Departmental Research Facility (DRF)

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: The BET surface area is the total surface area (m2/g) per unit mass of material. The pore size distribution refers to the change of pore volume with the pore size of the material. Both are the most important physical properties of porous materials, especially nano-materials. There are many methods for determining BET surface area and pore size distribution. Nitrogen adsorption is the most commonly used and reliable method Brunauer-Emmett-Teller (BET) surface area analysis is the multi-point measurement of an analyte’s specific surface area (m2/g) through gas adsorption analysis, where an inert gas such as nitrogen is continuously flowed over a solid sample, or the solid sample is suspended in a defined gaseous volume. Small gas molecules adsorb to the solid substrate and its porous structures due to weak van der Waals forces, forming a monolayer of adsorbed gas. This monomolecular layer, and the rate of adsorption, can be used to calculate the specific surface area of a solid sample and its porous geometry, informing studies into the reactivity and bioavailability of pharmaceutical products.

The 3Flex high-performance gas adsorption analyzer is the most advanced instrument for measuring surface area, pore size, and pore volume of both powders and particulate materials.The 3Flex is ideally suited for gas or vapor adsorption analysis of microporous (< 2 nm) and mesoporous (2 to 50 nm) samples and a wide variety of porous and non-porous materials. Brunauer-Emmett-Teller (BET) surface area analysis is the multi-point measurement of an analyte’s specific surface area (m2/g) through gas adsorption analysis, where an inert gas such as nitrogen is continuously flowed over a solid sample, or the solid sample is suspended in a defined gaseous volume. Features: a)Surface area b)Mesopore c)Micropore d)Vapor sorption

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The AMI-300 Catalyst Characterization System is designed to aid the user to perform a host of automated analytical functions. These functions are separated into several groups some of which are made available to the user as options. The standard AMI-300 system performs Temperature Programmed Reduction (TPR), Temperature Programmed Oxidation (TPO), Temperature Programmed Desorption (TPD), Pulse Chemisorption. In addition Treatment and Pulse Calibration procedures are included for treatment and degassing of samples and calibration of results, respectively. The TPR/TPO procedure consists of three steps: • Start Conditions , Ramp&Hold , Postflush The TPD procedure consists of four steps, in addition to the adsorption step: • Flush • Initial Conditions • Ramp&Hold • Postflush In Pulse Chemisorption a series of premeasured pulses of an adsorbate are passed through the catalyst bed at regular intervals. The amount of gas that is not adsorbed by the catalyst is detected.

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The Differential Scanning Calorimetry (DSC) Analyzer is a core thermal analysis instrument used to measure how a material’s physical properties change with temperature. It operates by heating or cooling a sample and an inert reference pan at a controlled, identical rate. The instrument monitors the difference in heat flow required to maintain both pans at the exact same temperature. When the sample undergoes a physical transformation—such as melting, crystallization, or a glass transition—it will either absorb heat (endothermic) or release heat (exothermic). The DSC records these energy changes in real time, producing a thermal curve that serves as a unique fingerprint for the material. Primary Uses: • Polymer & Plastic Characterization: To find the glass transition temperature (T_g), melting point (T_m), and percentage of crystallinity. • Pharmaceutical Analysis: To check drug purity, detect different crystalline structures (polymorphs), and test shelf-life stability. • Chemical Reaction Monitoring: To study curing profiles, cross-linking in resins, and thermal decomposition limits.

FE-SEM is typically performed in a high vacuum because gas molecules tend to disturb the electron beam and the emitted secondary and backscattered electrons used for imaging. In addition to FE-SEM, energy-dispersive X-ray (EDX) was conducted on the same specimens for further analysis. EDX is an X-ray technique used to identify the elemental composition of materials. These systems are attachments to electron microscopy instruments where the imaging capability of the microscope identifies the specimens of interest

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Thermogravimetric Analysis-Mass Spectrometry (TGA-MS) Analyzer: Comprehensive Description 1. Overview: The Thermogravimetric Analysis-Mass Spectrometry (TGA-MS) Analyzer is an advanced hyphenated analytical instrument that combines Thermogravimetric Analysis (TGA) with Mass Spectrometry (MS) to study the thermal decomposition and evolved gas composition of materials. This system provides simultaneous measurement of weight loss (TGA) and gas-phase analysis (MS), offering valuable insights into material stability, decomposition mechanisms, and volatile byproducts. 2. Key Components: A TGA-MS system consists of two main modules: 2.1 Thermogravimetric Analyzer (TGA): - Measures changes in a sample’s mass as a function of temperature or time in a controlled atmosphere (inert, oxidizing, or reducing). - Key Features: - High-precision microbalance (±0.1 µg sensitivity). - Programmable temperature range (ambient to 1200°C). - Controlled gas flow (N₂, O₂, He, etc.). - Multiple heating rates (isothermal, dynamic, modulated). 2.2 Mass Spectrometer (MS): - Detects and identifies gaseous species evolved during thermal decomposition. - Common MS Types Used: - Quadrupole MS: Fast scanning, good sensitivity, moderate resolution. - Key Features: - Real-time monitoring of evolved gases (H₂O, CO₂, CO, hydrocarbons, etc.) - Detection limits in the ppm to ppb range. - Electron Ionization (EI) mode. 2.3 Interface Between TGA and MS: - A heated transfer line prevents gas condensation. - Capillary or jet separator for efficient gas transfer. - May include a gas dilution system for high-concentration samples. 3. Working Principle : 1. Sample Loading: A small sample (typically 5–15 mg) is placed in a ceramic crucible inside the TGA furnace. 2. Temperature Program: The sample is heated under controlled conditions (ramp, isotherm, etc.). 3. Mass Loss Measurement (TGA): The microbalance records weight changes as the sample decomposes. 4. Gas Evolution (MS): Volatilized gases are transferred to the MS via a heated transfer line. 5. Mass Spectral Analysis: The MS ionizes and detects gas molecules, providing mass-to-charge (m/z) ratios for identification. 4. Advantages of TGA-MS: ✔ Simultaneous Data: Combines weight loss and gas analysis in a single experiment. ✔ High Sensitivity: Detects trace-level evolved gases. ✔ Versatile: Works with solids and powders. ✔ Quantitative & Qualitative: Provides both mass loss curves and gas identification. 5. Limitations: ✖ Complex Data Interpretation: Requires expertise in both TGA and MS. ✖ Overlapping Peaks: Some gases may have similar m/z ratios. ✖ Sample Limitation: Don't Works with liquid samples and that are explosive or toxic samples.

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In materials research, the scientist has many analytical questions related to the chemical composition and crystalline constitution of materials. X-ray diffraction (XRD) is the only laboratory technique that non-destructively and accurately obtains information such as chemical composition, crystal structure, crystal orientation, crystallite size, lattice strain, preferred orientation and layer thickness. Materials researchers therefore use XRD to analyze a wide range of materials, from powders to solids, thin films and nanomaterials.

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