Infrared spectroscopy (IR or vibrational spectroscopy) is a powerful tool for material identification. It relies on the interaction of IR radiation with matter. When a material is irradiated with IR radiation, those chemical bonds with definite dipole moments start vibrating, and each vibration will give rise to characteristic peaks. FTIR spectrum will provide information on the functional groups present in the materials. As the fingerprint region of the FTIR spectrum is unique for every molecule, it can be used for the identification and purity analysis of materials.

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Nicolet iS50 is equipped with an elaborated database comprising more than 30,000 FTIR spectra of materials such as polymers, organic compounds, plasticizers, additives, common materials, organic solvents, hydrocarbons, and biomolecules. Thus, iS50 is a potential tool for material identification by spectral matching.

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FTIR spectroscopic analysis can be used for the identification of materials, especially polymers and organic materials. It can be used for establishing the equivalence of materials with materials already in practice, assessing the purity of materials used for device development, and also for the structural elucidation of unknown materials. It could also be used for monitoring the course of chemical reactions, ensuring the completion of the reactions, and consumption of reactants.

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UV-visible spectrophotometry is one of the most frequently used structural characterization techniques based on Beer-Lambert’s law. It works on the principle that compounds containing π-electrons or non-bonding electrons (n-electrons) can absorb the energy in the form of ultraviolet or visible light to excite these electrons to higher anti-bonding molecular orbitals. The wavelength of maximum absorption is inversely proportional to the energy gap between the HOMO and the LUMO of molecules. UV-Vis spectrophotometer can be used for the qualitative analysis (simple read and spectrum scan) as well as quantitative determination of UV/Vis active analytes such as organic compounds, biological macromolecules, and surface plasmon resonance (SPR) of active nanomaterials.

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UV-visible spectroscopic analysis can be used for the structural elucidation of materials. UV-visible spectra could be used to assess the electronic levels and optical band gap of the materials. Loading and release kinetics of drugs to/from drug delivery systems (DDS) could be monitored by this technique. Transmittance measurement would give the transparency range of optical devices like contact lenses. Reflectance measurement would give the UV reflecting capacity of coatings and paints. Peltier attachment would enable the equipment to study the temperature-dependent variation in the absorbance/transmittance of thermos-responsive material solutions. Color measurements would help to assess the variation in the color parameters of the material before and after treatment. The surface plasmon resonance (SPR) of nanomaterials could be analyzed using a UV-visible spectrometer. As SPR has a direct relation with the shape and size of nanomaterials, the technique could distinguish nanomaterials based on their aspect ratio. It could also be used for the detection of heavy metal ions from their solutions by colorimetric methods.

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Spectrofluorometry is an essential structural characterization technique. When compounds containing π-electrons or nonbonding electrons are excited with radiation with a wavelength corresponding to their absorption maximum, these electrons will migrate to high-energy anti-bonding molecular orbitals. An excited state is highly unstable; hence, the electrons will return to the ground state by emitting absorbed energy in the form of radiation. A spectrofluorometer measures the emitted radiation from an excited molecule and provides information about the compound's chemical structure. It can be used for qualitative analysis (simple read and spectrum scan) and quantitative estimation of emissive materials in solutions.

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Just like UV-visible spectrometer, a spectrofluorometer could also be used for the structural elucidation of materials. It could be used for studying the enhancement or quenching of emissions in the presence of certain molecules. The emission analysis could be used for detecting the presence of emissive molecules.

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High-performance liquid chromatography (HPLC) is an efficient technique for separating, identifying, and quantifying components in a mixture. It relies on pumps to pass a pressurized liquid solvent (mobile phase) containing the sample mixture through a column filled with a solid adsorbent material (stationary phase). Each component in the sample interacts slightly differently with the adsorbent material, causing different flow rates for the various constituents and separating them as they flow out of the column. UV and RI detectors are used for detecting the components. The time the components take to reach the detector is termed the retention time (TR). Different components in a mixture will have different TR values, based on which they can be identified. Calibration plots connecting the concentration of analytes vs. peak area can be used for their quantification.

Gel permeation chromatographic (GPC) analysis is a vital characterization tool for polymers and macromolecules. GPC separates polymeric molecules based on their size (size exclusion chromatography) when pumped through a column packed with beads composed of cross-linked polymers (styragel or ultrahydrogel). This method can be used for the qualitative purity assay of macromolecular solutions and the estimation of the relative molecular weight and polydispersity index (PDI) of polymers.

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HPLC can be used for the purity analysis of materials, detection, and quantification of specific components (analytes) in mixtures. The analyte matrix of HPLC encompasses a wide range of materials viz. small organic molecules, amino acids, drugs, enzymes, biomolecules, biomarkers, etc. It could be used for the extractable and leachable analysis of polymeric materials specifically for the estimation of residual content of monomers, plasticizers, and solvents. GPC can be used for the analysis of macromolecules of natural or synthetic origin. It would give an idea about their molecular weight distribution and polydispersity index.

