DCS Lab Report Name: Manab Kumar Jena Roll No: MIM20B036 Des: © The Differential Scanning Calorimetry (DSC) technique has garnered immense fluctuations that popularity in thermal analysis due to its ability to track the energy come when a material undergoes heating, cooling or isothermally held, as a function of temperature, In this report, we delve into the principles of operation, methodology and parameters that are extracted through DSC analysis. Principle: In a basic DSC experiment, energy is introduced simultancously into a sample cell(which contains solution with the molecule of interest) and a reference cell (containing only the solvent). Temperatures of both cells are raised identically over time. We require only 10 milligrams of the reference and the sample for analysis.Both solid and liquid samples can be analysed using DSC. We typically use powdered samples of both metals and nonmetals, A controlled atmosphere is maintained using Argon or Nitrogen gas to prevent contamination. The air is also compressed to reduce moisture content in the environment of the experiment. The calorimeter can go from room temperature to 1500 degree Celsius temperatures and we typically use platinum/alumina crucibles due to their stability and heat resistance. We calibrate the equipment prior to usage for zero error and improvement of accuracy. Typical materials used for calibration are: Indium, Tin, Bismuth, Zine, Aluminium, SilverGold and Nickel. Calibrations are done for measurements of temperature and sensitivity (to ensure uniform application of heat). The heating rate is usually between 5 to 20 degree Celsius per second. Components: Crueibles: Platinum (100 #1) is used for Gp measurements of minerals, organic samples, and polymers while Alumina (8o zl) is used for metallic samples Furnace: Used to heat the sample and reference materials at a controlled rate during the experiment‘© Thermocouple: Used to measure the temperature of the sample and reference sections ‘© Temperature Control Unit: Used to maintain a constant temperature different between the sample and reference materials * Heat Flux Sensor: Used to measure the heat flow between the sample and reference materials Procedure: ‘+ The sample is prepared according to the specific requirements of the experiment, Typically, the sample should be homogeneous and representative of the material being studied. ‘* The DSC instrument must be calibrated before use to ensure accurate and consistent measurements. Calibration involves using standard materials with well-defined thermal properties to establish a reference baselin ‘* The sample is loaded into the DSC instrument, which is typically in the form of a small sample pan or crucible, The sample should be placed carefully and securely in ‘the sample holder to ensure accurate measurements, ‘© The sample is subjected to a controlled temperature program, which involves heating or cooling the sample ata specific rate. The temperature program may vary depending on the specific experiment being performed. * Data Collection: During the heating or cooling process, the DSC instrument ‘measures the heat flow or heat capacity of the sample as a function of temperature This data is collected and recorded for further analysis. ‘The collected data is analysed to determine the thermal properties of the sample, such as the glass transition temperature, melting temperature, or enthalpy of fusion. ‘The data may be analysed using various software programs or mathematical models. Uses: ‘© Characterization of materials © Phase transition temperature * Analysis of chemical reactions © Quality control * Pharmaceutical research ‘* Food science ete. ‘* DSC measurements provide several important parameters, including: 1. Melting point and crystallisation temperature 2. Glass transition temperature 4. Enthalpy of transition