A manufacturer wishes to incorporate a plastic coating on the inside of a utensil. One factor to be evaluated is the stability of the following polymer.<\/p>\n<p class=\"import-Normal\">a. Polyethylene<\/p>\n<p class=\"import-Normal\">b. Polypropylene<\/p>\n<p class=\"import-Normal\">c. PVC<\/p>\n<p class=\"import-Normal\">d. Polytetrafluoroethylene<\/p>\n<p class=\"import-Normal\">Figure below gives TG curves for the above polymers.<\/p>\n<\/div>\n<p><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image15-4.png\" width=\"289\" height=\"239\" alt=\"image\" class=\"\" \/><\/p>\n<div class=\"2.-thermogravimetry\">\n<ol>\n<li class=\"import-Normal\">Which polymer is the least stable?<\/li>\n<li class=\"import-Normal\">Which polymer decomposes at the slowest rate?<\/li>\n<li class=\"import-Normal\">Which polymer shows no decomposition below 450<sup>o<\/sup>C ?<\/li>\n<li class=\"import-Normal\">Which polymer gives rise to more than one type of thermal decomposition?<\/li>\n<\/ol>\n<p class=\"import-Normal\">So far, we have discussed qualitative applications of TGA. Let us see some quantitative applications of thermogravimetric measurement.<\/p>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-29.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2J: Numerical Problems <\/strong><\/p>\n<p class=\"import-Normal\" style=\"text-align: justify\">1) Calculate the percent weight changes W% for each of the following reactions which occur on heating the parent material. Can you predict the nature of TG curve in each case?<\/p>\n<p class=\"import-Normal\">a) Ca(OH)<sub>2(s)<\/sub> \u2192CaO <sub>(S) <\/sub> +H<sub>2<\/sub>O<sub>(g)<\/sub><\/p>\n<p class=\"import-Normal\">b) 6PbO<sub>(s)<\/sub> + O<sub>2(g)<\/sub> \u2192 2Pb<sub>3<\/sub>O<sub>4(S)<\/sub><\/p>\n<p class=\"import-Normal\">[Ca=40.1, H=1.0, O=16.0, Pb=207.2]<\/p>\n<p class=\"import-Normal\" style=\"text-align: justify\">2) A mixture of calcium oxide and calcium carbonate is analysed by thermogravimetry. The resultant curve indicates one decomposition only between 600-900<sup>0 <\/sup>C during which the weight of the sample decreases from 250.6 mg to 190.8 mg. What is the percentage of calcium carbonate in a mixture by weight?<\/p>\n<p class=\"import-Normal\">[Atomic mass: H=1.0, Pb=207.2, C=12.0, O=16.0, Ca= 40.1]<\/p>\n<p class=\"import-Normal\" style=\"text-align: justify\">3) The thermogram given below shows the mass of a sample of calcium oxalate monohydrate, CaC<sub>2<\/sub>O<sub>4<\/sub>.H<sub>2<\/sub>O, as a function of temperature. The original sample of 17.61 mg was heated from room temperature to 1000<sup>o<\/sup>C at a rate of 20<sup>o<\/sup>C per minute. For each step in the thermogram.<\/p>\n<p class=\"import-Normal\" style=\"text-align: justify;text-indent: 36pt\">i. Identify the volatilization product and the solid residue that remains.<\/p>\n<p class=\"import-Normal\" style=\"text-align: justify;text-indent: 36pt\">ii. Calculate the % weight loss at each step.<\/p>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image16-2.png\" width=\"419.513910761155px\" height=\"278.904461942257px\" alt=\"image\" \/><\/p>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image3-30.png\" width=\"32.6666666666667px\" height=\"32.6666666666667px\" alt=\"image\" \/><strong>Activity 2K: Puzzle <\/strong><\/p>\n<p class=\"import-Normal\"><img decoding=\"async\" src=\"http:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-content\/uploads\/sites\/37\/2024\/05\/image2-15.png\" width=\"38px\" height=\"28.6666666666667px\" alt=\"image\" \/><a class=\"rId30\" href=\"https:\/\/thewordsearch.com\/puzzle\/6923734\/thermal-analysis\/\">https:\/\/thewordsearch.com\/puzzle\/6923734\/thermal-analysis\/<\/a><\/p>\n<p class=\"import-Normal\">\n<\/div>\n","protected":false},"author":16,"menu_order":2,"template":"","meta":{"om_disable_all_campaigns":false,"_monsterinsights_skip_tracking":false,"_monsterinsights_sitenote_active":false,"_monsterinsights_sitenote_note":"","_monsterinsights_sitenote_category":0,"_uf_show_specific_survey":0,"_uf_disable_surveys":false,"pb_show_title":"on","pb_short_title":"","pb_subtitle":"","pb_authors":[],"pb_section_license":""},"chapter-type":[],"contributor":[],"license":[],"class_list":["post-252","chapter","type-chapter","status-publish","hentry"],"aioseo_notices":[],"part":3,"_links":{"self":[{"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/pressbooks\/v2\/chapters\/252","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/pressbooks\/v2\/chapters"}],"about":[{"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/wp\/v2\/types\/chapter"}],"author":[{"embeddable":true,"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/wp\/v2\/users\/16"}],"version-history":[{"count":19,"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/pressbooks\/v2\/chapters\/252\/revisions"}],"predecessor-version":[{"id":461,"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/pressbooks\/v2\/chapters\/252\/revisions\/461"}],"part":[{"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/pressbooks\/v2\/parts\/3"}],"metadata":[{"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/pressbooks\/v2\/chapters\/252\/metadata\/"}],"wp:attachment":[{"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/wp\/v2\/media?parent=252"}],"wp:term":[{"taxonomy":"chapter-type","embeddable":true,"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/pressbooks\/v2\/chapter-type?post=252"},{"taxonomy":"contributor","embeddable":true,"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/wp\/v2\/contributor?post=252"},{"taxonomy":"license","embeddable":true,"href":"https:\/\/pressbooks.justwrite.in\/thermalmethodsofanalysis\/wp-json\/wp\/v2\/license?post=252"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}