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LC-2010A HT is a high throughput HPLC system capable of analyzing samples in bulk (up to 210). Analytes are detected using a UV-visible detector. This equipment is suitable for method development and quality control analyses.

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Gas chromatography (GC) is used to analyze compounds that can be vaporized without decomposition. GC can be employed to test the purity of volatile substances like organic solvents, separate the components of a mixture (the relative amounts of such components can also be determined), and quantify volatile residues from materials or devices. During GC analysis, the gaseous analytes interact with the column walls coated with a stationary phase and elute at different retention times (TR). Compounds can be identified and quantified by comparing the TR and peak area under specific conditions. Headspace GC analysis is used to analyze highly reactive/toxic chemicals such as pesticides, sterilizing agents, monomers, etc.

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GC-FID can be used for the detection and quantification of organic molecules especially hydrocarbons, solvents, etc. Ethylene Oxide (EtO) has been utilized as a sterilizing agent for biomedical devices owing to its convenient usage. However, the determination of residual EtO is a mandatory post-sterilization analysis due to its toxicity. ISO 10993-7 outlines the methods for estimating residual EtO in sterilized devices and the allowable limits. Headspace gas chromatographic analysis of the extracts of sterilized medical devices and biomaterials will give the idea of residual etO content. The residual content of solvents and monomers in polymeric medical devices could also be analyzed using HS-GC.

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Differential scanning calorimetry, or DSC, measures the heat flow from or to a sample as a function of temperature in comparison with a reference material maintained at an identical temperature. The instrument can monitor thermotropic events such as melting, crystallization, glass transition, curing, sorption, etc. In addition to the precise monitoring of thermal events, it could also deduce thermodynamic properties like enthalpy change and the heat capacity of the materials. Modulated Differential Scanning Calorimetry (mDSC) efficiently monitors even weak thermotropic changes like liquid crystalline phase transitions. The crystallinity, tacticity, and purity of the materials could also be analyzed.

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DSC is a robust technique to monitor the thermal transitions of materials such as melting, crystallization, glass transition, etc. In addition to the thermal transitions, the thermodynamic parameters associated with the transition (enthalpy of fusion, enthalpy of crystallization, etc.) could also be calculated using DSC. Other information that could be deduced from DSC analysis are heat capacity, crystallinity, tacticity, liquid crystalline phase transitions, denaturing of protein, etc.

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Thermogravimetric analysis determines the weight change of a material as a function of temperature. In differential thermal analysis, the temperature difference between a reactive sample and a non-reactive reference is determined as a function of time/temperature, providing helpful information about the temperatures, thermodynamics, and kinetics of reactions. In a combined DTA-TGA system, thermal and mass change effects are measured concurrently on the same sample (DTA, TG, DTG). Weight changes & enthalpy changes of materials corresponding to the transitions and reactions are monitored as a function of temperature (or time) under a controlled atmosphere. In addition to thermal stability, compositional analysis of the materials can also be performed with this equipment. It can differentiate endothermic and exothermic events, which are not associated with a weight change (e.g., melting and curing) from those involving weight changes (e.g., degradation). Filler content, char residue content, moisture content, etc. can also be determined using this instrument.

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TGA would help to understand the thermal stability of materials which is a necessary pre-requisite for any material to be used for device development. The technique can be used to estimate the percentage composition of constituents in polymer composites. Ash content, moisture content, and filler content of polymer-based materials could also be obtained by Thermogravimetric analysis.

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Texture analyzer is used for mechanical testing of tissues, food, cosmetics, pharmaceuticals, adhesives, and other consumer products in compression or tension mode. It assesses textural properties by capturing force, distance, and time data at nearly 500 points per second. Samples are either placed on the base of the texture analyzer or held between two suitable fixtures. In a simple test, the arm of the texture analyzer containing a load cell moves down to penetrate or compress the product and then returns to its initial position. It is capable of performing a wide array of tests.

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Textural analyzers can be used for mechanical testing (tensile, compression, and flexural) of small devices and biological samples that cannot be analyzed by conventional mechanical testing systems like UTM. In addition to mechanical testing of films/tissues (Compression and tension), the texture analyzer can perform fracturability, muco-adhesiveness, tear strength, burst resistance, peel strength, conformability, and burst strength of films, fabrics, wound dressings, and polymers. It is capable of performing the characterization of gel samples by gel strength (bloom strength for Gelatin), injectability, and syringeability of gels. It could also be used for studying the compression characteristics of devices like stents, vascular grafts, and intraocular lenses.

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The Raman Effect is based on the scattering of light when interacting with the chemical bonds of a compound. The interaction of photons with chemical bonds causes specific energy shifts in the backscattered light which could be analyzed to get the Raman spectrum of the compound. The Raman spectrum is unique for each chemical composition and can provide qualitative and quantitative information about the material. Confocal Raman microscopy is a high-resolution imaging technique widely used to characterize materials and specimens in terms of their chemical composition without any labeling. The following information can be obtained using this equipment: Determination of the chemical structure of molecules by Micro Raman spectroscopy, Confocal Raman imaging (hyperspectral image generation with details of complete Raman spectrum at pixel level), Chemical mapping of the distribution of components in a mixture by Raman imaging, depth profiling, drug in excipients/tablets, drug-eluting stent coatings, live-cell imaging, bacterial imaging, etc.

