Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 3371

Search results for: thin layer chromatography

3371 Study on Meristem Culture of Purwoceng (Pimpinella pruatjan Molk.) and Its Stigmasterol Detected by Thin Layer Chromatography

Authors: Totik Sri Mariani, Sukrasno Isna, Tet Fatt Chia


Purwoceng (Pimpinella pruatjan Molk) is a legend plant used for increasing stamina by Kings in Java Island, Indonesia. Purpose of this study was to perform meristem culture and detected its stigmasterol by thin layer chromatography (TLC). Our result show that meristem culture could be propagated and grew into plantlet. After extracting intact acclimatized plant derived from meristem culture by hexane, we could detected stigmasterol by TLC. For suggestion, our extraction and TLC method could be used for detecting stigmasterol in others plant.

Keywords: purwoceng (pimpinella pruatjan), meristem culture, extraction, thin layer chromatography

Procedia PDF Downloads 357
3370 Comparative Forensic Analysis of Lipsticks Using Thin Layer Chromatography and Gas Chromatography

Authors: M. O. Ezegbogu, H. B. Osadolor


Lipsticks constitute a significant source of transfer evidence, and can, therefore, provide corroborative or inclusionary evidence in criminal investigation. This study aimed to determine the uniqueness and persistence of different lipstick smears using Thin Layer Chromatography (TLC), and Gas Chromatography with a Flame Ionisation Detector (GC-FID). In this study, we analysed lipstick smears retrieved from tea cups exposed to the environment for up to four weeks. The n-alkane content of each sample was determined using GC-FID, while TLC was used to determine the number of bands, and retention factor of each band per smear. This study shows that TLC gives more consistent results over a 4-week period than GC-FID. It also proposes a maximum exposure time of two weeks for the analysis of lipsticks left in the open using GC-FID. Finally, we conclude that neither TLC nor GC-FID can distinguish lipstick evidence recovered from hypothetical crime scenes.

Keywords: forensic science, chromatography, identification, lipstick

Procedia PDF Downloads 71
3369 Assessment of Aminopolyether on 18F-FDG Samples

Authors: Renata L. C. Leão, João E. Nascimento, Natalia C. E. S. Nascimento, Elaine S. Vasconcelos, Mércia L. Oliveira


The quality control procedures of a radiopharmaceutical include the assessment of its chemical purity. The method suggested by international pharmacopeias consists of a thin layer chromatographic run. In this paper, the method proposed by the United States Pharmacopeia (USP) is compared to a direct method to determine the final concentration of aminopolyether in Fludeoxyglucose (18F-FDG) preparations. The approach (no chromatographic run) was achieved by placing the thin-layer chromatography (TLC) plate directly on an iodine vapor chamber. Both methods were validated and they showed adequate results to determine the concentration of aminopolyether in 18F-FDG preparations. However, the direct method is more sensitive, faster and simpler when compared to the reference method (with chromatographic run), and it may be chosen for use in routine quality control of 18F-FDG.

Keywords: chemical purity, Kryptofix 222, thin layer chromatography, validation

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3368 Modified Ninhydrin Reagent for the Detection of Amino Acids on TLC Paper

Authors: H. Elgubbi, A. Mlitan, A. Alzridy


Ninhydrin is the most well known spray reagent for identification of amino acids. Spring with Ninhydrin as a non-specific reagent is well-known and widely used for its remarkable high sensitivity. Using Ninhydrin reagent alone to detect amino acid on thin layer chromatography (TLA) paper is not advisable due to its lower sensitivity. A new spray reagent, Stannus chloride solution (Sn CL2) has been used to detect amino acids on filtter paper (witman 14) and TLC paper, silica Gel, 60 F254 TLC Aluminium Sheet 20x20cm Merck- Germany. Also, modified TLC pre-staining method was used, which only consisted of 3 steps: spotting, separating and color. The improved method was rapid and inexpensive and the results obtained were clear and reliable. In addition, it is suitable for screening different amino acid.

Keywords: amino acid, ninhydrin, modified ninhydrin reagent, stannus chloride reagent, thin-layer chromatography (TLC), TLC pre-staining

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3367 Thin-Layer Drying Characteristics and Modelling of Instant Coffee Solution

Authors: Apolinar Picado, Ronald Solís, Rafael Gamero


The thin-layer drying characteristics of instant coffee solution were investigated in a laboratory tunnel dryer. Drying experiments were carried out at three temperatures (80, 100 and 120 °C) and an air velocity of 1.2 m/s. Drying experimental data obtained are fitted to six (6) thin-layer drying models using the non-linear least squares regression analysis. The acceptability of the thin-layer drying model has been based on a value of the correlation coefficient that should be close to one, and low values for root mean square error (RMSE) and chi-square (x²). According to this evaluation, the most suitable model for describing drying process of thin-layer instant coffee solution is the Page model. Further, the effective moisture diffusivity and the activation energy were computed employing the drying experimental data. The effective moisture diffusivity values varied from 1.6133 × 10⁻⁹ to 1.6224 × 10⁻⁹ m²/s over the temperature range studied and the activation energy was estimated to be 162.62 J/mol.

