Search results for: Column chromatography

Authors: Ghasem Khodahami, Vahid Rowshan, Mojtaba Pakparvar

Abstract:

Stachys forms one of the largest genera in the flowering plant family Lamiaceae. The number of species in the genus is estimated from about 300 to about 450 and comprises some 34 species in Iran. This genus is one of the richest sources of diterpenes which are particularly interesting because of their ecological role as antifeedants against different species of insects and for their role as the medicinal properties of the plants. The ecological distribution of Stachys inflata was studied and the resulted eco-types were sampled from four regions ranging 230-340 mm of rainfall and 1690-2125 m a.s.l of height In Fars Province Southern Iran. The essential oils of air-dried samples were obtained by hydrodistillation and analyzed by gas chromatography and gas chromatography/mass spectrometry. The number of secondary metabolites varied from 25 to 50 depending to ecological conditions. The main compounds in these areas were: Germacrene D, Bicyclogermacrene, spathulenol, δ-cadinene. Statistical analysis of photochemical resulted in recognizing 3 distinct groups that show internal variety in these herbs.

Keywords: eco-type, phytochemistry, secondary metabolites, Stachys inflata

Procedia PDF Downloads 189

Authors: Bong Keun Kang, Sung Suk Oh, Jeong-Woo Sohn, Jong-Ryul Choi, Young Ho Kim

Abstract:

In this paper, we describe two-step micro-pattering by using laser cutting and wax printing. Wax printing is performed only on the bridges for hydrophobic barriers. We prepared 405nm blue-violet laser module and wax pencil module. And, this two modules combine x-y plot. The hollow microstructure formed by laser patterning define the hydrophilic flowing paths. However, bridges are essential to avoid the cutting area being the island. Through the support bridges, microfluidic solution spread out to the unnecessary areas. Chromatography blotting paper was purchased from Whatman. We used 20x20 cm and 46x57 cm of chromatography blotting paper. Axis moving speed of x-y plot was the main parameter of optimization. For aligning between the two patterning, the paper sheet was taped at the bottom. After the two-step patterning, temperature curing step was done at 110-130 °C. The resolution of the fabrication and the potential of the multiplex detection were investigated.

Keywords: µPADs, microfluidic, biosensor, mass-fabrication

Procedia PDF Downloads 441

Authors: Anupalli Roja Rani, Saraswathi Jaggali

Abstract:

Rose-scented geranium (Pelargonium graveolens L’Hér.) is an erect, much-branched shrub. It is indigenous to various parts of southern Africa, and it is often called Geranium. Pelargonium species are widely used by traditional healers in the areas of Southern Africa by Sotho, Xhosa, Khoi-San and Zulus for its curative and palliative effects in the treatment of diarrhea, dysentery, fever, respiratory tract infections, liver complaints, wounds, gastroenteritis, haemorrhage, kidney and bladder disorders. We have used Plant materials for extracting active compounds from analytical grades of solvents methanol, ethyl acetate, chloroform and water by a soxhlet apparatus. The phytochemical screening reveals that extracts of Pelargonium graveolens contains alkaloids, glycosides, steroids, tannins, saponins and phenols in ethyl acetate solvent. The antioxidant activity was determined using 1, 1-diphenyl-2-picrylhydrazyl (DPPH) bleaching method and the total phenolic content in the extracts was determined by the Folin–Ciocalteu method. Due to the presence of different phytochemical compounds in Pelargonium the anti-microbial activity against different micro-organisms like E.coli, Streptococcus, Klebsiella and Bacillus. Fractionation of plant extract was performed by column chromatography and was confirmed with HPLC analysis, NMR and FTIR spectroscopy for the compound identification in different organic solvent extracts.

Keywords: Pelargonium graveolens L’Hér, DPPH, micro-organisms, HPLC analysis, NMR, FTIR spectroscopy

Procedia PDF Downloads 464

Authors: Harshada Vaidya-Kannur, Dattatraya Naik

Abstract:

Propolis, one of the beehive products also referred as bee-glue is sticky dark coloured complex mixture of compounds. The volatile oil can be isolated from the propolis by hydrodistillation. The mark that is left behind after the removal of volatile oil is referred as the de-oiled propolis. Antioxidant as well as anti-inflammatory properties of total ethanolic extract of de-oiled propolis (TEEDP) was investigated. Another lot of deoiled propolis was successively exacted with hexane, ethyl acetate and ethanol. Activities of these fractions were also determined. Antioxidant activity was determined by studying ABTS, DPPH and NO radical scavenging. Determination of anti-inflammatory activity was carried out by topical TPA induced mouse ear oedema model. It is noteworthy that ethyl acetate fraction of deoiled propolis (EAFDP) exhibited 49.45 % TEAC activity at the concentration 0.2 mg/ml which is equivalent to the activity of trolox at the concentration 0.2 mg/ml. Its DPPH scavenging activity (72.56%) was closely comparable to that of trolox (75%). However its NO scavenging activity was comparatively low. From IC50 values it could be concluded that the efficiency of scavenging ABTS radicals by the de-oiled propolis was more pronounced as compared to scavenging of other radicals. Studies by TPA induced mouse ear inflammation model indicated that the de-oiled propolis of Indian origin had significant topical anti-inflammatory activity. The EAFDP was found to be the most active fraction for this activity also. The purification of EAFP yielded six pure crystalline compounds. These compounds were identified by their physical data and spectral data.

