Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 175

Search results for: desorption

175 Thermal Technologies Applications for Soil Remediation

Authors: A. de Folly d’Auris, R. Bagatin, P. Filtri


This paper discusses the importance of having a good initial characterization of soil samples when thermal desorption has to be applied to polluted soils for the removal of contaminants. Particular attention has to be devoted on the desorption kinetics of the samples to identify the gases evolved during the heating, and contaminant degradation pathways. In this study, two samples coming from different points of the same contaminated site were considered. The samples are much different from each other. Moreover, the presence of high initial quantity of heavy hydrocarbons strongly affected the performance of thermal desorption, resulting in formation of dangerous intermediates. Analytical techniques such TGA (Thermogravimetric Analysis), DSC (Differential Scanning Calorimetry) and GC-MS (Gas Chromatography-Mass) provided a good support to give correct indication for field application.

Keywords: desorption kinetics, hydrocarbons, thermal desorption, thermogravimetric measurements

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174 Identification and Quantification of Acid Sites of M(X)X Zeolites (M= Cu2+ and/or Zn2+,X = Level of Exchange): An In situ FTIR Study Using Pyridine Adsorption/Desorption

Authors: H. Hammoudi, S. Bendenia, I. Batonneau-Gener, J. Comparot, K. Marouf-Khelifa, A. Khelifa


X zeolites were prepared by ion-exchange with Cu2+ and/or Zn2+ cations, at different concentrations of the exchange solution, and characterised by thermal analysis and nitrogen adsorption. The acidity of the samples was investigated by pyridine adsorption–desorption followed by in situ Fourier transform infrared (FTIR) spectroscopy. Desorption was carried out at 150, 250 and 350 °C. The objective is to estimate the nature and concentration of acid sites. A comparison between the binary (Cu(x)X, Zn(x)X) and ternary (CuZn(x)X) exchanges was also established (x = level of exchange) through the Cu(43)X, Zn(48)X and CuZn(50)X samples. Lewis acidity decreases overall with desorption temperature and the level of exchange. As the latter increases, there is a conversion of some Lewis sites into those of Brønsted during thermal treatment. In return, the concentration of Brønsted sites increases with the degree of exchange. The Brønsted acidity of CuZn(50)X at 350 °C is more important than the sum of those of Cu(43)X and Zn(48)X. The found values were 73, 32 and 15 μmol g-1, respectively. Besides, the concentration of Brønsted sites for CuZn(50)X increases with desorption temperature. These features indicate the presence of a synergistic effect amplifying the strength of these sites when Cu2+ and Zn2+ cations compete for the occupancy of sites distributed inside zeolitic cavities.

Keywords: acidity, adsorption, pyridine, zeolites

Procedia PDF Downloads 151
173 Degradation of Hydrocarbons by Surfactants and Biosurfactants

Authors: Samira Ferhat, Redha Alouaoui, Leila Trifi, Abdelmalek Badis


The objective of this work is the use of natural surfactant (biosurfactant) and synthetic (sodium dodecyl sulfate and tween 80) for environmental application. In fact the solubility of the polycyclic hydrocarbon (naphthalene) and the desorption of the heavy metals in the presence of surfactants. The microorganisms selected in this work are bacterial strain (Bacillus licheniformis) for the production of biosurfactant for use in this study. In the first part of this study, we evaluated the effectiveness of surfactants solubilization certain hydrocarbons few soluble in water such as polyaromatic (case naphthalene). Tests have shown that from the critical micelle concentration, decontamination is performed. The second part presents the results on the desorption of heavy metals (for copper) by the three surfactants, using concentrations above the critical micelle concentration. The comparison between the desorption of copper by the three surfactants, it is shown that the biosurfactant is more effective than tween 80 and sodium dodecyl sulfate.

Keywords: surfactants, biosurfactant, naphthalene, copper, critical micelle concentration, solubilization, desorption

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172 Numerical Simulation of the Dynamic Behavior of a LaNi5 Water Pumping System

Authors: Miled Amel, Ben Maad Hatem, Askri Faouzi, Ben Nasrallah Sassi


Metal hydride water pumping system uses hydrogen as working fluid to pump water for low head and high discharge. The principal operation of this pump is based on the desorption of hydrogen at high pressure and its absorption at low pressure by a metal hydride. This work is devoted to study a concept of the dynamic behavior of a metal hydride pump using unsteady model and LaNi5 as hydriding alloy. This study shows that with MHP, it is possible to pump 340l/kg-cycle of water in 15 000s using 1 Kg of LaNi5 at a desorption temperature of 360 K, a pumping head equal to 5 m and a desorption gear ratio equal to 33. This study reveals also that the error given by the steady model, using LaNi5 is about 2%.A dimensional mathematical model and the governing equations of the pump were presented to predict the coupled heat and mass transfer within the MHP. Then, a numerical simulation is carried out to present the time evolution of the specific water discharge and to test the effect of different parameters (desorption temperature, absorption temperature, desorption gear ratio) on the performance of the water pumping system (specific water discharge, pumping efficiency and pumping time). In addition, a comparison between results obtained with steady and unsteady model is performed with different hydride mass. Finally, a geometric configuration of the reactor is simulated to optimize the pumping time.