Keywords: activation energy, diffusivity, instant coffee, thin-layer models

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3366 Ruta graveolens Fingerprints Obtained with Reversed-Phase Gradient Thin-Layer Chromatography with Controlled Solvent Velocity

Authors: Adrian Szczyrba, Aneta Halka-Grysinska, Tomasz Baj, Tadeusz H. Dzido


Since prehistory, plants were constituted as an essential source of biologically active substances in folk medicine. One of the examples of medicinal plants is Ruta graveolens L. For a long time, Ruta g. herb has been famous for its spasmolytic, diuretic, or anti-inflammatory therapeutic effects. The wide spectrum of secondary metabolites produced by Ruta g. includes flavonoids (eg. rutin, quercetin), coumarins (eg. bergapten, umbelliferone) phenolic acids (eg. rosmarinic acid, chlorogenic acid), and limonoids. Unfortunately, the presence of produced substances is highly dependent on environmental factors like temperature, humidity, or soil acidity; therefore standardization is necessary. There were many attempts of characterization of various phytochemical groups (eg. coumarins) of Ruta graveolens using the normal – phase thin-layer chromatography (TLC). However, due to the so-called general elution problem, usually, some components remained unseparated near the start or finish line. Therefore Ruta graveolens is a very good model plant. Methanol and petroleum ether extract from its aerial parts were used to demonstrate the capabilities of the new device for gradient thin-layer chromatogram development. The development of gradient thin-layer chromatograms in the reversed-phase system in conventional horizontal chambers can be disrupted by problems associated with an excessive flux of the mobile phase to the surface of the adsorbent layer. This phenomenon is most likely caused by significant differences between the surface tension of the subsequent fractions of the mobile phase. An excessive flux of the mobile phase onto the surface of the adsorbent layer distorts the flow of the mobile phase. The described effect produces unreliable, and unrepeatable results, causing blurring and deformation of the substance zones. In the prototype device, the mobile phase solution is delivered onto the surface of the adsorbent layer with controlled velocity (by moving pipette driven by 3D machine). The delivery of the solvent to the adsorbent layer is equal to or lower than that of conventional development. Therefore chromatograms can be developed with optimal linear mobile phase velocity. Furthermore, under such conditions, there is no excess of eluent solution on the surface of the adsorbent layer so the higher performance of the chromatographic system can be obtained. Directly feeding the adsorbent layer with eluent also enables to perform convenient continuous gradient elution practically without the so-called gradient delay. In the study, unique fingerprints of methanol and petroleum ether extracts of Ruta graveolens aerial parts were obtained with stepwise gradient reversed-phase thin-layer chromatography. Obtained fingerprints under different chromatographic conditions will be compared. The advantages and disadvantages of the proposed approach to chromatogram development with controlled solvent velocity will be discussed.

Keywords: fingerprints, gradient thin-layer chromatography, reversed-phase TLC, Ruta graveolens

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3365 Electrochemical Layer by Layer Assembly

Authors: Mao Li, Yuguang Ma, Katsuhiko Ariga


The performance of functional materials is governed by their ability to interact with surrounding environments in a well-defined and controlled manner. Layer-by-Layer (LbL) assembly is one of the most widely used technologies for coating both planar and particulate substrates in a diverse range of fields, including optics, energy, catalysis, separations, and biomedicine. Herein, we introduce electrochemical-coupling layer-by-layer assembly as a novel fabrication methodology for preparing layered thin films. This assembly method not only determines the process properties (such as the time, scalability, and manual intervention) but also directly control the physicochemical properties of the films (such as the thickness, homogeneity, and inter- and intra-layer film organization), with both sets of properties linked to application-specific performance.

Keywords: layer by layer assembly, electropolymerization, carbazole, optical thin film, electronics

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3364 TiN/TiO2 Nanostructure Coating on Glass Substrate

Authors: F. Dabir, R. Sarraf-Mamoory, N. Riahi-Noori


In this work, a nanostructured TiO2 layer was coated onto a FTO-less glass substrate using screen printing technique for back contact DSSC application. Then, titanium nitride thin film was applied on TiO2 layer by plasma assisted chemical vapor deposition (PACVD) as charge collector layer. The microstructure of prepared TiO2 layer was characterized by SEM. The sheet resistance, microstructure and elemental composition of titanium nitride thin films were analysed by four point probe, SEM, and EDS, respectively. TiO2 layer had porous nanostructure. The EDS analysis of TiN thin film showed presence of chlorine impurity. Sheet resistance of TiN thin film was 30 Ω/sq. With respect to the results, PACVD TiN can be a good candidate as a charge collector layer in back contacts DSSC.