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Micro Raman spectroscopy can be used as a tool for material identification complementary to FTIR spectroscopy. The advantage of Raman over FTIR is that it can be used for the analysis of materials having moisture content. Hence this technique is suitable for the analysis of biomolecules, live cells, tissues, etc. It is suitable for the analysis of all kinds of materials encompassing polymers, organic molecules, inorganic materials, ceramics, metals, and alloys. Raman chemical mapping can be effectively used to distinguish materials of different chemical origins, cells with distinct features, adsorption or inclusion of certain chemical moieties on or in the cells, imaging bacterial colonies, etc. It can be used for analyzing forensic samples for detecting forgery, fingerprint analysis, gunpowder residue analysis, etc. It can be used in the pharmaceutical sector for analyzing the distribution of drugs in combinations, coating of drugs in combinatorial devices, drug emulsions, etc.

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By using a wide variety of light sources and optical filters, fluorescence and chemiluminescence of the samples, especially biological samples, can be quantified and imaged. It has a multipurpose CCD camera system for sensitive and quantitative imaging of membranes, gels, colony counting, etc.

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The luminescent image analyzer is suitable for the imaging of samples and small animals with suitable light sources covering IR, Visible light, and UV. It can also image samples of Agarose and polyacrylamide gels, Western blot imaging, thin layer chromatography plates, etc.

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Rapid Visco Analyzer is a viscometer with ramped temperature and variable shear capability optimized for testing the viscous properties of different types of samples. However, it is essential to highlight its versatility due to its capacity to analyze the viscosity in heating-cooling cycles. It can determine the solution viscosity and the viscous properties of biopolymers such as starch, alginate, chitosan, hydrocolloids, proteins, etc.

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This equipment is useful in estimating the solution viscosities of biopolymer solutions and their variation in response to temperature. In addition to viscosity, the equipment can be used for analyzing the pasting strength of starch.

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The Force tensiometer is used for the surface property analysis of liquids and solids. As the testing is carried out as force measurements, the dynamic changes of the surface properties can be analyzed accurately by this equipment. Its high sensitivity enables the accurate estimation of surface and interface properties. Apart from the surface and interfacial tensions, it could be used to estimate critical micelle concentration, the dynamic contact angle of the materials, powder wettability, and surface-free energy calculations.

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A force tensiometer is a package for the surface analysis of liquids and solids. It can be used for the analysis of surface tension/ interfacial tension of liquids, critical micelle concentration, and the dynamic contact angle of solids by Du Nouy Ring and Wilhelmy methods. It could be used for the powder wettability analysis to estimate the contact angles of powders in various liquids by the Washburn approach. The system is capable of the surface free energy calculations of solids by analyzing contact angles in different solvents.

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Universal testing machine is used for determining the mechanical properties of materials. The accessory, BioPuls temperature-controlled bath, enables the system to perform mechanical testing at ambient and simulated physiological conditions. The instrument can analyze a wide variety of samples, such as Polymer films, fabrics, gloves, polymer or ceramic composites, dental materials, etc., in tension and compression modes.

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Instron 3345 with BioPuls temperature-controlled bath is capable of the mechanical testing of samples in ambient and physiological conditions. In addition to tensile and compression analysis of materials, the equipment can be used for estimating the tear strength, conformability, and burst resistance of materials.

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Water vapor transmission rate (WVTR) is one of the inevitable tests to qualify textile materials, personal protective equipment, and wound dressing materials. CAF employs a Payne permeability cup (Make: Elcometer; Area: 30 cm2; volume capacity: 50 ml.) to estimate the water vapor transmission rate of films as per international standards (Gravimetric method).

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The synthetic blood penetration test is one of the inevitable tests to qualify the medical textile materials including personal protective equipment (PPE), coveralls, drapes, gowns, etc. This test qualifies the medical textile to be safe to guard the user from undesirable contact with patient blood. CAF employs a method as per ASTM F1670 to check the resistance of medical textiles to prevent the penetration of synthetic blood.

Handheld X-ray fluorescence (XRF) analyzer is a powerful tool to analyze the elemental composition of samples in a wide range of applications. This is a fast, accurate, and non-destructive testing equipment that utilizes energy-dispersive X-ray fluorescence for the detection and analysis of elements ranging from Mg to U without any sample preparation. Here the X-ray produced by the Rh anode source is used to irradiate the sample which results in the emission of X-rays with discrete energies unique for different elements present in the sample. Analysis of fluorescent X-rays will help to identify and quantify the elements present.

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XRF analysis would help in the elemental analysis of materials. The relative composition of elements can be used to identify the alloy grades as well. The inbuilt alloy library could be useful for the identification of over 300 grades of alloys. In addition to the alloy analysis, the equipment has modules for RoHS compliance testing, precious metal analysis, and coating thickness measurements.

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