Keywords: dynamic behavior, LaNi5, performance of water pumping system, unsteady model

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171 Alumina Generated by Electrocoagulation as Adsorbent for the Elimination of the Iron from Drilling Water

Authors: Aimad Oulebsir, Toufik Chaabane, Venkataraman Sivasankar, André Darchen, Titus A. M. Msagati


Currently, the presence of pharmaceutical substances in the environment is an emerging pollution leading to the disruption of ecosystems. Indeed, water loaded with pharmaceutical residues is an issue that has raised the attention of researchers. The aim of this study was to monitor the effectiveness of the alumina electro-generated by the adsorption process the iron of well water for the production of drugs. The Fe2+ was removed from wastewater by adsorption in a batch cell. Performance results of iron removal by alumina electro-generated revealed that the efficiency of the carrier in the method of electro-generated adsorption. The overall Fe2+ of the synthetically solutions and simulated effluent removal efficiencies reached 75% and 65%, respectively. The application of models and isothermal adsorption kinetics complement the results obtained experimentally. Desorption of iron was investigated using a solution of 0.1M NaOH. Regeneration of the tests shows that the adsorbent maintains its capacity after five adsorption/desorption cycles.

Keywords: electrocoagulation, aluminum electrode, electrogenerated alumina, iron, adsorption/desorption

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170 Study on the Thermal Conductivity about Porous Materials in Wet State

Authors: Han Yan, Jieren Luo, Qiuhui Yan, Xiaoqing Li


The thermal conductivity of porous materials is closely related to the thermal and moisture environment and the overall energy consumption of the building. The study of thermal conductivity of porous materials has great significance for the realization of low energy consumption building and economic construction building. Based on the study of effective thermal conductivity of porous materials at home and abroad, the thermal conductivity under a variety of different density of polystyrene board (EPS), plastic extruded board (XPS) and polyurethane (PU) and phenolic resin (PF) in wet state through theoretical analysis and experimental research has been studied. Initially, the moisture absorption and desorption properties of specimens had been discussed under different density, which led a result indicates the moisture absorption of four porous materials all have three stages, fast, stable and gentle. For the moisture desorption, there are two types. One is the existence of the rapid phase of the stage, such as XPS board, PU board. The other one does not have the fast desorption, instead, it is more stabilized, such as XPS board, PF board. Furthermore, the relationship between water content and thermal conductivity of porous materials had been studied and fitted, which figured out that in the wake of the increasing water content, the thermal conductivity of porous material is continually improving. At the same time, this result also shows, in different density, when the same kind of materials decreases, the saturated moisture content increases. Finally, the moisture absorption and desorption properties of the four kinds of materials are compared comprehensively, and it turned out that the heat preservation performance of PU board is the best, followed by EPS board, XPS board, PF board.

Keywords: porous materials, thermal conductivity, moisture content, transient hot-wire method

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169 A Step-by-Step Analytical Protocol For Detecting and Identifying Minor Differences In Like Materials and Polymers Using Pyrolysis -Gas Chromatography/Mass Spectrometry Technique

Authors: Athena Nguyen, Rojin Belganeh


Detecting and identifying differences in like polymer materials are key factors in failure and deformulation analysis, and reverse engineering. Pyrolysis-GC/MS is an easy solid sample introduction technique which expands the application areas of gas chromatography and mass spectrometry. The Micro furnace pyrolyzer is directly interfaced with the GC injector preventing any potential of cold spot, carryover, and cross contamination. In this presentation, the analysis of the differences in three polystyrene samples is demonstrated. Although the three samples look very similar by Evolve gas analysis (EGA) and Flash pyrolysis, there are indications of small levels of other materials. By performing Thermal desorption-GC/MS, the additive compounds between samples show the differences. EGA, flash pyrolysis, and thermal desorption analysis are the different modes of operations of the micro-furnace pyrolyzer enabling users to perform multiple analytical techniques.

Keywords: Gas chromatography/Mass spectrometry, pyrolysis, pyrolyzer, thermal desorption-GC/MS

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168 Basic One-Dimensional Modelica®-Model for Simulation of Gas-Phase Adsorber Dynamics

Authors: Adrian Rettig, Silvan Schneider, Reto Tamburini, Mirko Kleingries, Ulf Christian Muller


Industrial adsorption processes are, mainly due to si-multaneous heat and mass transfer, characterized by a high level of complexity. The conception of such processes often does not take place systematically; instead scale-up/down respectively number-up/down methods based on existing systems are used. This paper shows how Modelica® can be used to develop a transient model enabling a more systematic design of such ad- and desorption components and processes. The core of this model is a lumped-element submodel of a single adsorbent grain, where the thermodynamic equilibria and the kinetics of the ad- and desorption processes are implemented and solved on the basis of mass-, momentum and energy balances. For validation of this submodel, a fixed bed adsorber, whose characteristics are described in detail in the literature, was modeled and simulated. The simulation results are in good agreement with the experimental results from the literature. Therefore, the model development will be continued, and the extended model will be applied to further adsorber types like rotor adsorbers and moving bed adsorbers.

Keywords: adsorption, desorption, linear driving force, dynamic model, Modelica®, integral equation approach

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167 Determination of Brominated Flame Retardants In Recycled Plastic Toys Using Thermal Desorption GC/MS

Authors: Athena Nguyen, Rojin Belganeh


In recycling plastics industries, waste plastics are converted into monomers and other useful molecules by chemical reactions. Thermal energy generated by incineration is recovered when waste plastics melt. During the process, Flame retardants containing products get in, and brominated flame retardants (BFRs) are often used to reduce the flammability of products. Some of the originally formulated brominated flame retardants additives are restricted by the RoHS Directive, such as PBDE and PBB. The determination of BFRs other than those restricted by the RoHS directive is required. Frontier Lab developed a pyrolyzer based on the vertical micro-furnace design. The multi-mode pyrolyzer with different modes of operations, including evolve gas analysis (EGA), flash pyrolysis, thermal desorption, heart cutting, allows users to choose among the techniques for their analysis purposes. The method requires very little sample preparation. The first step is to perform an EGA using temperature programs. This technique provides information about the thermal temperature behaviors of the sample. The EGA thermogram is then used to determine the next steps in the analysis process. In this presentation, with an Optimal thermal temperature zone identified based on EGA thermogram, thermal desorption GC/MS is a chosen technique for the determination of brominated flame retardants in recycled plastic toys. Five types of general-purpose brominated flame retardants other than those restricted by the RoHS Directive are determined by the standard addition method.