Keywords: TiO2, TiN, charge collector, DSSC

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3363 Graphene/ZnO/Polymer Nanocomposite Thin Film for Separation of Oil-Water Mixture

Authors: Suboohi Shervani, Jingjing Ling, Jiabin Liu, Tahir Husain


Offshore oil-spill has become the most emerging problem in the world. In the current paper, a graphene/ZnO/polymer nanocomposite thin film is coated on stainless steel mesh via layer by layer deposition method. The structural characterization of materials is determined by Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD). The total petroleum hydrocarbons (TPHs) and separation efficiency have been measured via gas chromatography – flame ionization detector (GC-FID). TPHs are reduced to 2 ppm and separation efficiency of the nanocomposite coated mesh is reached ≥ 99% for the final sample. The nanocomposite coated mesh acts as a promising candidate for the separation of oil- water mixture.

Keywords: oil spill, graphene, oil-water separation, nanocomposite

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3362 Developing Stability Monitoring Parameters for NIPRIMAL®: A Monoherbal Formulation for the Treatment of Uncomplicated Malaria

Authors: Ekere E. Kokonne, Isimi C. Yetunde, Okoh E. Judith, Okafor E. Ijeoma, Ajeh J. Isaac, Olobayo O. Kunle, Emeje O. Martins


NIPRIMAL® is a mono herbal formulation of Nauclea latifolia used in the treatment of malaria. The stability of extracts made from plant material is essential to ensure the quality, safety and efficacy of the finished product. This study assessed the stability of the formulation under three different storage conditions; normal room temperature, infrared and under refrigeration. Differential Scanning Calorimetry (DSC) and Thin Layer Chromatography (TLC) were used to monitor the formulations. The DSC analysis was done from 0oC to 350oC under the three storage conditions. Results obtained indicate that NIPRIMAL® was stable at all the storage conditions investigated. Thin layer chromatography (TLC) after 6 months showed there was no significant difference between retention factor (RF) values for the various storage conditions. The reference sample had four spots with RF values of 0.47, 0.68, 0.76, 0.82 respectively and these spots were retained in the test formulations with corresponding RF values were after 6 months at room temperature and refrigerated temperature been 0.56, 0.73, 0.80, 0.92 and 0.47, 0.68, 0.76, 0.82 respectively. On the other hand, the RF values (0.55, 0.74, 0.77, 0.93) obtained under infrared after 1 month varied slightly from the reference. The sample exposed to infrared had a lower heat capacity compared to that stored under room temperature or refrigeration. A combination of TLC and DSC measurements has been applied for assessing the stability of NIPRIMAL®. Both methods were found to be rapid, sensitive and reliable in determining its stability. It is concluded that NIPRIMAL® can be stored under any of the tested conditions without degradation. This study is a major contribution towards developing appropriate stability monitoring parameters for herbal products.

Keywords: differential scanning calorimetry, formulation, NIPRIMAL®, stability, thin layer hromatography

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3361 Multi-Layer Mn-Doped SnO2 Thin Film for Multi-State Resistive Switching

Authors: Zhemi Xu, Dewei Chu, Sean Li


Well self-assembled pure and Mn-doped SnO2 nanocubes were synthesized by interface thermodynamic method, which is ideal for highly homogeneous large scale thin film deposition on flexible substrates for various electric devices. Mn-doped SnO2 shows very good resistive switching with high On/Off ratio (over 103), endurance and retention characteristics. More important, the resistive state can be tuned by multi-layer fabrication by alternate pure SnO2 and Mn-doped SnO2 nanocube layer, which improved the memory capacity of resistive switching effectively. Thus, such a method provides transparent, multi-level resistive switching for next generation non-volatile memory applications.

Keywords: metal oxides, self-assembly nanoparticles, multi-level resistive switching, multi-layer thin film

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3360 Mathematical Modeling of Thin Layer Drying Behavior of Bhimkol (Musa balbisiana) Pulp

Authors: Ritesh Watharkar, Sourabh Chakraborty, Brijesh Srivastava


Reduction of water from the fruits and vegetables using different drying techniques is widely employed to prolong the shelf life of these food commodities. Heat transfer occurs inside the sample by conduction and mass transfer takes place by diffusion in accordance with temperature and moisture concentration gradient respectively during drying. This study was undertaken to study and model the thin layer drying behavior of Bhimkol pulp. The drying was conducted in a tray drier at 500c temperature with 5, 10 and 15 % concentrations of added maltodextrin. The drying experiments were performed at 5mm thickness of the thin layer and the constant air velocity of 0.5 m/s.Drying data were fitted to different thin layer drying models found in the literature. Comparison of fitted models was based on highest R2(0.9917), lowest RMSE (0.03201), and lowest SSE (0.01537) revealed Middle equation as the best-fitted model for thin layer drying with 10% concentration of maltodextrin. The effective diffusivity was estimated based on the solution of Fick’s law of diffusion which is found in the range of 3.0396 x10-09 to 5.0661 x 10-09. There was a reduction in drying time with the addition of maltodextrin as compare to the raw pulp.

