...Fourier Transform Infrared (FTIR) Spectroscopy Group 1 (Monday 1-5pm) Author Reshma Reji Outline Introduction Objective of the Experiment Theory * FTIR Spectroscopy * FTIR Spectrophotometer * Samples Experimental Physical properties of reagents used Solution Preparation Procedure Instrument settings Data 1. IR spectrum of Chloroform and D-chloroform 2. Rotational Spectrum of CO2 (Standard Resolution) 3. Rotational Spectrum of CO2 (High Resolution) 4. Carbonyl stretch in 2-butanone solutions (wavenumber vs. % T) 5. Carbonyl stretch in 2-butanone solutions (wavenumber Vs Absorbance) 6. Calibration curve of 2-butanone solutions (concentration vs. absorbance) * Calculations a. Preparation of solutions b. Concentration of the unknown c. Percent error of observed and theoretical ratios of CH, CD stretch frequencies Results and Conclusion References Objective The goal of the first part of the experiment was to study the effects of isotopes on bond stretching. In the second part of the experiment, the influence of instrument resolution on the rotational spectrum of carbon dioxide was studied. The purpose of the third part of the experiment was to create a calibration curve to find the unknown concentration of 2-butanone. Introduction Fourier Transform Infrared Spectroscopy (FTIR) is a very useful analytical technique used for qualitative and quantitative analysis of organic and inorganic...
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...4A. Vesicular transfersome and liposome based transdermal gel of aceclofenac: 4A.1 Preformulation studies: Identification of drug was carried out by DSC, FTIR and UV spectrophotometry 4A.1.1 DSC studies-DSC studies were carried out at a temperature range of 25 º C to 165 º C at 10 º C increments of temperature. Figure4A.1-DSC Thermogram of Aceclofenac DSC thermogram indicates the M.P of 154º C which fairly matches with reported M.P of Aceclofenac, thus confirming the identity and purity of aceclofenac. 4A.1.2. FTIR studies- Figure4A.2 . FTIR spectra of Aceclofenac Figure.4A.3 Standard FTIR spectra of aceclofenac FTIR Interpretation: Figure 4A.4 Chemical structure of aceclofenac Table 4A.1 Interpretation...
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...pH 4.5 23.469 0.098 Phosphate Buffer pH 6.8 23.350 0.093 7.1.3: Physical properties Table 7.3: Physical Evaluation of Aspirin Physical properties Observations Bulk density(gm/mL) 0.682 Tap density(gm/mL) 0.883 Carr’s index (%) 22.72% Hausner’s ratio 1.29 7.1.4: Fourier transforms infrared (FTIR) Spectroscopy The IR spectrum of the pure Aspirin sample was recorded by FTIR Spectrometer is shown in Figure 7.1 which was compared with standard functional group frequencies of Aspirin as shown in Table 7.4 Table 7.4: Reported and observed IR frequencies of Aspirin Functional groups (Observed Frequency) (cm-1) (Reported Frequency) (cm-1) O-H-(Stretch) 3350.00 3100-3500 O-H stretch from CO-OH dimer 2991.59 3200-2800 Aromatic C-H stretch 3015.99 3150-3050 Aliphatic C-H Stretch 2898.28 2950-2850 -C=O stretch 1695.82 1700 Aromatic C=C stretch 1548.73 1600-1500 Aromatic C-H bending 713.46 600-850 The Functional group frequencies of Aspirin were in the reported range which indicates that the obtained sample was of Aspirin and was pure. Figure 7.1: FTIR spectrum of pure Aspirin 7.1.5: Differential scanning calorimetry (DSC) The DSC spectrum of pure drug was obtained and is given in Figure 7.2....
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...Introduction This research paper is mainly concerned with the production of lightweight geopolymer concrete using expanded poelystyrene (EPS) beads as part replacement of the normal aggregates for precast building components as well as in sandwich construction, the information on properties of lightweight geopolymer concrete with different percentage of EPS bead aggregate is given and it is also compared with the with the existing guidelines (ASTM C 90). Furthermore, performance of EPS/geopolymer concretes is discussed in relation to their flammability and insulation characteristics (Techniques used; DSC (Differential scanning calorimetry, based on heat difference), TG/DTA (Differential thermal analysis, based on temperature difference) and FTIR (Fourier transform infrared spectroscopy) under quasi-isothermal mode). Geopolymers as an alternative to ordinary Portland cement for concrete is used because it has high early compressive strength, low drying shrinkage, good fire resistance and superior durability in aggressive environment compared to Portland cement concrete. Geopolymers are produced through reactions between the alumino-silicate reactive materials (metakaoline, slag, fly ash etc) and their strength and microstructural properties are studied under fresh and hardened states. The selection of EPS bead aggregate was made mainly due to its low density, closed cellular structure, hydrophobic and energy absorbing characteristics. Experiment Materials * Class F fly...