Keywords: gas chromatography/mass spectrometry, pyrolysis, pyrolyzer, thermal desorption-GC/MS

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166 Efficient of Technology Remediation Soil That Contaminated by Petroleum Based on Heat without Combustion

Authors: Gavin Hutama Farandiarta, Hegi Adi Prabowo, Istiara Rizqillah Hanifah, Millati Hanifah Saprudin, Raden Iqrafia Ashna


The increase of the petroleum’s consumption rate encourages industries to optimize and increase the activity in processing crude oil into petroleum. However, although the result gives a lot of benefits to humans worldwide, it also gives negative impact to the environment. One of the negative impacts of processing crude oil is the soil will be contaminated by petroleum sewage sludge. This petroleum sewage sludge, contains hydrocarbon compound and it can be calculated by Total Petroleum Hydrocarbon (TPH).Petroleum sludge waste is accounted as hazardous and toxic. The soil contamination caused by the petroleum sludge is very hard to get rid of. However, there is a way to manage the soil that is contaminated by petroleum sludge, which is by using heat (thermal desorption) in the process of remediation. There are several factors that affect the success rate of the remediation with the help of heat which are temperature, time, and air pressure in the desorption column. The remediation process using the help of heat is an alternative in soil recovery from the petroleum pollution which highly effective, cheap, and environmentally friendly that produces uncontaminated soil and the petroleum that can be used again.

Keywords: petroleum sewage sludge, remediation soil, thermal desorption, total petroleum hydrocarbon (TPH)

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165 Effects of Polymer Adsorption and Desorption on Polymer Flooding in Waterflooded Reservoir

Authors: Sukruthai Sapniwat, Falan Srisuriyachai


Polymer Flooding is one of the most well-known methods in Enhanced Oil Recovery (EOR) technology which can be implemented after either primary or secondary recovery, resulting in favorable conditions for the displacement mechanism in order to lower the residual oil in the reservoir. Polymer substances can lower the mobility ratio of the whole process by increasing the viscosity of injected water. Therefore, polymer flooding can increase volumetric sweep efficiency, which leads to a better recovery factor. Moreover, polymer adsorption onto rock surface can help decrease reservoir permeability contrast with high heterogeneity. Due to the reduction of the absolute permeability, effective permeability to water, representing flow ability of the injected fluid, is also reduced. Once polymer is adsorbed onto rock surface, polymer molecule can be desorbed when different fluids are injected. This study is performed to evaluate the effects of the adsorption and desorption process of polymer solutions to yield benefits on the oil recovery mechanism. A reservoir model is constructed by reservoir simulation program called STAR® commercialized by the Computer Modeling Group (CMG). Various polymer concentrations, starting times of polymer flooding process and polymer injection rates were evaluated with selected values of polymer desorption degrees including 0, 25, 50, 75 and 100%. The higher the value, the more adsorbed polymer molecules to return back to flowing fluid. According to the results, polymer desorption lowers polymer consumption, especially at low concentrations. Furthermore, starting time of polymer flooding and injection rate affect the oil production. The results show that waterflooding followed by earlier polymer flooding can increase the oil recovery factor while the higher injection rate also enhances the recovery. Polymer concentration is related to polymer consumption due to the two main benefits of polymer flooding control described above. Therefore, polymer slug size should be optimized based on polymer concentration. Polymer desorption causes polymer re-employment that is previously adsorbed onto rock surface, resulting in an increase of sweep efficiency in the further period of polymer flooding process. Even though waterflooding supports polymer injectivity, water cut at the producer can prematurely terminate the oil production. The injection rate decreases polymer adsorption due to decreased retention time of polymer flooding process.

Keywords: enhanced oil recovery technology, polymer adsorption and desorption, polymer flooding, reservoir simulation

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164 Synthesis of Nanoparticle Mordenite Zeolite for Dimethyl Ether Carbonylation

Authors: Zhang Haitao


The different size of nanoparticle mordenite zeolites were prepared by adding different soft template during hydrothermal process for carbonylation of dimethyl ether (DME) to methyl acetate (MA). The catalysts were characterized by X-ray diffraction, Ar adsorption-desorption, high-resolution transmission electron microscopy, NH3-temperature programmed desorption, scanning electron microscopy and Thermogravimetric. The characterization results confirmed that mordenite zeolites with small nanoparticle showed more strong acid sites which was the active site for carbonylation thus promoting conversion of DME and MA selectivity. Furthermore, the nanoparticle mordenite had increased the mass transfer efficiency which could suppress the formation of coke.

Keywords: nanoparticle mordenite, carbonylation, dimethyl ether, methyl acetate

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163 Deformulation and Comparative Analysis of Apparently Similar Polymers Using Multiple Modes of Pyrolysis-Gc/Ms

Authors: Athena Nguyen, Rojin Belganeh


Detecting and identifying differences in like polymer materials are key factors in deformulation, comparative analysis as well as reverse engineering. Pyrolysis-GC/MS is an easy solid sample introduction technique which expands the application areas of gas chromatography and mass spectrometry. The Micro-furnace pyrolyzer is directly interfaced with the GC injector preventing any potential of cold spot, carryover, and cross contamination. This presentation demonstrates the study of two similar polymers by performing different mode of operations in the same system: Evolve gas analysis (EGA), Flash pyrolysis, Thermal desorption analysis, and Heart-cutting analysis. Unknown polymer materials and their chemical compositions are identified.