Keywords: Bhimkol, diffusivity, maltodextrine, Midilli model

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3359 Influence of Maturity Stage on Nutritional and Therapeutic Potentialities of Solanum anguivi Lam Berries (Gnagnan) Cultivated in CôTe D'Ivoire

Authors: G. Dan Chépo, L. Ban-Koffi, N. Kouassi Kouakou, M. Dje Kouakou, J. Nemlin, A. Sahore Drogba, L. Kouame Patrice


Solanum anguivi Lam, collectively called Gnagnan in Côte d'Ivoire is an eggplant with nutritional and therapeutic potentialities more or less known. The present study was undertaken to analyze the biochemical composition of berries at the different stages of maturity. Data showed that at the first stage of maturity (green berries), fruits are rich in ascorbic acid (34.48 ± 1.7 mg / 100 g dm), phenolic compounds (956.7 ± 71.14 mg / 100 g dm), iron (467.7 ± 1.84 mg / 100 g dm), magnesium (404.6 ± 16.25 mg / 100 g dm) and potassium (404.64 ± 16.25 mg/100 g dm). However, at the last stage of maturity (red berries), fruits are rich in proteins, cellulose, total sugars, fat and potassium with the values of 22.53 ± 2 g/100 g dm, 19.12 ± 0.35 g/100 g dm, 3.7 ± 0.2 g/100 g dm, 2.65 ± 0.19 g/100 g dm and 2290.84 ± 22.24 mg / 100 g dm, respectively. The chromatography on thin layer revealed the presence of glucose, ribose, xylose, arabinose and fructose at all the maturity stages. Except for alkaloids and gallic tannins, the phytochemical sorting revealed that Gnagnan contain many pharmacological components. According to the maturity stages, orange and red berries showed a higher content in sterols and polyterpens, flavonoids and saponins. The green berries contain most of polyphenols, catechintannins and quinons. As for the yellow berries, they are rich in polyphenols and catechintannins. These data contribute to enhance clinical researches on nutritional and pharmacological properties of S. anguivi Lam.

Keywords: Gnagnan, maturity stage, chemical composition, chromatography thin layer, phytochemical sorting

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3358 HPTLC Fingerprint Profiling of Protorhus longifolia Methanolic Leaf Extract and Qualitative Analysis of Common Biomarkers

Authors: P. S. Seboletswe, Z. Mkhize, L. M. Katata-Seru


Protorhus longifolia is known as a medicinal plant that has been used traditionally to treat various ailments such as hemiplegic paralysis, blood clotting related diseases, diarrhoea, heartburn, etc. The study reports a High-Performance Thin Layer Chromatography (HPTLC) fingerprint profile of Protorhus longifolia methanolic extract and its qualitative analysis of gallic acid, rutin, and quercetin. HPTLC analysis was achieved using CAMAG HPTLC system equipped with CAMAG automatic TLC sampler 4, CAMAG Automatic Developing Chamber 2 (ADC2), CAMAG visualizer 2, CAMAG Thin Layer Chromatography (TLC) scanner and visionCATS CAMAG HPTLC software. Mobile phase comprising toluene, ethyl acetate, formic acid (21:15:3) was used for qualitative analysis of gallic acid and revealed eight peaks while the mobile phase containing ethyl acetate, water, glacial acetic acid, formic acid (100:26:11:11) for qualitative analysis of rutin and quercetin revealed six peaks. HPTLC sillica gel 60 F254 glass plates (10 × 10) were used as the stationary phase. Gallic acid was detected at the Rf = 0.35; while rutin and quercetin were not evident in the extract. Further studies will be performed to quantify gallic acid in Protorhus longifolia leaves and also identify other biomarkers.

Keywords: biomarkers, fingerprint profiling, gallic acid, HPTLC, Protorhus longifolia

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3357 Optimization of Cu (In, Ga)Se₂ Based Thin Film Solar Cells: Simulation

Authors: Razieh Teimouri


Electrical modelling of Cu (In,Ga)Se₂ thin film solar cells is carried out with compositionally graded absorber and CdS buffer layer. Simulation results are compared with experimental data. Surface defect layers (SDL) are located in CdS/CIGS interface for improving open circuit voltage simulated structure through the analysis of the interface is investigated with or without this layer. When SDL removed, by optimizing the conduction band offset (CBO) position of the buffer/absorber layers with its recombination mechanisms and also shallow donor density in the CdS, the open circuit voltage increased significantly. As a result of simulation, excellent performance can be obtained when the conduction band of window layer positions higher by 0.2 eV than that of CIGS and shallow donor density in the CdS was found about 1×10¹⁸ (cm⁻³).