Keywords: anti-inflammatory activity, anti-oxidant activity, column chromatography, de-oiled propolis

Procedia PDF Downloads 267

Authors: Zandi Ahmad, Sokhanguei Yahya, Saboonchi Reza

Abstract:

Objective: The new and modern lifestyle, especially in the twenty-first century and lack of movement in spinal structure have made patients and the physicians in the field of health and also other insurance companies in the developed and developing countries worry more than before about the abnormalities of spinal column- this great healthcare problem. The high prevalence of spinal column in all age groups -from children to adults- and in all professions have led the researchers to the idea of giving an opportunity to all those who worry about the dangers threatening the spinal column. Therefore, one of the corrective methods for these patients is using SEAS exercises. Materials and Methods: This study aims at investigating the effect of one-period of SEAS exercises on some spinal biomechanical and postural parameters in the students with idiopathic scoliosis. According to the nature of the study and research objectives as well as the data collection methods, the current research is a semi-empirical survey. The research population is comprised of students with idiopathic scoliosis. A total number of 30 students were selected using available sampling and divided into two groups of control and SEAS exercises. Scoliometer was used for data collection. Descriptive statistics were used to categorize the findings. Kolmogorov-Smirnov statistical models were used to confirm that the distribution of the data is normal and T-test was used for effectiveness. Hypothesis testing was done using SPSS21. Conclusion: Results show that SEAS exercises have a significant effect in Adam’s Test. Therefore, according to the obtained results, SEAS exercises can be used to recover idiopathic scoliosis among the students. Further studies in larger samples and treatment, periods as well as more follow-up investigations appear to be essential to prove these effects.

Keywords: SEAS exercises, idiopathic scoliosis, Adam’s test, exercise

Procedia PDF Downloads 262

Authors: Shuyuan Lin, Zhaohui Huang, Mizi Fan

Abstract:

In the majority of previous research into modelling large scale composite floor subjected to fire, the beam-to-column and beam-to-beam connections were assumed to behave either as pinned or rigid for simplicity, and the vertical shear and axial tension failures of the connection were not taken into account. We have recently developed robust two-noded connection models for modeling endplate and partial endplate steel connections under fire conditions. The main objective of this research is to systematically investigate the impact of the connections of protected beams, on the tensile membrane actions of supported floor slabs in which the failures of the connections, such as, axial tension, vertical shear and bending are accounted for. The models developed have very good numerical stability under a static solver condition, and can be used for large scale modelling of composite buildings in fire.

Keywords: fire, steel structure, component-based model, beam-to-column connections

Procedia PDF Downloads 423

Authors: Ferhat Mohamed, Boukhatem Mohamed Nadjib, Chemat Farid

Abstract:

Simultaneous distillation–extraction (SDE) is routinely used by analysts for sample preparation prior to gas chromatography analysis. In this work, a new process design and operation for microwave assisted simultaneous distillation – solvent extraction (MW-SDE) of volatile compounds was developed. Using the proposed method, isolation, extraction and concentration of volatile compounds can be carried out in a single step. To demonstrate its feasibility, MW-SDE was compared with the conventional technique, Simultaneous distillation–extraction (SDE), for gas chromatography-mass spectrometry (GC-MS) analysis of volatile compounds in a fresh orange juice and a dry spice “carvi seeds”. SDE method required long time (3 h) to isolate the volatile compounds, and large amount of organic solvent (200 mL of hexane) for further extraction, while MW-SDE needed little time (only 30 min) to prepare sample, and less amount of organic solvent (10 mL of hexane). These results show that MW-SDE–GC-MS is a simple, rapid and solvent-less method for determination of volatile compounds from aromatic plants.

Keywords: essential oil, extraction, distillation, carvi seeds

Procedia PDF Downloads 536

Authors: Mahdi Sadeghian, Mahmoud Hassanlourad, Alireza Ardakani, Reza Dinarvand

Abstract:

In this research, the behavior of monopiles, under lateral loads, was investigated with vertical and oblique piles by Finite Element Method. In engineering practice when soil-pile interaction comes to the picture some simplifications are applied to reduce the design time. As a simplified replacement of soil and pile interaction analysis, pile could be replaced by a column. The height of the column would be equal to the free length of the pile plus a portion of the embedded length of it. One of the important factors studied in this study was that columns with an equivalent length (free length plus a part of buried depth) could be used instead of soil and pile modeling. The results of the analysis show that the more internal friction angle of the soil increases, the more the bearing capacity of the soil is achieved. This additional length is 6 to 11 times of the pile diameter in dense soil although in loose sandy soil this range might increase.

Keywords: Depth of fixity, Lateral bearing capacity, Oblique pile, Pile group, Soil-structure interaction

Procedia PDF Downloads 197

Authors: Li Xu, Yang Hong, T. Zhao Wen

Abstract:

Experimental results of many RC beam-column subassemblage indicate that slippage of longitudinal beam rebar within the joint and the shear deformation of joint core have significant influence on seismic behavior of the subassemblage. However, rigid joint assumption has been generally used in the seismic response analysis of RC frames, in which two kinds of inelastic deformation of joint have been ignored. Based on OpenSees platform, ‘Super Joint Element Model’ with more detailed inelastic mechanism is used to simulate the inelastic response of joints. Two finite element models of typical RC plane frame, namely considering or ignoring the inelastic deformation of joint respectively, were established and analyzed under seven strong earthquake waves. The simulated global and local inelastic deformations of the RC plane frame is shown and discussed. The analyses also confirm the security of the earthquake-resistant frame designed according to Chinese codes.