Keywords: gas chromatography/mass spectrometry, pyrolysis, pyrolyzer, thermal desorption-GC/MS

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162 A Plasmonic Mass Spectrometry Approach for Detection of Small Nutrients and Toxins

Authors: Haiyang Su, Kun Qian


We developed a novel plasmonic matrix assisted laser desorption/ionization mass spectrometry (MALDI MS) approach to detect small nutrients and toxin in complex biological emulsion samples. We used silver nanoshells (SiO₂@Ag) with optimized structures as matrices and achieved direct analysis of ~6 nL of human breast milk without any enrichment or separation. We performed identification and quantitation of small nutrients and toxins with limit-of-detection down to 0.4 pmol (for melamine) and reaction time shortened to minutes, superior to the conventional biochemical methods currently in use. Our approach contributed to the near-future application of MALDI MS in a broad field and personalized design of plasmonic materials for real case bio-analysis.

Keywords: plasmonic materials, laser desorption/ionization, mass spectrometry, small nutrients, toxins

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161 Morphological Characterization and Gas Permeation of Commercially Available Alumina Membrane

Authors: Ifeyinwa Orakwe, Ngozi Nwogu, Edward Gobina


This work presents experimental results relating to the structural characterization of a commercially available alumina membrane. A γ-alumina mesoporous tubular membrane has been used. Nitrogen adsorption-desorption, scanning electron microscopy and gas permeability test has been carried out on the alumina membrane to characterize its structural features. Scanning electron microscopy (SEM) was used to determine the pore size distribution of the membrane. Pore size, specific surface area and pore size distribution were also determined with the use of the Nitrogen adsorption-desorption instrument. Gas permeation tests were carried out on the membrane using a variety of single and mixed gases. The permeabilities at different pressure between 0.05-1 bar and temperature range of 25-200oC were used for the single and mixed gases: nitrogen (N2), helium (He), oxygen (O2), carbon dioxide (CO2), 14%CO₂/N₂, 60%CO₂/N₂, 30%CO₂/CH4 and 21%O₂/N₂. Plots of flow rate verses pressure were obtained. Results got showed the effect of temperature on the permeation rate of the various gases. At 0.5 bar for example, the flow rate for N2 was relatively constant before decreasing with an increase in temperature, while for O2, it continuously decreased with an increase in temperature. In the case of 30%CO₂/CH4 and 14%CO₂/N₂, the flow rate showed an increase then a decrease with increase in temperature. The effect of temperature on the membrane performance of the various gases is presented and the influence of the trans membrane pressure drop will be discussed in this paper.

Keywords: alumina membrane, Nitrogen adsorption-desorption, scanning electron microscopy, gas permeation, temperature

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160 Waste Derived from Refinery and Petrochemical Plants Activities: Processing of Oil Sludge through Thermal Desorption

Authors: Anna Bohers, Emília Hroncová, Juraj Ladomerský


Oil sludge with its main characteristic of high acidity is a waste product generated from the operation of refinery and petrochemical plants. Former refinery and petrochemical plant - Petrochema Dubová is present in Slovakia as well. Its activities was to process the crude oil through sulfonation and adsorption technology for production of lubricating and special oils, synthetic detergents and special white oils for cosmetic and medical purposes. Seventy years ago – period, when this historical acid sludge burden has been created – comparing to the environmental awareness the production was in preference. That is the reason why, as in many countries, also in Slovakia a historical environmental burden is present until now – 229 211 m3 of oil sludge in the middle of the National Park of Nízke Tatry mountain chain. Neither one of tried treatment methods – bio or non-biologic one - was proved as suitable for processing or for recovery in the reason of different factors admission: i.e. strong aggressivity, difficulty with handling because of its sludgy and liquid state et sim. As a potential solution, also incineration was tested, but it was not proven as a suitable method, as the concentration of SO2 in combustion gases was too high, and it was not possible to decrease it under the acceptable value of 2000 That is the reason why the operation of incineration plant has been terminated, and the acid sludge landfills are present until nowadays. The objective of this paper is to present a new possibility of processing and valorization of acid sludgy-waste. The processing of oil sludge was performed through the effective separation - thermal desorption technology, through which it is possible to split the sludgy material into the matrix (soil, sediments) and organic contaminants. In order to boost the efficiency in the processing of acid sludge through thermal desorption, the work will present the possibility of application of an original technology – Method of Blowing Decomposition for recovering of organic matter into technological lubricating oil.

Keywords: hazardous waste, oil sludge, remediation, thermal desorption

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159 Removal Efficiency of Some Heavy Metals from Aqueous Solution on Magnetic Nanoparticles

Authors: Gehan El-Sayed Sharaf El-Deen


In this study, super paramagnetic iron-oxide nano- materials (SPMIN) were investigated for removal of toxic heavy metals from aqueous solution. The magnetic nanoparticles of 12 nm were synthesized using a co-precipitation method and characterized by transmission electron microscopy (TEM), transform infrared spectroscopy (FTIR), x-ray diffraction (XRD) and vibrating sample magnetometer (VSM). Batch experiments carried out to investigate the influence of different parameters such as contact time, initial concentration of metal ions, the dosage of SPMIN, desorption,pH value of solutions. The adsorption process was found to be highly pH dependent, which made the nanoparticles selectively adsorb these three metals from wastewater. Maximum sorption for all the studies cations obtained at the first half hour and reached equilibrium at one hour. The adsorption data of heavy metals studied were well fitted with the Langmuir isotherm and the equilibrium data show the percent removal of Ni2+, Zn2+ and Cd2+ were 96.5%, 80% and 75%, respectively. Desorption studies in acidic medium indicate that Zn2+, Ni2+ and Cd2+ were removed by 89%, 2% and 18% from the first cycle. Regeneration studies indicated that SPMIN nanoparticles undergoing successive adsorption–desorption processes for Zn2+ ions retained original metal removal capacity. The results revealed that the most prominent advantage of the prepared SPMIN adsorbent consisted in their separation convenience compared to the other adsorbents and SPMIN has high efficiency for removal the investigated metals from aqueous solution.