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...Forensics includes the analysis of proof for criminal examinations and experts in this field are essential in piecing together the intricate details of a crime which can be later used in court during testimony. From the crime scene, materials are collected that can potentially solve the case. Bodily fluids such as blood, saliva, and urine must be studied to gain information about what had occurred. Forensic assessments must be conducted in a beneficial way for the evidence to make sure it will not be damaged in any way. The traditional methods for doing this are usually harmful and unsuccessful due to the workers needing very particular skills for the process to work correctly. In addition, chemicals can possibly be hazardous which makes...
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...The crystalline structure of regenerated lignocellulose as well as the untreated one are usually expressed by Total Crystallinity Index (TCI) and Lateral Order Index (LOI) using FTIR [318]. Purwandari et al. [310] reported that TCI (the absorbance ratio A1427/A898 calculated by FTIR spectra) of oil palm empty fruit bunch (OPEFB) reduced by up to 78%, during the pretreatment in 85% NMMO at 120°C for 3 h. In addition, ballooning and swelling modes of NMMO result in lower total crystallinity indexes at 120°C rather than 90°C. This finding is in contrast with ballooning and swelling modes of NMMO pretreated of cotton that result in lower crystallinity indexes at 90°C than 120°C [297]. However, crystallinity indexes decrease slightly for different modes of dissolution, ballooning, and swelling. Besides, the intramolecular hydrogen-bonding OH stretching at about 3,350 cm-l in pretreated cotton is broadened and shifted to a higher wave number, which is an indication of transforming...
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...All reactants were reagent grade and provided by the University of Colorado Denver Chemistry Department. FTIR spectra were obtained with a Nicolet iS5 ATR FTIR spectrometer and all measurements were in cm-1. The following abbreviations were used to describe transmittance bands: b (broad), n (narrow), sh (sharp), w (weak), m (medium), and s (strong). Isolation of Ibuprofen: 15 tablets contain 200 mg ibuprofen was obtained resulting in 3.54 g (17.1 mmol) Ibuprofen. Add 25 mL of acetone to the beaker and stirred for 5-10 minutes. Vacuum filtration was used to remove the acetone insoluble components. The ibuprofen was concentrated using the rotary evaporation. The mass of the crude ibuprofen was 3.54 g (17.1 mmol, 118%). Melting point was 67.2-70.2°C. For the isolation of ibuprofen, the major peaks are 3399.16 cm-1 O-H stretch, H-bonded, 2979.17 cm-1 C-H stretch, and 1700.18 cm-1 C=O stretch Formation of Diastereomeric Salts:...
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...Banana Peel as Alternative Bio-sorbent Material for Removal of 2-Chlorophenol from Water Salma I. M. Ibrahim1,2,3 Torsten C. Schmidt2; Samy M. Abd El-azeem3 1: Holding Company for Potable Water and Sanitation, Fayoum, Egypt 2: Instrumental Analytical Chemistry, University of Duisburg-Essen, Essen, Germany 3: Chemistry Departement, Faculty of Science, Fayoum University, Fayoum, Egypt Introduction Water is one of the vital necessities for the survival of human beings. Wastewater reclamation, recycling and reuse are vital to meet the water requirements for irrigation, industry and domestic use due to increasing population and development in many parts of the world. Industrial wastewaters largely possess organic and inorganic materials such as dyes, phenols, aromatic compounds, and heavy metals [1]. Phenols cause bad taste and odor of drinking water and can exert negative effects on different biological processes. Phenol and its derivatives also show mutagenic effects by unbinding of the DNA helix, inhibition of DNA synthesis in human, induction of gene mutations, chromosome aberrations and a neuploid formations (phenol, catechol) [2]. Because of this increased awareness and concern about environmental pollution, stringent national and international legislation has been set up, generating more efforts of research work in this area, especially in finding better and more efficient techniques to treat wastewater bearing these organic pollutants [3]. Bio-sorbents are certain...