Keywords: frame structure, beam-column joint, longitudinal bar slippage, shear deformation, nonlinear analysis

Procedia PDF Downloads 385

Authors: Riya Roy, Anjana Bhasi

Abstract:

Column-supported embankments provide a practical and efficient solution for construction on soft soil due to the low cost and short construction times. In the recent years, geosynthetic have been used in combination with column systems to support embankments. The load transfer mechanism in these systems is a combination of soil arching effect, which occurs between columns and membrane effect of the geosynthetic. This paper aims at the study of soil arching effect on columnar embankments using finite element software, ABAQUS. An axisymmetric finite element model is generated and using this model, parametric studies are carried out. Thus the effects of various factors such as height of embankment fill, elastic modulus of pile and tensile stiffness of geosynthetic, on soil arching have been studied. The development of negative skin friction along the pile-soil interface have also been studied and the results obtained from this study are compared with the current design methods.

Keywords: ABAQUS, geosynthetic, negative skin friction, soil arching

Procedia PDF Downloads 349

Authors: C. Shim, C. Koem, S. Park, S. Lee

Abstract:

This paper deals with experimental studies on pre stressed precast concrete columns with continuous reinforcing bars and pre stressing tendons. Design requirements on minimum transverse reinforcement ratio are not included in current design codes. Pre stressing introduces additional compression to the column. Precast columns with different transverse reinforcement ratios were tested to derive adequate design requirement. Displacement ductility of the pre stressed precast columns was evaluated and compared with previous studies. Design of axial steels including reinforcing bars and pre stressing tendons influenced on the seismic performance. Without significant increase of transverse reinforcement ratio, the specimens showed required displacement ductility without reduction of their flexural strength. Design recommendations for precast bridge piers were derived.

Keywords: displacement ductility, flexural strength, prestressed precast column, transverse reinforcement

Procedia PDF Downloads 259

Authors: M. Kakavand, S. A. Naeini

Abstract:

Dynamic properties of soil in small strains, especially for geotechnical engineers, are important for describing the behavior of soil and estimation of the earth structure deformations and structures, especially significant structures. This paper presents the effect of density on the shear modulus and damping ratio of saturated clean sand at various isotropic confining pressures. For this purpose, the specimens were compared with two different relative densities, loose Dr = 30% and dense Dr = 70%. Dynamic parameters were attained from a series of consolidated undrained fixed – free type torsional resonant column tests in small strain. Sand No. 161 is selected for this paper. The experiments show that by increasing sand density and confining pressure, the shear modulus increases and the damping ratio decreases.

Keywords: dynamic properties, shear modulus, damping ratio, clean sand, density, confining pressure, resonant column/torsional simple shear, TSS

Procedia PDF Downloads 95

Authors: Furqan M. Kadhum, Asmaa A. Hussein, Maysaa Ch. Hatem

Abstract:

Hyaluronidase enzyme was purified from the clinical isolate Staphyloccus aureus in three purification steps, first by precipitation with 90% saturated ammonium sulfate, ion exchange chromatography on DEAE-Cellulose, and gel filtration chromatography throughout Sephacryl S-300. Specific activity of the purified enzyme was reached 930 U/mg protein with 7.4 folds of purification and 46.5% recovery. The enzyme has an average molecular weight of about 69 kDa, with an optimum pH of enzyme activity and stability at pH 7, also the optimum temperature for activity was 37oC. The enzyme was stable with full activity at a temperature ranged between 30-40 oC. Metal ions showed variable inhibitory degree with the strongest effect for Fe+3, however, the chelating and reducing agents had no or little effects. Cytotoxic studies for purified and crude hyaluronidase against cancer cell Hep G2 type at different enzyme concentrations and exposure times showed that the inhibition effect of both crude and purified enzyme increased by increasing the enzyme concentration with no change was observed at 24hr, while at 48 and 72 hrs the same inhibition rate were observed for purified enzyme and differ for the crude filtrate.

Keywords: hyaluronidase, S. aureus, metal ions, cytotoxicity

Procedia PDF Downloads 421

Authors: M. Jerold, V. Sivasubramanian

Abstract:

In this study, nano zero valent iron Sargassum swartzii (nZVI-SS) biocomposite a marine algal based biosorbent was used for the removal of simulated crystal violet (CV) in batch and continuous fixed bed operation. The Box-Behnen design (BBD) experimental results revealed the biosoprtion was maximum at pH 7.5, biosorbent dosage 0.1 g/L and initial CV concentration of 100 mg/L. The effect of various column parameters like bed depth (3, 6 and 9 cm), flow rate (5, 10 and 15 mL/min) and influent CV concentration (5, 10 and 15 mg/L) were investigated. The exhaustion time increased with increase of bed depth, influent CV concentration and decrease of flow rate. Adam-Bohart, Thomas and Yoon-Nelson models were used to predict the breakthrough curve and to evaluate the model parameters. Out of these models, Thomas and Yoon-Nelson models well described the experimental data. Therefore, the result implies that nZVI-SS biocomposite is a cheap and most promising biosorbent for the removal of CV from wastewater.