Keywords: CIGS solar cells, thin film, SCAPS, buffer layer, conduction band offset

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3356 Physicochemical Characterization of Asphalt Ridge Froth Bitumen

Authors: Nader Nciri, Suil Song, Namho Kim, Namjun Cho


Properties and compositions of bitumen and bitumen-derived liquids have significant influences on the selection of recovery, upgrading and refining processes. Optimal process conditions can often be directly related to these properties. The end uses of bitumen and bitumen products are thus related to their compositions. Because it is not possible to conduct a complete analysis of the molecular structure of bitumen, characterization must be made in other terms. The present paper focuses on physico-chemical analysis of two different types of bitumens. These bitumen samples were chosen based on: the original crude oil (sand oil and crude petroleum), and mode of process. The aim of this study is to determine both the manufacturing effect on chemical species and the chemical organization as a function of the type of bitumen sample. In order to obtain information on bitumen chemistry, elemental analysis (C, H, N, S, and O), heavy metal (Ni, V) concentrations, IATROSCAN chromatography (thin layer chromatography-flame ionization detection), FTIR spectroscopy, and 1H NMR spectroscopy have all been used. The characterization includes information about the major compound types (saturates, aromatics, resins and asphaltenes) which can be compared with similar data for other bitumens, more importantly, can be correlated with data from petroleum samples for which refining characteristics are known. Examination of Asphalt Ridge froth bitumen showed that it differed significantly from representative petroleum pitches, principally in their nonhydrocarbon content, heavy metal content and aromatic compounds. When possible, properties and composition were related to recovery and refining processes. This information is important because of the effects that composition has on recovery and processing reactions.

Keywords: froth bitumen, oil sand, asphalt ridge, petroleum pitch, thin layer chromatography-flame ionization detection, infrared spectroscopy, 1H nuclear magnetic resonance spectroscopy

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3355 Determination of the Inhibitory Effects of N-Methylpyrrole Derivatives on Glutathione Reductase Enzyme

Authors: Esma Kocaoglu, Oktay Talaz, Huseyin Cavdar, Murat Senturk, Deniz Eki̇nci̇


Glutathione reductase (GR) is a crucial antioxidant enzyme which is responsible for the maintenance of the antioxidant GSH (glutathione) molecule. Antimalarial effects of some chemical molecules are attributed to their inhibition of GR; thus inhibitors of this enzyme are expected to be promising candidates for the treatment of malaria. In this work, GR inhibitory properties of N-Methylpyrrole derivatives are reported. Firstly, GR was purified by means of affinity chromatography using 2’,5’-ADP-Sepharose 4B as ligand. Enzymatic activity was measured by Beutler’s method. Synthesis of the compounds was approved by thin layer chromatography and column chromatography. Different inhibitor concentrations were used and all compounds were tested in triplicate at each concentration used. It was found that all compounds have better inhibitory activity than the strong GR inhibitor N,N-bis(2-chloroethyl)-N-nitrosourea, especially three molecules, 8m, 8n, and 8q, are the best among them with low micromolar I₅₀ values. Findings of our study indicate that these Schiff base derivatives are strong GR inhibitors which can be used as leads for designation of novel antimalaria candidates.

Keywords: glutathione reductase, antimalaria, inhibitor, enzyme

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3354 High-Performance Thin-layer Chromatography (HPTLC) Analysis of Multi-Ingredient Traditional Chinese Medicine Supplement

Authors: Martin Cai, Khadijah B. Hashim, Leng Leo, Edmund F. Tian


Analysis of traditional Chinese medicinal (TCM) supplements has always been a laborious task, particularly in the case of multi‐ingredient formulations. Traditionally, herbal extracts are analysed using one or few markers compounds. In the recent years, however, pharmaceutical companies are introducing health supplements of TCM active ingredients to cater to the needs of consumers in the fast-paced society in this age. As such, new problems arise in the aspects of composition identification as well as quality analysis. In most cases of products or supplements formulated with multiple TCM herbs, the chemical composition, and nature of each raw material differs greatly from the others in the formulation. This results in a requirement for individual analytical processes in order to identify the marker compounds in the various botanicals. Thin-layer Chromatography (TLC) is a simple, cost effective, yet well-regarded method for the analysis of natural products, both as a Pharmacopeia-approved method for identification and authentication of herbs, and a great analytical tool for the discovery of chemical compositions in herbal extracts. Recent technical advances introduced High-Performance TLC (HPTLC) where, with the help of automated equipment and improvements on the chromatographic materials, both the quality and reproducibility are greatly improved, allowing for highly standardised analysis with greater details. Here we report an industrial consultancy project with ONI Global Pte Ltd for the analysis of LAC Liver Protector, a TCM formulation aimed at improving liver health. The aim of this study was to identify 4 key components of the supplement using HPTLC, following protocols derived from Chinese Pharmacopeia standards. By comparing the TLC profiles of the supplement to the extracts of the herbs reported in the label, this project proposes a simple and cost-effective analysis of the presence of the 4 marker compounds in the multi‐ingredient formulation by using 4 different HPTLC methods. With the increasing trend of small and medium-sized enterprises (SMEs) bringing natural products and health supplements into the market, it is crucial that the qualities of both raw materials and end products be well-assured for the protection of consumers. With the technology of HPTLC, science can be incorporated to help SMEs with their quality control, thereby ensuring product quality.