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...fitted with a stirrer, a thermometer and a condenser and was dissolved in DMF solvent (20 mL). To that formaldehyde (0.3 mol as 37%) and a solution of resorcinol/ M-Cresol (0.1 mol) in 10 mL DMF were added simultaneously drop wise giving a clear solution and was stirred for 1 h. The mixture was refluxed in microwave oven using irradiation of 2.46 GHz at 80±2ºC for 50s until a viscous solution was obtained with the formation of a hard mass of resin. The colour of resultant resin is red-brown. Then sealed and cured at 70-75ºC for 12 h stored in polyethylene bottle. As carboxylic acid groups normally are decomposed above 100ºC, the resin was cured below 90ºC. The dry resin sample free from impurities was directly examined for FTIR, SEM, and elemental analysis..To convert the FAR and FAM resin samples in H+ form, the resulting hard mass was crushed to 20+30 or -60 +100 BSS mesh size as needed. The resin was conditioned by 0.1 N HCl solutions. The resins were washed with distilled water until free from acid. The resin was air dried to remove surface moisture. Where Y= -OH for resorcinol (FAR) and – CH3 for M cresol (FAM). Physico-chemical properties: FAR Properties Moisture content (%) 14.02 True density (dres) g/cm3 1.06 Apparent density (dcol) g/ml 0.71 Void volume fraction 0.36 Sodium ion-exchange 6.50 capacity mmol/g dry resin Concentration of fixed 6.21 ionogenic group mmol/cm3 Volume capacity 3.85 FAM 12.11 1.11 0.69 0.40 ...
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...Invitro evaluation and optimization of controlled release chitosan beads of Metformin hydrochloride Manjisa Choudhury, Tanaya Sarma, Samridh Srivastava, Vino S. School of Bio Sciences and Technology, VIT University, Vellore - 632014, Tamil Nadu, India manji.choudhury@gmail.com; +91-9626413610 Abstract Beads of chitosan, in the free and metformin HCl encapsulated forms were prepared by Chitosan/ TPP polyelectrolyte complex. The particles were further stabilized by crosslinking with glutaraldehyde. The size of the particles was found to be in the range of 1.0 to 2.0 mm. Both free and metformin HCL encapsulated Chitosan beads were analyzed by FTIR, Differential Scanning Calorimetry and X-ray diffraction studies. The rate of drug release was investigated by in vitro dissolution studies using UV spectroscopy. The results indicate that these Crosslinked chitosan beads are capable of controlled and sustained release of meformin HCL upto a maximum time of 12 h in PBS at pH 7.4. Keywords: Chitosan, Metformin HCl, Controlled drug delivery, In-Vitro release. Introduction Large number of active compounds is discovered that could serve as therapeutics but very few candidates show clinical success. Their poor activity in vivo is often due to the reason of their low bioavailability. Bioavailability is basically the rate and the extent at which a drug enters and affects the target tissue (Kidane, 2005). When a drug is administered systemically, its bioavailability is...
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...FTIR of ACS film were compared with PCS film (Fig. 3 (a & b)). In general, chitosan shows bands at 3000 to 3500 cm−1 (NH bond) and at 1400 to 1650 cm−1 (C=O bond) (Chatterjee et al., 2005). In ACS film, 5 prominent bands at 2921, 1638, 1556, 1376 and 1017cm−1 were recorded. The broad band inthe range 3000 to 3500 cm−1 is due to O–H and N-H stretching vibrations (George et al., 2011). Band at 1638 cm−1 represents acetylated amino group of chitin (C=O stretching, amide 1), which indicates the extent of deacetylation of chitosan (Saraswathy et al., 2001). Peak at 2921 and 1417 cm−1 corresponds to aliphatic C-H stretching and –CO stretching of primary alcoholic group, respectively (–CH2–OH) (Pranoto and others 2005). Another major absorption band observed at 1017 cm−1 represents the free primary amino group (–NH2) at C2 position of glucosamine, a major group present in chitosan (Xiao et al., 2003). In total, the FTIR spectra of ACS showed 7 prominent peaks explaining the stretching absorption due to aldehyde and esters, bending absorption due to methylene and methyl groups and double bond absorptions...
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...Clays and Clay Minerals, Vol. 49, No. 5, 410–432, 2001. BASELINE STUDIES OF THE CLAY MINERALS SOCIETY SOURCE CLAYS: INFRARED METHODS ´ JANA MADEJOVA AND PETER KOMADEL Institute of Inorganic Chemistry, Slovak Academy of Sciences, SK-842 36 Bratislava, Slovakia INTRODUCTION Infrared (IR) spectroscopy has a long and successful history as an analytical technique and is used extensively (McKelvy et al., 1996; Stuart, 1996). It is mainly a complementary method to X-ray diffraction (XRD) and other methods used to investigate clays and clay minerals. It is an economical, rapid and common technique because a spectrum can be obtained in a few minutes and the instruments are sufficiently inexpensive as to be available in many laboratories. An IR spectrum can serve as a fingerprint for mineral identification, but it can also give unique information about the mineral structure, including the family of minerals to which the specimen belongs and the degree of regularity within the structure, the nature of isomorphic substituents, the distinction of molecular water from constitutional hydroxyl, and the presence of both crystalline and non-crystalline impurities (Farmer, 1979). The interpretation of the absorption spectra of the Source Clays in the middle-IR (MIR) region (4000– 400 cm 1) given here follows those of Farmer and Russell (1964), Farmer (1974a, 1979) and Russell and Fraser (1994). In addition, reflectance spectra in the near-IR (NIR) region (11,000–4000 cm 1), where overtones...