Keywords: algae, biosorption, zero-valent, dye, wastewater

Procedia PDF Downloads 153

Authors: Hoda Mahgoub, Abeer Hanafy

Abstract:

Linagliptin (LNG) belongs to dipeptidyl-peptidase-4 (DPP-4) inhibitor class. DPP-4 inhibitors represent a new therapeutic approach for the treatment of type 2 diabetes in adults. The aim of this work was to develop and validate an accurate and reproducible HPLC method for the determination of LNG with high sensitivity in rat plasma. The method involved separation of both LNG and pindolol (internal standard) at ambient temperature on a Zorbax Eclipse XDB C18 column and a mobile phase composed of 75% methanol: 25% formic acid 0.1% pH 4.1 at a flow rate of 1.0 mL.min-1. UV detection was performed at 254nm. The method was validated in compliance with ICH guidelines and found to be linear in the range of 5–1000ng.mL-1. The limit of quantification (LOQ) was found to be 5ng.mL-1 based on 100µL of plasma. The variations for intra- and inter-assay precision were less than 10%, and the accuracy values were ranged between 93.3% and 102.5%. The extraction recovery (R%) was more than 83%. The method involved a single extraction step of a very small plasma volume (100µL). The assay was successfully applied to an in-vivo pharmacokinetic study of LNG in rats that were administered a single oral dose of 10mg.kg-1 LNG. The maximum concentration (Cmax) was found to be 927.5 ± 23.9ng.mL-1. The area under the plasma concentration-time curve (AUC0-72) was 18285.02 ± 605.76h.ng.mL-1. In conclusion, the good accuracy and low LOQ of the bioanalytical HPLC method were suitable for monitoring the full pharmacokinetic profile of LNG in rats. The main advantages of the method were the sensitivity, small sample volume, single-step extraction procedure and the short time of analysis.

Keywords: HPLC, linagliptin, pharmacokinetic study, rat plasma

Procedia PDF Downloads 222

Authors: Nataša Stojić, Mira Pucarević, Nebojša Ralević, Vojislava Bursić, Gordan Stojić

Abstract:

Surface soil (0 – 10 cm) samples from 52 sampling sites along the length of railway tracks on the territory of Srem (the western part of the Autonomous Province of Vojvodina, itself part of Serbia) were collected and analyzed for 7 polychlorinated biphenyls (PCBs) in order to see how the distance from the railroad on the one hand and dump on the other hand, affect the concentration of PCBs (CPCBs) in the soil. Samples were taken at a distance of 0.03 to 4.19 km from the railway and 0.43 to 3.35 km from the landfills. For the soil extraction the Soxhlet extraction (USEPA 3540S) was used. The extracts were purified on a silica-gel column (USEPA 3630C). The analysis of the extracts was performed by gas chromatography with tandem mass spectrometry. PCBs were not detected only at two locations. Mean total concentration of PCBs for all other sampling locations was 0,0043 ppm dry weight (dw) with a range of 0,0005 to 0,0227 ppm dw. On the part of the data that were interesting for this research with statistical methods (PCA) were isolated factors that affect the concentration of PCBs. Data were also analyzed using the Pearson's chi-squared test which showed that the hypothesis of independence of CPCBs and distance from the railway can be rejected. Hypothesis of independence between CPCB and the percentage of humus in the soil can also be rejected, in contrast to dependence of CPCB and the distance from the landfill where the hypothesis of independence cannot be rejected. Based on these results can be said that railway transport is a potential source of PCBs. The next step in this research is to establish the position of transformers which are located near sampling sites as another important factor that affects the concentration of PCBs in the soil.

Keywords: GC/MS, landfill, PCB, railway, soil

Procedia PDF Downloads 302

Authors: Birute Bugelyte, Ingrida Jurkute, Vida Vickackaite

Abstract:

The most complicated step of the determination of volatile compounds in complex matrices is the separation of analytes from the matrix. Traditional analyte separation methods (liquid extraction, Soxhlet extraction) require a lot of time and labour; moreover, there is a risk to lose the volatile analytes. In recent years, headspace gas chromatography has been used to determine volatile compounds. To date, traditional extraction solvents have been used in headspace gas chromatography. As a rule, such solvents are rather volatile; therefore, a large amount of solvent vapour enters into the headspace together with the analyte. Because of that, the determination sensitivity of the analyte is reduced, a huge solvent peak in the chromatogram can overlap with the peaks of the analyts. The sensitivity is also limited by the fact that the sample can’t be heated at a higher temperature than the solvent boiling point. In 2018 it was suggested to replace traditional headspace gas chromatographic solvents with non-volatile, eco-friendly, biodegradable, inexpensive, and easy to prepare deep eutectic solvents (DESs). Generally, deep eutectic solvents have low vapour pressure, a relatively wide liquid range, much lower melting point than that of any of their individual components. Those features make DESs very attractive as matrix media for application in headspace gas chromatography. Also, DESs are polar compounds, so they can be applied for microwave assisted extraction. The aim of this work was to investigate the possibility of applying deep eutectic solvents for microwave assisted extraction and headspace gas chromatographic determination of hexanal in fat-rich food. Hexanal is considered one of the most suitable indicators of lipid oxidation degree as it is the main secondary oxidation product of linoleic acid, which is one of the principal fatty acids of many edible oils. Eight hydrophilic and hydrophobic deep eutectic solvents have been synthesized, and the influence of the temperature and microwaves on their headspace gas chromatographic behaviour has been investigated. Using the most suitable DES, microwave assisted extraction conditions and headspace gas chromatographic conditions have been optimized for the determination of hexanal in potato chips. Under optimized conditions, the quality parameters of the prepared technique have been determined. The suggested technique was applied for the determination of hexanal in potato chips and other fat-rich food.