Keywords: traditional Chinese medicine supplement, high performance thin layer chromatography, active ingredients, product quality

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3353 Uniform Porous Multilayer-Junction Thin Film for Enhanced Gas-Sensing Performance

Authors: Ping-Ping Zhang, Hui-Zhang, Xu-Hui Sun


Highly-uniform In2O3/CuO bilayer and multilayer porous thin films were successfully fabricated using self-assembled soft template and simple sputtering deposition technique. The sensor based on the In2O3/CuO bilayer porous thin film shows obviously improved sensing performance to ethanol at the lower working temperature, compared to single layer counterpart sensors. The response of In2O3/CuO bilayer sensors exhibits nearly 3 and 5 times higher than those of the single layer In2O3 and CuO porous film sensors over the same ethanol concentration, respectively. The sensing mechanism based on p-n hetero-junction, which contributed to the enhanced sensing performance was also experimentally confirmed by a control experiment which the SiO2 insulation layer was inserted between the In2O3 and CuO layers to break the p-n junction. In addition, the sensing performance can be further enhanced by increasing the number of In2O3/CuO junction layers. The facile process can be easily extended to the fabrication of other semiconductor oxide gas sensors for practical sensing applications.

Keywords: gas sensor, multilayer porous thin films, In2O3/CuO, p-n junction

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3352 Solar Cell Using Chemical Bath Deposited PbS:Bi3+ Films as Electron Collecting Layer

Authors: Melissa Chavez Portillo, Mauricio Pacio Castillo, Hector Juarez Santiesteban, Oscar Portillo Moreno


Chemical bath deposited PbS:Bi3+ as an electron collection layer is introduced between the silicon wafer and the Ag electrode the performance of the PbS heterojunction thin film solar thin film solar cells with 1 cm2 active area. We employed Bi-doping to transform it into an n-type semiconductor. The experimental results reveal that the cell response parameters depend critically on the deposition procedures in terms of bath temperature, deposition time. The device achieves an open-circuit voltage of 0.4 V. The simple and low-cost deposition method of PbS:Bi3+ films is promising for the fabrication.

Keywords: Bi doping, PbS, thin films, solar cell

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3351 Metal-Organic Chemical Vapor Deposition (MOCVD) Process Investigation for Co Thin Film as a TSV Alternative Seed Layer

Authors: Sajjad Esmaeili, Robert Krause, Lukas Gerlich, Alireza Mohammadian Kia, Benjamin Uhlig


This investigation aims to develop the feasible and qualitative process parameters for the thin films fabrication into ultra-large through-silicon-vias (TSVs) as vertical interconnections. The focus of the study is on TSV metallization and its challenges employing new materials for the purpose of rapid signal propagation in the microsystems technology. Cobalt metal-organic chemical vapor deposition (Co-MOCVD) process enables manufacturing an adhesive and excellent conformal ultra-thin film all the way through TSVs in comparison with the conventional non-conformal physical vapor deposition (PVD) process of copper (Cu) seed layer. Therefore, this process provides a Cu seed-free layer which is capable of direct Cu electrochemical deposition (Cu-ECD) on top of it. The main challenge of this metallization module is to achieve the proper alternative seed layer with less roughness, sheet resistance and granular organic contamination (e.g. carbon) which intensify the Co corrosion under the influence of Cu electrolyte.

Keywords: Cobalt MOCVD, direct Cu electrochemical deposition (ECD), metallization technology, through-silicon-via (TSV)

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3350 Microstructural Study of Mechanically Alloyed Powders and the Thin Films of Cufe Alloys

Authors: Mechri hanane, Azzaz Mohammed


Polycrystalline CuFe thin film was prepared by thermal evaporation process (Physical vapor deposition), using the nanocrystalline CuFe powder obtained by mechanical alloying After 24 h of milling elemental powders. The microscopic study of nanocrystalline powder and the thin film of Cu70Fe30 binary alloy were examined using transmission electron microscopy (TEM) and scanning electron microscope (SEM). The cross-sectional TEM images showed that the obtained CuFe layer was polycrystalline film of about 20 nm thick and composed of grains of different size ranging from 4 nm to 18 nm.

Keywords: nanomaterials, thin films, TEM, SEM

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3349 Surface Active Phthalic Acid Ester Produced by a Rhizobacterial Strain

Authors: M. L. Ibrahim, A. Abdulhamid


A surface active molecule synthesized by a rhizobacterial strain Bacillus lentus isolated from Cajanus cajan was investigated. The bioemulsifier was extracted, purified and partially characterized using standard methods. Surface properties of the bioemulsifier were determined by studying the emulsification index, solubility test and stability studies. Partial purification of the bioemulsifier was carried out using FT-IR analysis, Silica-gel column chromatography and thin layer chromatography. GC-MS analysis was carried out to detect the composition and mass of the lipids and esters. The isolate showed an emulsifying activity of 57% and surface activity of 36mm. The stability studies revealed that the bioemulsifier had better stability at temperature of 70oC, 8% pH and 8% NaCl concentration. FT-IR indicated the bioemulsifier to contain peptide and aliphatic chain, TLC revealed the compound to be ninhydrin positive and Column chromatography showed the presence of three amino acids namely; glutamine, valine and cysteine. GC-MS indicated the lipid moiety to contain aliphatic chain ranging from C9-C16 and two major peaks of 1,2-benzenedicarboxylic acid diethyl octyl ester. Therefore, surface active agent from Bacillus lentus can be used effectively in a wide range of applications such as in MEOR and in the biosynthesis of plasticizers for industrial uses.