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...|CM2101 (Principles of Spectroscopy) | |Experiment 1: Rovibrational Spectrum of Hydrogen Chloride | AIM To measure the infra-red (IR) spectrum of gaseous HCl using Fourier Transform Infra-Red (FTIR) spectrometer, and analyse the rotational fine structures. ABSTRACT The experiment aims to identify various parameters of gaseous HCl related to quantum mechanics by using high-resolution IR spectrum and graphical method of analysis. The values that are being investigated specifically are νe (equilibrium vibrational frequency), νeχe (product of equilibrium vibrational frequency and anharmonicity constant), k (force constant), B0 (rotational constant at n = 0), B1 (rotational constant at n = 1), Be (rotational constant at equilibrium internuclear distance), α (Coriolis constant) and re (equilibrium internuclear distance). The spectrum obtained shows strong fundamental absorption band approximately between 3100 and 2600 cm-1, with the origin of the band approximately at 2880 cm-1. It is also characterised by the presence of P and R branches which spreads out from the origin, with the former being present at a lower wavenumber region than the latter. In addition, double peaks are observed due to the presence of two isotopes of chlorine: 35Cl and 37Cl. INTRODUCTION One of the areas being...
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...N-acetylation using acetic anhydride and trimethylsylilation. 1μl of sample was injected into the GC-MS (Perkin Elmer ClarusSQ 8 GCMS with autosampler) using autosampler. GC-MS conditions used was- Column : RTX-5MS 30M, 0.32mm ID, Gradient conditions: (Total run time: 30 min), Carrier gas: Helium at a flow rate of 1ml min-1. Initial temperature was 0°C min-1 to 100°C with hold time 1min. Ramp 1 was 8°C min-1 to 260°C min-1 with hold time 5min and Ramp 2 was 10°C min-1 to 300°C min-1 with no hold time. For identification, six different standard sugars were processed and carried out with the same method. Sample runs were carried out in duplicates. Attenuated total reflectance- Fourier transform infrared spectroscopy (ATR-FTIR) For determination of functional group, ATR-FTIR spectra was obtained for fine lyophilized RPS powder placed on the Selenium crystal and scanned in the region of 4,000 to 600cm-1 on Perkin Elmer Spectrum 2 (Perkin Elmer, USA). Thermogravimetric (TGA) and Differential Scanning Calorimetry (DSC) analysis Thermogravimetric and DSC analyzes were carried out in NETZSCH STA 449 F3Jupiter® thermal analyzer. Simultaneous thermal analysis (TGA and DSC) was performed to measure two of the thermal properties at the same time. The RPS sample loaded on an alumina (Al2O3) pan was subjected to a freely selectable temperature (30°C to 500°C) under pure Nitrogen atmosphere at a temperature gradient of 10°C min-1. Analysis of rheological properties Rheological behaviour (shear viscosity...
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...Şencan & Mustafa Karaboyacı & Mehmet Kılıç Received: 26 November 2013 / Accepted: 23 April 2014 # Springer-Verlag Berlin Heidelberg 2014 Abstract This study aimed to determine the Pb+2 adsorption capacities of hazelnut shell and activated carbon obtained from hazelnut shell. It also aimed to determine the effect of ZnCl2 in the activation process. The hazelnut was pyrolyzed at 250 and 700 °C. For determining the capture speed of the adsorbents, the pseudo-first- and second-order kinetic studies were performed. The Freundlich and Langmuir isotherm models were used to determine adsorption equilibrium. The surface characterization of hazelnut shell and activated carbon was determined by Brunauer-Emmett-Teller (BET) analysis and FTIR spectrum. Pb+2 adsorption capacity of obtaining activated carbon was determined by ICP-OES analysis. The raw hazelnut shell’s BET surface area is 5.92 m2/g and the surface area of activated carbons which is pyrolyzed at 250 and 700 °C were determined (270.2 and 686.7 m2/g, respectively. The surface area of hazelnut shell, which pyrolyzed at 700 °C after being activated with ZnCl2, was determined to be 736.49 m2/g. Results show that physical adsorption process is dominant for the activated carbon pyrolysis at 700 °C but the chemical adsorption is dominant for the activated carbon pyrolysis at lower degrees and for raw hazelnut shell. Keywords Activated carbon . Heavy metals . Lead(II) . Kinetic . Isotherm . Hazelnut Responsible...
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