Keywords: deep eutectic solvents, headspace gas chromatography, hexanal, microwave assisted extraction

Procedia PDF Downloads 160

Authors: Mohamed H. Sorour, Hayam F. Shaalan, Heba A. Hani, Eman S. Sayed, Amany A. El-Mansoup

Abstract:

Heavy metals (HMs) present an increasing threat to aquatic and soil environment. Thus, techniques should be developed for the removal and/or recovery of those HMs from point sources in the generating industries. This paper reports our endeavors concerning the development of in-house developed weak cation exchange polyacrylate hydrogel kaolin composites for heavy metals removal. This type of composite enables desirable characteristics and functions including mechanical strength, bed porosity and cost advantages. This paper emphasizes the effect of varying crosslinker (methylenebis(acrylamide)) concentration. The prepared cation exchanger has been subjected to intensive characterization using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), X-ray fluorescence (XRF) and Brunauer Emmett and Teller (BET) method. Moreover, the performance was investigated using synthetic and real wastewater for an industrial complex east of Cairo. Simulated and real wastewater compositions addressed; Cr, Co, Ni, and Pb are in the range of (92-115), (91-103), (86-88) and (99-125), respectively. Adsorption experiments have been conducted in both batch and column modes. In general, batch tests revealed enhanced cation exchange capacities of 70, 72, 78.2 and 99.9 mg/g from single synthetic wastes while, removal efficiencies of 82.2, 86.4, 44.4 and 96% were obtained for Cr, Co, Ni and Pb, respectively from mixed synthetic wastes. It is concluded that the mixed synthetic and real wastewaters have lower adsorption capacities than single solutions. It is worth mentioned that Pb attained higher adsorption capacities with comparable results in all tested concentrations of synthetic and real wastewaters. Pilot scale experiments were also conducted for mixed synthetic waste in a fluidized bed column for 48 hour cycle time which revealed 86.4%, 58.5%, 66.8% and 96.9% removal efficiency for Cr, Co, Ni, and Pb, respectively with maximum regeneration was also conducted using saline and acid regenerants. Maximum regeneration efficiencies for the column studies higher than the batch ones about by about 30% to 60%. Studies are currently under way to enhance the regeneration efficiency to enable successful scaling up of the adsorption column.

Keywords: polyacrylate hydrogel kaolin, ultrasonic irradiation, heavy metals, adsorption and regeneration

Procedia PDF Downloads 98

Authors: S. B. Bhandare, K. S. Laddha

Abstract:

Podphyllum hexandrum belonging to family berberidaceae has gained attention in phytochemical and pharmacological research as it shows excellent anticancer activity and has been used in treatment of skin diseases, sunburns and radioprotection. Chemically it contains lignans and flavonoids such as kaempferol, quercetin and their glycosides. Objective: To isolate and identify Kaempferol and Quercetin from Podophyllum rhizome. Method: The powdered rhizome of Podophyllum hexandrum was subjected to soxhlet extraction with methanol. This methanolic extract is used to obtain podophyllin. Podohyllin was extracted with ethyl acetate and this extract was then concentrated and subjected to column chromatography to obtain purified kaempferol and quercetin. Result: Isolated kaempferol, quercetin were light yellow and dark yellow in colour respectively. TLC of the isolated compounds was performed using chloroform: methanol (9:1) which showed single band on silica plate at Rf 0.6 and 0.4 for kaempferol and quercetin. UV spectrometric studies showed UV maxima (methanol) at 259, 360 nm and 260, 370 nm which are identical with standard kaempferol and quercetin respectively. Both IR spectra exhibited prominent absorption bands for free phenolic OH at 3277 and 3296.2 cm-1 and for conjugated C=O at 1597 and 1659.7 cm-1 respectively. The mass spectrum of kaempferol and quercetin showed (M+1) peak at m/z 287 and 303.09 respectively. 1H NMR analysis of both isolated compounds exhibited typical four-peak pattern of two doublets at δ 6.86 and δ 8.01 which was assigned to H-3’,5’ and H-2’,6’ respectively. Absence of signals less than δ 6.81 in the 1H NMR spectrum supported the aromatic nature of compound. Kaempferol and Quercetin showed 98.1% and 97% purity by HPLC at UV 370 nm. Conclusion: Easy and simple method for isolation of Kaempferol and Quercetin was developed and their structures were confirmed by UV, IR, NMR and mass studies. Method has shown good reproducibility, yield and purity.

Keywords: flavonoids, kaempferol, podophyllum rhizome, quercetin

Procedia PDF Downloads 283

Authors: Luke Andrighetto, Paul G. Stevenson, Luke C. Henderson, Jim Pearson, Xavier A. Conlan

Abstract:

As pseudoephedrine, a common ingredient in cold and flu medications is closely monitored and restricted in Australia, alternative methods of accessing it are of interest. The impurities and by-products of every reaction step of pseudoephedrine/ephedrine and methamphetamine synthesis have been mapped in order to develop a chemical fingerprint based on synthetic route. Likewise, seized methamphetamine contains a combination of different cutting agents and starting materials. Therefore, in-silico optimised two-dimensional HPLC with DryLab® and OpenMS® software has been used to efficiently separate complex seizure samples. An excellent match between simulated and real separations was observed. Targeted separation of model compounds was completed with significantly reduced method development time. This study produced a two-dimensional separation regime that offers unprecedented separation power (separation space) while maintaining a rapid analysis time that is faster than those previously reported for gas chromatography, single dimension high performance liquid chromatography or capillary electrophoresis.