Keywords: Bacillus lentus, bioemulsifiers, phthalic acid ester, Rhizosphere

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3348 Determination of Phytostearol in Serial Grains

Authors: Sumonthip Kongtun Janphuk


Ten cereal grains that usually used as ingredients in healthy products were studied for phytosteryl glucoside contents. β-sitosteryl glucoside in 10 cereal grains, including Phasecolus vulgaris L. (kidney bean), Sorghum bicolor (sorghum), Moringa oleifera Lam. (drumstick), Nelumbo nucifera (lotus), Vigna radiate L. (mung bean), Coix lacrymajobi (job’tears), Oryza sativa. (red rice), Glycine max L. Merrill. (soybean),Cucurbita maschata Decne (pumpkin) and Helianthas annuus (sunflower seeds), were analyzed using Thin-layer chromatography (TLC) and High-Performance liquid chromatography (HPLC). All grains were extracted with methanol before analysis. Red bean showed the maximum phytosteryl glucoside content of 0.42% w/w. The content of others were as follows: pumpkin seed 0.173%, mung bean 0.099 %, soybean 0.07%, dried moringa seed 0.067%, lotus seed 0.044%, sorghum 0.032%, sunflower seed 0.016%, Job's tears 0.012%, and brown rice 0.006%.

Keywords: cereal grains, phytosterol, β-sitosteryl glucoside, food analysis.

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3347 Preparation of Porous Metal Membrane by Thermal Annealing for Thin Film Encapsulation

Authors: Jaibir Sharma, Lee JaeWung, Merugu Srinivas, Navab Singh


This paper presents thermal annealing dewetting technique for the preparation of porous metal membrane for thin film encapsulation application. Thermal annealing dewetting experimental results reveal that pore size in porous metal membrane depend upon i.e. 1. The substrate on which metal is deposited for formation of porous metal cap membrane, 2. Melting point of metal used for porous metal cap layer membrane formation, 3. Thickness of metal used for cap layer, 4. Temperature used for porous metal membrane formation. Silver (Ag) was used as a metal for preparation of porous metal membrane by annealing the film at different temperature. Pores in porous silver film were analyzed using Scanning Electron Microscope (SEM). In order to check the usefulness of porous metal film for thin film encapsulation application, the porous silver film prepared on amorphous silicon (a-Si) was release using XeF2. Finally, guide line and structures are suggested to use this porous membrane for thin film encapsulation (TFE) application.

Keywords: dewetting, themal annealing, metal, melting point, porous

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3346 In2S3 Buffer Layer Properties for Thin Film Solar Cells Based on CIGS Absorber

Authors: A. Bouloufa, K. Djessas


In this paper, we reported the effect of substrate temperature on the structural, electrical and optical properties of In2S3 thin films deposited on soda-lime glass substrates by physical vapor deposition technique at various substrate temperatures. The In2Se3 material used for deposition was synthesized from its constituent elements. It was found that all samples exhibit one phase which corresponds to β-In2S3 phase. Values of band gap energy of the films obtained at different substrate temperatures vary in the range of 2.38-2.80 eV and decrease with increasing substrate temperature.

Keywords: buffer layer, In2S3, optical properties, PVD, structural properties

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3345 Gas Separation by Water-Swollen Membrane

Authors: Lenka Morávková, Zuzana Sedláková, Jiří Vejražka, Věra Jandová, Pavel Izák


The need to minimize the costs of biogas upgrading leads to a continuous search for new and more effective membrane materials. The improvement of biogas combustion efficiency is connected with polar gases removal from a feed stream. One of the possibilities is the use of water–swollen polyamide layer of thin film composite reverse osmosis membrane for simultaneous carbon dioxide and hydrogen sulphide removal. Transport properties and basic characteristics of a thin film composite membrane were compared in the term of appropriate water-swollen membrane choice for biogas upgrading. SEM analysis showed that the surface of the best performing composites changed significantly upon swelling by water. The surface changes were found to be a proof that the selective skin polyamide layer was swollen well. Further, the presence of a sufficient number of associative centers, namely amido groups, inside the upper layer of the hydrophilic thin composite membrane can play an important role in the polar gas separation from a non-polar gas. The next key factor is a high porosity of the membrane support.