Keywords: heavy metals, magnetic nanoparticles, removal efficiency, Batch technique

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158 Improvement in Ni (II) Adsorption Capacity by Using Fe-Nano Zeolite

Authors: Pham-Thi Huong, Byeong-Kyu Lee, Jitae Kim, Chi-Hyeon Lee


Fe-nano zeolite adsorbent was used for removal of Ni (II) ions from aqueous solution. The adsorbent was characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and the surface area Brunauer–Emmett–Teller (BET) using for analysis of functional groups, morphology and surface area. Bath adsorption experiments were analyzed on the effect of pH, time, adsorbent doses and initial Ni (II) concentration. The optimum pH for Ni (II) removal using Fe-nano zeolite was found at 5.0 and 90 min of reaction time. The maximum adsorption capacity of Ni (II) was 231.68 mg/g based on the Langmuir isotherm. The kinetics data for the adsorption process was fitted with the pseudo-second-order model. The desorption of Ni (II) from Ni-loaded Fe-nano zeolite was analyzed and even after 10 cycles 72 % desorption was achieved. These finding supported that Fe-nano zeolite with high adsorption capacity, high reuse ability would be utilized for Ni (II) removal from water.

Keywords: Fe-nano zeolite, adsorption, Ni (II) removal, regeneration

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157 Body Fluids Identification by Raman Spectroscopy and Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

Authors: Huixia Shi, Can Hu, Jun Zhu, Hongling Guo, Haiyan Li, Hongyan Du


The identification of human body fluids during forensic investigations is a critical step to determine key details, and present strong evidence to testify criminal in a case. With the popularity of DNA and improved detection technology, the potential question must be revolved that whether the suspect’s DNA derived from saliva or semen, menstrual or peripheral blood, how to identify the red substance or aged blood traces on the spot is blood; How to determine who contribute the right one in mixed stains. In recent years, molecular approaches have been developing increasingly on mRNA, miRNA, DNA methylation and microbial markers, but appear expensive, time-consuming, and destructive disadvantages. Physicochemical methods are utilized frequently such us scanning electron microscopy/energy spectroscopy and X-ray fluorescence and so on, but results only showing one or two characteristics of body fluid itself and that out of working in unknown or mixed body fluid stains. This paper focuses on using chemistry methods Raman spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry to discriminate species of peripheral blood, menstrual blood, semen, saliva, vaginal secretions, urine or sweat. Firstly, non-destructive, confirmatory, convenient and fast Raman spectroscopy method combined with more accurate matrix-assisted laser desorption/ionization time-of-flight mass spectrometry method can totally distinguish one from other body fluids. Secondly, 11 spectral signatures and specific metabolic molecules have been obtained by analysis results after 70 samples detected. Thirdly, Raman results showed peripheral and menstrual blood, saliva and vaginal have highly similar spectroscopic features. Advanced statistical analysis of the multiple Raman spectra must be requested to classify one to another. On the other hand, it seems that the lactic acid can differentiate peripheral and menstrual blood detected by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, but that is not a specific metabolic molecule, more sensitivity ones will be analyzed in a forward study. These results demonstrate the great potential of the developed chemistry methods for forensic applications, although more work is needed for method validation.

Keywords: body fluids, identification, Raman spectroscopy, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

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156 Thermal Regeneration of CO2 Spent Palm Shell-Polyetheretherketone Activated Carbon Sorbents

Authors: Usman D. Hamza, Noor S. Nasri, Mohammed Jibril, Husna M. Zain


Activated carbons (M4P0, M4P2, and M5P2) used in this research were produced from palm shell and polyetherether ketone (PEEK) via carbonization, impregnation, and microwave activation. The adsorption/desorption process was carried out using static volumetric adsorption. Regeneration is important in the overall economy of the process and waste minimization. This work focuses on the thermal regeneration of the CO2 exhausted microwave activated carbons. The regeneration strategy adopted was thermal with nitrogen purge desorption with N2 feed flow rate of 20 ml/min for 1 h at atmospheric pressure followed by drying at 1500C. Seven successive adsorption/regeneration processes were carried out on the material. It was found that after seven adsorption regeneration cycles; the regeneration efficiency (RE) for CO2 activated carbon from palm shell only (M4P0) was more than 90% while that of hybrid palm shell-PEEK (M4P2, M5P2) was above 95%. The cyclic adsorption and regeneration shows the stability of the adsorbent materials.

Keywords: activated carbon, palm shell-PEEK, regeneration, thermal

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155 The Performance of PtSn/Al₂O₃ with Cylindrical Particles for Acetic Acid Hydrogenation

Authors: Mingchuan Zhou, Haitao Zhang, Hongfang Ma, Weiyong Ying


Alumina supported PtSn catalysts with cylindrical particles were prepared and characterized by using low temperature N2 adsorption/desorption and X-ray diffraction. Low temperature N2 adsorption/desorption demonstrate that the tableting changed the texture properties of catalysts. XRD pattern indicate that the crystal structure of supports had no change after reaction. The performances over particles of PtSn/Al2O3 catalysts were investigated with regards to reaction temperature, pressure, and H2/AcOH mole ratio. After tableting, the conversion of acetic acid and selectivity of ethanol and acetyl acetate decreased. High reaction temperature and pressure can improve conversion of acetic acid. H2/AcOH mole ratio of 9.36 showed the best performance on acetic acid hydrogenation. High pressure had benefits for the selectivity of ethanol and other two parameters had no obvious effect on selectivity.  