Keywords: chemical fingerprint, ephedrine, methamphetamine, two-dimensional HPLC

Procedia PDF Downloads 439

Authors: Baki Cicek, Umit Calisir

Abstract:

Carbazoles have been replaced lots of studies from 1960's to present and also still continues. In 1987, the first diode device had been developed. Thanks to that study, light emitting devices have been investigated and developed and also have been used on commercial applications. Nowadays, OLED (Organic Light Emitting Diodes) technology is using on lots of electronic screen such as (mobile phone, computer monitors, televisions, etc.) Carbazoles were subject a lot of study as a semiconductor material. Although this technology is used commen and widely, it is still development stage. Metal complexes of these compounds are using at pigment dyes because of colored substances, polymer technology, medicine industry, agriculture area, preparing rocket fuel-oil, determine some of biological events, etc. Becides all of these to preparing of schiff base synthesis is going on intensely. In this study, some of novel carbazole schiff bases were synthesized starting from carbazole. For that purpose, firstly, carbazole was alkylated. After purification of N-substituted-carbazole was nitrated to sythesized 3-nitro-N-substituted and 3,6-dinitro-N-substituted carbazoles. At next step, nitro group/groups were reduced to amines. Purified with using a type of silica gel-column chromatography. At the last step of our study, with sythesized 3,6-diamino-N-substituted carbazoles and 3-amino-N-substituted carbazoles were reacted with aldehydes to condensation reactions. 3-(imino-p-hydroxybenzyl)-N-isobutyl -carbazole, 3-(imino-2,3,4-trimethoxybenzene)-N-butylcarbazole, 3-(imino-3,4-dihydroxybenzene)-N-octylcarbazole, 3-(imino-2,3-dihydroxybenzene)-N-octylkarbazole and 3,6-di(α-imino-β-naphthol) -N-hexylcarbazole compounds were synthesized. All of synthesized compounds were characterized with FT-IR, 1H-NMR, 13C-NMR, and LC-MS.

Keywords: carbazole, carbazol schiff base, condensation reactions, OLED

Procedia PDF Downloads 418

Authors: R. F. Vieira, S. A. Figueiredo, O. M. Freitas, V. F. Domingues, C. Delerue-Matos

Abstract:

The presence of sulphur compounds like hydrogen sulphide and mercaptans is one of the reasons for waste-water treatment and waste management being associated with odour emissions. In this context having a quantifying method for these compounds helps in the optimization of treatment with the goal of their elimination, namely biofiltration processes. The aim of this study was the development of a method for quantification of odorous gases in waste treatment plants air samples. A method based on head space solid phase microextraction (HS-SPME) coupled with gas chromatography - flame photometric detector (GC-FPD) was used to analyse H2S and Metil Mercaptan (MM). The extraction was carried out with a 75-μm Carboxen-polydimethylsiloxane fiber coating at 22 ºC for 20 min, and analysed by a GC 2010 Plus A from Shimadzu with a sulphur filter detector: splitless mode (0.3 min), the column temperature program was from 60 ºC, increased by 15 ºC/min to 100 ºC (2 min). The injector temperature was held at 250 ºC, and the detector at 260 ºC. For calibration curve a gas diluter equipment (digital Hovagas G2 - Multi Component Gas Mixer) was used to do the standards. This unit had two input connections, one for a stream of the dilute gas and another for a stream of nitrogen and an output connected to a glass bulb. A 40 ppm H2S and a 50 ppm MM cylinders were used. The equipment was programmed to the selected concentration, and it automatically carried out the dilution to the glass bulb. The mixture was left flowing through the glass bulb for 5 min and then the extremities were closed. This method allowed the calibration between 1-20 ppm for H2S and 0.02-0.1 ppm and 1-3.5 ppm for MM. Several quantifications of air samples from inlet and outlet of a biofilter operating in a waste management facility in the north of Portugal allowed the evaluation the biofilters performance.

Keywords: biofiltration, hydrogen sulphide, mercaptans, quantification

Procedia PDF Downloads 449

Authors: Hanifeh Imanian, Morteza Kolahdoozan

Abstract:

The purpose of this study is to present a mathematical phrase for calculating the dispersion rate of spilled oil in water column under non-breaking waves. In this regard, a multiphase numerical model is applied for which waves and oil phase were computed concurrently, and accuracy of its hydraulic calculations have been proven. More than 200 various scenarios of oil spilling in wave waters were simulated using the multiphase numerical model and its outcome were collected in a database. The recorded results were investigated to identify the major parameters affected vertical oil dispersion and finally 6 parameters were identified as main independent factors. Furthermore, some statistical tests were conducted to identify any relationship between the dependent variable (dispersed oil mass in the water column) and independent variables (water wave specifications containing height, length and wave period and spilled oil characteristics including density, viscosity and spilled oil mass). Finally, a mathematical-statistical relationship is proposed to predict dispersed oil in marine waters. To verify the proposed relationship, a laboratory example available in the literature was selected. Oil mass rate penetrated in water body computed by statistical regression was in accordance with experimental data was predicted. On this occasion, it was necessary to verify the proposed mathematical phrase. In a selected laboratory case available in the literature, mass oil rate penetrated in water body computed by suggested regression. Results showed good agreement with experimental data. The validated mathematical-statistical phrase is a useful tool for oil dispersion prediction in oil spill events in marine areas.