Keywords: biogas upgrading, carbon dioxide separation, hydrogen sulphide separation, water-swollen membrane

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3344 CuIn₃Se₅ Colloidal Nanocrystals and Its Ink-Coated Films for Photovoltaics

Authors: M. Ghali, M. Elnimr, G. F. Ali, A. M. Eissa, H. Talaat


CuIn₃Se₅ material is indexed as ordered vacancy compounds having excellent matching properties with CuInGaSe (CIGS) solar absorber layer. For example, the valence band offset of CuIn₃Se₅ with CIGS is nearly 0.3 eV, and the lattice mismatch is less than 1%, besides the absence of discontinuity in their conduction bands. Thus, CuIn₃Se₅ can work as a passivation layer for repelling holes from CIGS/CdS interface and hence to reduce the interface carriers recombination and consequently enhancing the efficiency of CIGS/CdS solar cells. Theoretically, it was reported earlier that an improvement in the efficiency of p-CIGS-based solar cell with a thin ~100 nm of n-CuIn₃Se₅ layer is expected. Recently, a reported experiment demonstrated significant improvement in the efficiency of Molecular Beam Epitaxy (MBE) grown CIGS solar cells from 13.4 to 14.5% via inserting a thin layer of MBE-grown Cu(In,Ga)₃Se₅ layer at the CdS/CIGS interface. It should be mentioned that CuIn₃Se₅ material in either bulk or thin film form, are usually fabricated by high vacuum physical vapor deposition techniques (e.g., three-source co-evaporation, RF sputtering, flash evaporation, and molecular beam epitaxy). In addition, achieving photosensitive films of n-CuIn₃Se₅ material is important for new hybrid organic/inorganic structures, where inorganic photo-absorber layer, with n-type conductivity, can form n–p junction with organic p-type material (e.g., conductive polymers). A detailed study of the physical properties of CuIn₃Se₅ is still necessary for better understanding of device operation and further improvement of solar cells performance. Here, we report on the low-cost synthesis of CuIn₃Se₅ material in nano-scale size, with an average diameter ~10nm, using simple solution-based colloidal chemistry. In contrast to traditionally grown bulk tetragonal CuIn₃Se₅ crystals using high Vacuum-based technology, our colloidal CuIn₃Se₅ nanocrystals show cubic crystal structure with a shape of nanoparticles and band gap ~1.33 eV. Ink-coated thin films prepared from these nanocrystals colloids; display n-type character, 1.26 eV band gap and strong photo-responsive behavior with incident white light. This suggests the potential use of colloidal CuIn₃Se₅ as an active layer in all-solution-processed thin film solar cells.

Keywords: nanocrystals, CuInSe, thin film, optical properties

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3343 Effect of Temperature on the Structural and Optical Properties of ZnS Thin Films Obtained by Chemical Bath Deposition in Acidic Medium

Authors: Hamid Merzouk, Dajhida Talantikite, Amel Tounsi


Thin films of ZnS have been deposited by chemical route into acidic medium. The deposition time fixed at 5 hours, and the bath temperature varied from 80° C to 95°C with an interval of 5°C. The X-ray diffraction (XRD), UV/ visible spectrophotometry, Fourier Transform Infrared spectroscopy (FTIR) have been used to study the effect of temperature on the structural and optical properties of ZnS thin films. The XRD spectrum of the ZnS layer obtained shows an increase of peaks intensity of ZnS with increasing bath temperature. The study of optical properties exhibit good transmittance (60–80% in the visible region), and the band gap energy of the ZnS thin film decrease from 3.71 eV to 3.64 eV while the refractive index (n) increase with increasing temperature bath. The FTIR analyze confirm our studies and show characteristics bands of vibration of Zn-S.

Keywords: ZnS thin films, XRD spectra, optical gap, XRD

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3342 Stability-Indicating High-Performance Thin-Layer Chromatography Method for Estimation of Naftopidil

Authors: P. S. Jain, K. D. Bobade, S. J. Surana


A simple, selective, precise and Stability-indicating High-performance thin-layer chromatographic method for analysis of Naftopidil both in a bulk and in pharmaceutical formulation has been developed and validated. The method employed, HPTLC aluminium plates precoated with silica gel as the stationary phase. The solvent system consisted of hexane: ethyl acetate: glacial acetic acid (4:4:2 v/v). The system was found to give compact spot for Naftopidil (Rf value of 0.43±0.02). Densitometric analysis of Naftopidil was carried out in the absorbance mode at 253 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2=0.999±0.0001 with respect to peak area in the concentration range 200-1200 ng per spot. The method was validated for precision, recovery and robustness. The limits of detection and quantification were 20.35 and 61.68 ng per spot, respectively. Naftopidil was subjected to acid and alkali hydrolysis, oxidation and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation and thermal conditions. This indicates that the drug is susceptible to acid, base, oxidation and thermal conditions. The degraded product was well resolved from the pure drug with significantly different Rf value. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of investigated drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of Naftopidil in bulk drug and pharmaceutical formulation.

Keywords: naftopidil, HPTLC, validation, stability, degradation

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