Keywords: acetic acid hydrogenation, cylindrical particles, ethanol, PtSn

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154 Co-Gasification of Petroleum Waste and Waste Tires: A Numerical and CFD Study

Authors: Thomas Arink, Isam Janajreh


The petroleum industry generates significant amounts of waste in the form of drill cuttings, contaminated soil and oily sludge. Drill cuttings are a product of the off-shore drilling rigs, containing wet soil and total petroleum hydrocarbons (TPH). Contaminated soil comes from different on-shore sites and also contains TPH. The oily sludge is mainly residue or tank bottom sludge from storage tanks. The two main treatment methods currently used are incineration and thermal desorption (TD). Thermal desorption is a method where the waste material is heated to 450ºC in an anaerobic environment to release volatiles, the condensed volatiles can be used as a liquid fuel. For the thermal desorption unit dry contaminated soil is mixed with moist drill cuttings to generate a suitable mixture. By thermo gravimetric analysis (TGA) of the TD feedstock it was found that less than 50% of the TPH are released, the discharged material is stored in landfill. This study proposes co-gasification of petroleum waste with waste tires as an alternative to thermal desorption. Co-gasification with a high-calorific material is necessary since the petroleum waste consists of more than 60 wt% ash (soil/sand), causing its calorific value to be too low for gasification. Since the gasification process occurs at 900ºC and higher, close to 100% of the TPH can be released, according to the TGA. This work consists of three parts: 1. a mathematical gasification model, 2. a reactive flow CFD model and 3. experimental work on a drop tube reactor. Extensive material characterization was done by means of proximate analysis (TGA), ultimate analysis (CHNOS flash analysis) and calorific value measurements (Bomb calorimeter) for the input parameters of the mathematical and CFD model. The mathematical model is a zero dimensional model based on Gibbs energy minimization together with Lagrange multiplier; it is used to find the product species composition (molar fractions of CO, H2, CH4 etc.) for different tire/petroleum feedstock mixtures and equivalence ratios. The results of the mathematical model act as a reference for the CFD model of the drop-tube reactor. With the CFD model the efficiency and product species composition can be predicted for different mixtures and particle sizes. Finally both models are verified by experiments on a drop tube reactor (1540 mm long, 66 mm inner diameter, 1400 K maximum temperature).

Keywords: computational fluid dynamics (CFD), drop tube reactor, gasification, Gibbs energy minimization, petroleum waste, waste tires

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153 Malaysian's Shale Formation Characterizations: Geochemical Properties, Mineralogy, Adsorption and Desorption Behavior

Authors: Ahmed M. Al-Mutarreb, Shiferaw R. Jufar


Global shale gas resource assessment is still in its preliminary stage in most of the countries including the development of shale gas reservoirs in Malaysia. This project presents the main geochemical and mineral characteristics of few Malaysian’s shale samples which contribute on evaluating shale gas reserve world resource evaluations. Three shale samples from the western part of Peninsular Malaysia (Batu-Caja, Kuala Lumpur, and Johor Baru shale formations) were collected for this study. Total organic carbon wt.%, thermal maturity, kerogen type, mineralogy and adsorption/desorption characteristics are measured at Universiti Teknologi PETRONAS laboratories. Two samples show good potential in TOC results exhibited > 2wt.% exceeding the minimum values of Shale gas potential, while the third revealed < 1.5wt. Mineralogical compositions for the three samples are within the acceptable range percentage% of quartz and clays compared to shale plays in USA. This research’s results are promising and recommend to continue exploring and assessing unconventional shale gas reserves values in these areas.

Keywords: shale gas characterizations, geochemical properties, Malaysia, shale gas reserve

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152 Treatment of a Galvanization Wastewater in a Fixed-Bed Column Using L. hyperborean and P. canaliculata Macroalgae as Natural Cation Exchangers

Authors: Tatiana A. Pozdniakova, Maria A. P. Cechinel, Luciana P. Mazur, Rui A. R. Boaventura, Vitor J. P. Vilar.


Two brown macroalgae, Laminaria hyperborea and Pelvetia canaliculata, were employed as natural cation exchangers in a fixed-bed column for Zn(II) removal from a galvanization wastewater. The column (4.8 cm internal diameter) was packed with 30-59 g of previously hydrated algae up to a bed height of 17-27 cm. The wastewater or eluent was percolated using a peristaltic pump at a flow rate of 10 mL/min. The effluent used in each experiment presented similar characteristics: pH of 6.7, 55 mg/L of chemical oxygen demand and about 300, 44, 186 and 244 mg/L of sodium, calcium, chloride and sulphate ions, respectively. The main difference was nitrate concentration: 20 mg/L for the effluent used with L. hyperborean and 341 mg/L for the effluent used with P. canaliculata. The inlet zinc concentration also differed slightly: 11.2 mg/L for L. hyperborean and 8.9 mg/L for P. canaliculata experiments. The breakthrough time was approximately 22.5 hours for both macroalgae, corresponding to a service capacity of 43 bed volumes. This indicates that 30 g of biomass is able to treat 13.5 L of the galvanization wastewater. The uptake capacities at the saturation point were similar to that obtained in batch studies (unpublished data) for both algae. After column exhaustion, desorption with 0.1 M HNO3 was performed. Desorption using 9 and 8 bed volumes of eluent achieved an efficiency of 100 and 91%, respectively for L. hyperborean and P. canaliculata. After elution with nitric acid, the column was regenerated using different strategies: i) convert all the binding sites in the sodium form, by passing a solution of 0.5 M NaCl, until achieve a final pH of 6.0; ii) passing only tap water in order to increase the solution pH inside the column until pH 3.0, and in this case the second sorption cycle was performed using protonated algae. In the first approach, in order to remove the excess of salt inside the column, distilled water was passed through the column, leading to the algae structure destruction and the column collapsed. Using the second approach, the algae remained intact during three consecutive sorption/desorption cycles without loss of performance.