Keywords: dispersion, marine environment, mathematical-statistical relationship, oil spill

Procedia PDF Downloads 213

Authors: Precious Ehiomogue, Ifechukwude Israel Ahuchaogu, Isiguzo Edwin Ahaneku

Abstract:

Vermicompost is the product of the decomposition process using various species of worms, to create a mixture of decomposing vegetable or food waste, bedding materials, and vemicast. This process is called vermicomposting, while the rearing of worms for this purpose is called vermiculture. Several works have verified the adsorption of toxic metals using vermicompost but the application is still scarce for the retention of organic compounds. This research brings to knowledge the effectiveness of earthworm waste (vermicompost) for the remediation of crude oil contaminated soils. The remediation methods adopted in this study were two soil washing methods namely, batch and column process which represent laboratory and in-situ remediation. Characterization of the vermicompost and crude oil contaminated soil were performed before and after the soil washing using Fourier transform infrared (FTIR), scanning electron microscopy (SEM), X-ray fluorescence (XRF), X-ray diffraction (XRD) and Atomic adsorption spectrometry (AAS). The optimization of washing parameters, using response surface methodology (RSM) based on Box-Behnken Design was performed on the response from the laboratory experimental results. This study also investigated the application of machine learning models [Artificial neural network (ANN), Adaptive neuro fuzzy inference system (ANFIS). ANN and ANFIS were evaluated using the coefficient of determination (R²) and mean square error (MSE)]. Removal efficiency obtained from the Box-Behnken design experiment ranged from 29% to 98.9% for batch process remediation. Optimization of the experimental factors carried out using numerical optimization techniques by applying desirability function method of the response surface methodology (RSM) produce the highest removal efficiency of 98.9% at absorbent dosage of 34.53 grams, adsorbate concentration of 69.11 (g/ml), contact time of 25.96 (min), and pH value of 7.71, respectively. Removal efficiency obtained from the multilevel general factorial design experiment ranged from 56% to 92% for column process remediation. The coefficient of determination (R²) for ANN was (0.9974) and (0.9852) for batch and column process, respectively, showing the agreement between experimental and predicted results. For batch and column precess, respectively, the coefficient of determination (R²) for RSM was (0.9712) and (0.9614), which also demonstrates agreement between experimental and projected findings. For the batch and column processes, the ANFIS coefficient of determination was (0.7115) and (0.9978), respectively. It can be concluded that machine learning models can predict the removal of crude oil from polluted soil using vermicompost. Therefore, it is recommended to use machines learning models to predict the removal of crude oil from contaminated soil using vermicompost.

Keywords: ANFIS, ANN, crude-oil, contaminated soil, remediation and vermicompost

Procedia PDF Downloads 68

Authors: Mohammadreza Akbari, Pooya Soleimani Besheli, Reza Khalili, Sara Akbari

Abstract:

In this study, we investigate building structures nonlinear behavior also solving analytic of nonlinear differential at vibrations. As we know most of engineering systems behavior in practical are non- linear process (especial at structural) and analytical solving (no numerical) these problems are complex, difficult and sometimes impossible (of course at form of analytical solving). In this symposium, we are going to exposure one method in engineering, that can solve sets of nonlinear differential equations with high accuracy and simple solution and so this issue will emerge after comparing the achieved solutions by Numerical Method (Runge-Kutte 4th) and exact solutions. Finally, we can proof AGM method could be created huge evolution for researcher and student (engineering and basic science) in whole over the world, because of AGM coding system, so by using this software, we can analytical solve all complicated linear and nonlinear differential equations, with help of that there is no difficulty for solving nonlinear differential equations.

Keywords: new method AGM, vibrations, beam-column, angular frequency, energy dissipated, critical load

Procedia PDF Downloads 358

Authors: Lian Song, Shao-Bo Kang, Bo Yang

Abstract:

Concrete filled steel tubular (CFST) structure has been widely used in construction practices due to its superior performances under various loading conditions. However, limited studies are available when this type of structure is subjected to impact or explosive loads. Current methods in relevant design codes are not specific for preventing progressive collapse of CFST structures. Therefore, it is necessary to carry out numerical simulations on CFST structure under impact loads. In this study, finite element analyses are conducted on the mechanical behaviour of composite frames which composed of CFST columns and steel beams subject to impact loading. In the model, CFST columns are simulated using finite element software ABAQUS. The model is verified by test results of solid and hollow CFST columns under lateral impacts, and reasonably good agreement is obtained through comparisons. Thereafter, a multi-scale finite element modelling technique is developed to evaluate the behaviour of a five-storey three-span planar composite frame. Alternate path method and direct simulation method are adopted to perform the dynamic response of the frame when a supporting column is removed suddenly. In the former method, the reason for column removal is not considered and only the remaining frame is simulated, whereas in the latter, a specific impact load is applied to the frame to take account of the column failure induced by vehicle impact. Comparisons are made between these two methods in terms of displacement history and internal force redistribution, and design recommendations are provided for the design of CFST structures under impact loads.

Keywords: planar composite frame, collapse analysis, impact loading, direct simulation method, alternate path method

Procedia PDF Downloads 493

Authors: Li Feng, Cheng Zhang, Chuanzhou Yuang

Abstract:

Understanding the macromolecular structure of low-rank coal is very important for its gasification and liquefaction. The pyrolysis is one of the methods of analyzing the macromolecular structure of coal. The gaseous products decomposed directly by the raw lignite at 500 °C and indirectly by tar products from raw lignite pyrolysis at 500 °C were investigated and compared by thermogravimetry, gas chromatography and mass spectrum coupled instrument system (TG/GC/MS) in this paper. The results show that 52 kinds of products were found from the raw lignite and 70 kinds of products from the tar. The pyrolysis products directly from the lignite appear more monocyclic aromatic hydrocarbons and less substituent groups or branch chain, compared with the products from the tar. There is less linear chain and double bonds structure in the tar, which can be speculated that linear chain and double bonds structure took part in the generation of condensed rings and other reactions. There are more kinds of phenol and furan in the tar, which indicate that these products may be generated from the secondary reaction. The formation process of phenol, phenol naphthalene, naphthene and furan are discussed.

Keywords: composition and structure, lignite, pyrolysis of coal, tar, TG/GC/MS

Procedia PDF Downloads 118

Authors: JinWoog Lee, SeongHyeok Lee, ChanYong Choi, Yujin Lim, Hojin Cho

Abstract:

Primary function of the trackbed in a conventional railway track system is to decrease the stresses in the subgrade to be in an acceptable level. A properly designed trackbed layer performs this task adequately. Many design procedures have used assumed and/or are based on critical stiffness values of the layers obtained mostly in the field to calculate an appropriate thickness of the sublayers of the trackbed foundation. However, those stiffness values do not consider strain levels clearly and precisely in the layers. This study proposes a method of computation of stiffness that can handle with strain level in the layers of the trackbed foundation in order to provide properly selected design values of the stiffness of the layers. The shear modulus values are dependent on shear strain level so that the strain levels generated in the subgrade in the trackbed under wheel loading and below plate of Repeated Plate Bearing Test (RPBT) are investigated by finite element analysis program ABAQUS and PLAXIS programs. The strain levels generated in the subgrade from RPBT are compared to those values from RC (Resonant Column) test after some consideration of strain levels and stress consideration. For comparison of shear modulus G obtained from RC test and stiffness moduli Ev2 obtained from RPBT in the field, many numbers of mid-size RC tests in laboratory and RPBT in field were performed extensively. It was found in this study that there is a big difference in stiffness modulus when the converted Ev2 values were compared to those values of RC test. It is verified in this study that it is necessary to use precise and increased loading steps to construct nonlinear curves from RPBT in order to get correct Ev2 values in proper strain levels.

Keywords: modulus, plate load test, resonant column test, trackbed foundation

Procedia PDF Downloads 470

Authors: Mizam Doğan

Abstract:

Adapazarı railway car factory, the only railway car factory of Turkey, was constructed in 1950. It was a steel design and it had filled beam sections and truss beam systems. Columns were steel profiles and box sections. The factory was damaged heavily on Izmit Earthquake and closed. In this earthquake 90% of damaged structures are reinforced concrete, the others are %7 prefabricated and 3% steel construction. As can be seen in statistical data, damaged industrial buildings in this earthquake were generally reinforced concrete and prefabricated structures. Adapazari railway car factory is the greatest steel structure damaged in the earthquake. This factory has 95% of the total damaged steel structure area. In this paper; earthquake damages on beams and columns of the factory are studied by considering TS648 'Turkish Standard Building Code for Steel Structures' and also damaged connection elements as welds, rivets and bolts are examined. A model similar to the damaged system is made and high-stress zones are searched. These examinations, conclusions, suggestions are explained by damage photos and details.

Keywords: column-beam connection, seismic analysis, seismic load, steel structure

Procedia PDF Downloads 251

Authors: Eman M. Morgan, Hayam M. Lotfy, Yasmin M. Fayez, Mohamed Abdelkawy, Engy Shokry

Abstract:

Two simple, selective, economic, safe, accurate, precise and environmentally friendly methods were developed and validated for the quantitative determination of valaciclovir (VAL) in the presence of its related substances R1 (acyclovir), R2 (guanine) in bulk powder and in the commercial pharmaceutical product containing the drug. Method A is a colorimetric method where VAL selectively reacts with ferric hydroxamate and the developed color was measured at 490 nm over a concentration range of 0.4-2 mg/mL with percentage recovery 100.05 ± 0.58 and correlation coefficient 0.9999. Method B is a reversed phase ultra performance liquid chromatographic technique (UPLC) which is considered superior in technology to the high-performance liquid chromatography with respect to speed, resolution, solvent consumption, time, and cost of analysis. Efficient separation was achieved on Agilent Zorbax CN column using ammonium acetate (0.1%) and acetonitrile as a mobile phase in a linear gradient program. Elution time for the separation was less than 5 min and ultraviolet detection was carried out at 256 nm over a concentration range of 2-50 μg/mL with mean percentage recovery 100.11±0.55 and correlation coefficient 0.9999. The proposed methods were fully validated as per International Conference on Harmonization specifications and effectively applied for the analysis of valaciclovir in pure form and tablets dosage form. Statistical comparison of the results obtained by the proposed and official or reported methods revealed no significant difference in the performance of these methods regarding the accuracy and precision respectively.

Keywords: hydroxamic acid, related substances, UPLC, valaciclovir

Procedia PDF Downloads 223