Keywords: biosorption, zinc, galvanization wastewater, packed-bed column

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151 Rapid Identification of Thermophilic Campylobacter Species from Retail Poultry Meat Using Matrix-Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry

Authors: Graziella Ziino, Filippo Giarratana, Stefania Maria Marotta, Alessandro Giuffrida, Antonio Panebianco


In Europe, North America and Japan, campylobacteriosis is one of the leading food-borne bacterial illnesses, often related to the consumption of poultry meats and/or by-products. The aim of this study was the evaluation of Campylobacter contamination of poultry meats marketed in Sicily (Italy) using both traditional methods and Matrix-Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry (MALDI-TOF MS). MALDI-TOF MS is considered a promising rapid (less than 1 hour) identification method for food borne pathogens bacteria. One hundred chicken and turkey meat preparations (no. 68 hamburgers, no. 21 raw sausages, no. 4 meatballs and no. 7 meat rolls) were taken from different butcher’s shops and large scale retailers and submitted to detection/enumeration of Campylobacter spp. according to EN ISO 10272-1:2006 and EN ISO 10272-2:2006. Campylobacter spp. was detected with general low counts in 44 samples (44%), of which 30 from large scale retailers and 14 from butcher’s shops. Chicken meats were significantly more contaminated than turkey meats. Among the preparations, Campylobacter spp. was found in 85.71% of meat rolls, 50% of meatballs, 44.12% of hamburgers and 28.57% of raw sausages. A total of 100 strains, 2-3 from each positive samples, were isolated for the identification by phenotypic, biomolecular and MALDI-TOF MS methods. C. jejuni was the predominant strains (63%), followed by C. coli (33%) and C. lari (4%). MALDI-TOF MS correctly identified 98% of the strains at the species level, only 1% of the tested strains were not identified. In the last 1%, a mixture of two different species was mixed in the same sample and MALDI-TOF MS correctly identified at least one of the strains. Considering the importance of rapid identification of pathogens in the food matrix, this method is highly recommended for the identification of suspected colonies of Campylobacteria.

Keywords: campylobacter spp., Food Microbiology, matrix-assisted laser desorption ionization-time of flight mass spectrometry, rapid microbial identification

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150 Removal of Pb(II) Ions from Wastewater Using Magnetic Chitosan–Ethylene Glycol Diglycidyl Ether Beads as Adsorbent

Authors: Pyar Singh Jassal, Priti Rani, Rajni Johar


The adsorption of Pb(II) ions from wastewater using ethylene glycol diglycidyl ether cross-linked magnetic chitosan beads (EGDE-MCB) was carried out by considering a number of parameters. The removal efficiency of the metal ion by magnetic chitosan beads (MCB) and its cross-linked derivatives depended on viz contact time, dose of the adsorbent, pH, temperature, etc. The concentration of Cd( II) at different time intervals was estimated by differential pulse anodic stripping voltammetry (DPSAV) using 797 voltametric analyzer computrace. The adsorption data could be well interpreted by Langmuir and Freundlich adsorption model. The equilibrium parameter, RL values, support that the adsorption (0Keywords: magnetic chitosan beads, ethylene glycol diglycidyl ether, equilibrium parameters, desorption

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149 Ultrasound-assisted Soil Washing Process for the Removal of Heavy Metals from Clays

Authors: Sophie Herr, Rachel Pflieger, Antoine Leybros, Yves Barre, Sergey Nikitenko


The proportion of soil contaminated by a wide range of pollutants (heavy metals, PCBs, pesticides, etc.) of anthropogenic origin is constantly increasing, and it is becoming urgent to address this issue. Among remediation methods, soil washing is an effective, relatively fast, and widely used process. This study assesses its coupling with ultrasound: indeed, sonication induces the formation of cavitation bubbles in solution that enhance local mass transfer through agitation and particle erosion. The removal of target toxic elements Ni(II) and Zn(II) from vermiculite clay has been studied under 20 kHz ultrasound and silent conditions. Several acids were tested, and HCl was chosen as solvent. The effects of solid/liquid ratio and particle size were investigated. Metal repartition in the clay has been followed by Tessier sequential extraction procedure. The results showed that more metal elements bound to the challenging residual phase were desorbed with 20 kHz ultrasound than in silent conditions. This supports the promising application of ultrasound for heavy metal desorption in difficult conditions. Further experiments were performed at high frequency US (362 kHz), and it was shown that fragmentation of the vermiculite particles is then limited, while positive effects of US in the decontamination are kept.

Keywords: desorption, heavy metals, ultrasound, vermiculite

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148 Competitive Adsorption of Al, Ga and In by Gamma Irradiation Induced Pectin-Acrylamide-(Vinyl Phosphonic Acid) Hydrogel

Authors: Md Murshed Bhuyan, Hirotaka Okabe, Yoshiki Hidaka, Kazuhiro Hara


Pectin-Acrylamide- (Vinyl Phosphonic Acid) Hydrogels were prepared from their blend by using gamma radiation of various doses. It was found that the gel fraction of hydrogel increases with increasing the radiation dose reaches a maximum and then started decreasing with increasing the dose. The optimum radiation dose and the composition of raw materials were determined on the basis of equilibrium swelling which resulted in 20 kGy absorbed dose and 1:2:4 (Pectin:AAm:VPA) composition. Differential scanning calorimetry reveals the gel strength for using them as the adsorbent. The FTIR-spectrum confirmed the grafting/ crosslinking of the monomer on the backbone of pectin chain. The hydrogels were applied in adsorption of Al, Ga, and In from multielement solution where the adsorption capacity order for those three elements was found as – In>Ga>Al. SEM images of hydrogels and metal adsorbed hydrogels indicate the gel network and adherence of the metal ions in the interpenetrating network of the hydrogel which were supported by EDS spectra. The adsorption isotherm models were studied and found that the Langmuir adsorption isotherm model was well fitted with the data. Adsorption data were also fitted to different adsorption kinetic and diffusion models. Desorption of metal adsorbed hydrogels was performed in 5% nitric acid where desorption efficiency was found around 90%.

Keywords: hydrogel, gamma radiation, vinyl phosphonic acid, metal adsorption

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147 Fire Safe Medical Oxygen Delivery for Aerospace Environments

Authors: M. A. Rahman, A. T. Ohta, H. V. Trinh, J. Hyvl


Atmospheric pressure and oxygen (O2) concentration are critical life support parameters for human-occupied aerospace vehicles and habitats. Various medical conditions may require medical O2; for example, the American Medical Association has determined that commercial air travel exposes passengers to altitude-related hypoxia and gas expansion. It may cause some passengers to experience significant symptoms and medical complications during the flight, requiring supplemental medical-grade O2 to maintain adequate tissue oxygenation and prevent hypoxemic complications. Although supplemental medical grade O2 is a successful lifesaver for respiratory and cardiac failure, O2-enriched exhaled air can contain more than 95 % O2, increasing the likelihood of a fire. In an aerospace environment, a localized high concentration O2 bubble forms around a patient being treated for hypoxia, increasing the cabin O2 beyond the safe limit. To address this problem, this work describes a medical O2 delivery system that can reduce the O2 concentration from patient-exhaled O2-rich air to safe levels while maintaining the prescribed O2 administration to the patient. The O2 delivery system is designed to be a part of the medical O2 kit. The system uses cationic multimetallic cobalt complexes to reversibly, selectively, and stoichiometrically chemisorb O2 from the exhaled air. An air-release sub-system monitors the exhaled air, and as soon the O2 percentage falls below 21%, the air is released to the room air. The O2-enriched exhaled air is channeled through a layer of porous, thin-film heaters coated with the cobalt complex. The complex absorbs O2, and when saturated, the complex is heated to 100°C using the thin-film heater. Upon heating, the complex desorbs O2 and is once again ready to absorb or remove the excess O2 from exhaled air. The O2 absorption is a sub-second process, and desorption is a multi-second process. While heating at 0.685 °C/sec, the complex desorbs ~90% O2 in 110 sec. These fast reaction times mean that a simultaneous absorb/desorb process in the O2 delivery system will create a continuous absorption of O2. Moreover, the complex can concentrate O2 by a factor of 160 times that in air and desorb over 90% of the O2 at 100°C. Over 12 cycles of thermogravimetry measurement, less than 0.1% decrease in reversibility in O2 uptake was observed. The 1 kg complex can desorb over 20L of O2, so simultaneous O2 desorption by 0.5 kg of complex and absorption by 0.5 kg of complex can potentially continuously remove 9L/min O2 (~90% desorbed at 100°C) from exhaled air. The complex is synthesized and characterized for reversible O2 absorption and efficacy. The complex changes its color from dark brown to light gray after O2 desorption. In addition to thermogravimetric analysis, the O2 absorption/desorption cycle is characterized using optical imaging, showing stable color changes over ten cycles. The complex was also tested at room temperature in a low O2 environment in its O2 desorbed state, and observed to hold the deoxygenated state under these conditions. The results show the feasibility of using the complex for reversible O2 absorption in the proposed fire safe medical O2 delivery system.

Keywords: fire risk, medical oxygen, oxygen removal, reversible absorption

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146 Acetic Acid Adsorption and Decomposition on Pt(111): Comparisons to Ni(111)

Authors: Lotanna Ezeonu, Jason P. Robbins, Ziyu Tang, Xiaofang Yang, Bruce E. Koel, Simon G. Podkolzin


The interaction of organic molecules with metal surfaces is of interest in numerous technological applications, such as catalysis, bone replacement, and biosensors. Acetic acid is one of the main products of bio-oils produced from the pyrolysis of hemicellulosic feedstocks. However, their high oxygen content makes them unsuitable for use as fuels. Hydrodeoxygenation is a proven technique for catalytic deoxygenation of bio-oils. An understanding of the energetics and control of the bond-breaking sequences of biomass-derived oxygenates on metal surfaces will enable a guided optimization of existing catalysts and the development of more active/selective processes for biomass transformations to fuels. Such investigations have been carried out with the aid of ultrahigh vacuum and its concomitant techniques. The high catalytic activity of platinum in biomass-derived oxygenate transformations has sparked a lot of interest. We herein exploit infrared reflection absorption spectroscopy(IRAS), temperature-programmed desorption(TPD), and density functional theory(DFT) to study the adsorption and decomposition of acetic acid on a Pt(111) surface, which was then compared with Ni(111), a model non-noble metal. We found that acetic acid adsorbs molecularly on the Pt(111) surface, interacting through the lone pair of electrons of one oxygen atomat 90 K. At 140 K, the molecular form is still predominant, with some dissociative adsorption (in the form of acetate and hydrogen). Annealing to 193 K led to complete dehydrogenation of molecular acetic acid species leaving adsorbed acetate. At 440 K, decomposition of the acetate species occurs via decarbonylation and decarboxylation as evidenced by desorption peaks for H₂,CO, CO₂ and CHX fragments (x=1, 2) in theTPD.The assignments for the experimental IR peaks were made using visualization of the DFT-calculated vibrational modes. The results showed that acetate adsorbs in a bridged bidentate (μ²η²(O,O)) configuration. The coexistence of linear and bridge bonded CO was also predicted by the DFT results. Similar molecular acid adsorption energy was predicted in the case of Ni(111) whereas a significant difference was found for acetate adsorption.

Keywords: acetic acid, platinum, nickel, infared-absorption spectrocopy, temperature programmed desorption, density functional theory

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