Improved Livingness and Control over Branching in RAFT Polymerization of Acrylates: Could Microflow Synthesis Make the Difference?

PubMed

Derboven, Pieter; Van Steenberge, Paul H M; Vandenbergh, Joke; Reyniers, Marie-Francoise; Junkers, Thomas; D'hooge, Dagmar R; Marin, Guy B

2015-12-01

The superior capabilities of structured microreactors over batch reactors are demonstrated for reversible addition-fragmentation chain transfer (RAFT) solution polymerization of n-butyl acrylate with the aid of simulations, explicitly accounting for the chain length distribution of all macrospecies types. Since perfect isothermicity can be established in a microreactor, less side products due to backbiting and β-scission are formed compared to the batch operation in which ineffective heat removal leads to an undesirable temperature spike. For a given RAFT chain transfer agent (CTA), additional microstructural control results under microflow conditions by optimizing the reaction temperature, lowering the dilution degree, or decreasing the initial molar ratio of monomer to RAFT CTA. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Modeling chemical vapor deposition of silicon dioxide in microreactors at atmospheric pressure

NASA Astrophysics Data System (ADS)

Konakov, S. A.; Krzhizhanovskaya, V. V.

2015-01-01

We developed a multiphysics mathematical model for simulation of silicon dioxide Chemical Vapor Deposition (CVD) from tetraethyl orthosilicate (TEOS) and oxygen mixture in a microreactor at atmospheric pressure. Microfluidics is a promising technology with numerous applications in chemical synthesis due to its high heat and mass transfer efficiency and well-controlled flow parameters. Experimental studies of CVD microreactor technology are slow and expensive. Analytical solution of the governing equations is impossible due to the complexity of intertwined non-linear physical and chemical processes. Computer simulation is the most effective tool for design and optimization of microreactors. Our computational fluid dynamics model employs mass, momentum and energy balance equations for a laminar transient flow of a chemically reacting gas mixture at low Reynolds number. Simulation results show the influence of microreactor configuration and process parameters on SiO2 deposition rate and uniformity. We simulated three microreactors with the central channel diameter of 5, 10, 20 micrometers, varying gas flow rate in the range of 5-100 microliters per hour and temperature in the range of 300-800 °C. For each microchannel diameter we found an optimal set of process parameters providing the best quality of deposited material. The model will be used for optimization of the microreactor configuration and technological parameters to facilitate the experimental stage of this research.

Chemical microreactor and method thereof

DOEpatents

Morse, Jeffrey D [Martinez, CA; Jankowski, Alan [Livermore, CA

2011-08-09

A method for forming a chemical microreactor includes forming at least one capillary microchannel in a substrate having at least one inlet and at least one outlet, integrating at least one heater into the chemical microreactor, interfacing the capillary microchannel with a liquid chemical reservoir at the inlet of the capillary microchannel, and interfacing the capillary microchannel with a porous membrane near the outlet of the capillary microchannel, the porous membrane being positioned beyond the outlet of the capillary microchannel, wherein the porous membrane has at least one catalyst material imbedded therein.

Selective synthesis of human milk fat-style structured triglycerides from microalgal oil in a microfluidic reactor packed with immobilized lipase

DOE PAGES

Wang, Jun; Liu, Xi; Wang, Xu -Dong; ...

2016-08-18

Human milk fat-style structured triacylglycerols were produced from microalgal oil in a continuous microfluidic reactor packed with immobilized lipase for the first time. A remarkably high conversion efficiency was demonstrated in the microreactor with reaction time being reduced by 8 times, Michaelis constant decreased 10 times, the lipase reuse times increased 2.25-fold compared to those in a batch reactor. In addition, the content of palmitic acid at sn-2 position (89.0%) and polyunsaturated fatty acids at sn-1, 3 positions (81.3%) are slightly improved compared to the product in a batch reactor. The increase of melting points (1.7 °C) and decrease ofmore » crystallizing point (3 °C) implied higher quality product was produced using the microfluidic technology. The main cost can be reduced from 212.3 to 14.6 per batch with the microreactor. Altogether, the microfluidic bioconversion technology is promising for modified functional lipids production allowing for cost-effective approach to produce high-value microalgal coproducts.« less

Selective synthesis of human milk fat-style structured triglycerides from microalgal oil in a microfluidic reactor packed with immobilized lipase

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Jun; Liu, Xi; Wang, Xu -Dong

Human milk fat-style structured triacylglycerols were produced from microalgal oil in a continuous microfluidic reactor packed with immobilized lipase for the first time. A remarkably high conversion efficiency was demonstrated in the microreactor with reaction time being reduced by 8 times, Michaelis constant decreased 10 times, the lipase reuse times increased 2.25-fold compared to those in a batch reactor. In addition, the content of palmitic acid at sn-2 position (89.0%) and polyunsaturated fatty acids at sn-1, 3 positions (81.3%) are slightly improved compared to the product in a batch reactor. The increase of melting points (1.7 °C) and decrease ofmore » crystallizing point (3 °C) implied higher quality product was produced using the microfluidic technology. The main cost can be reduced from 212.3 to 14.6 per batch with the microreactor. Altogether, the microfluidic bioconversion technology is promising for modified functional lipids production allowing for cost-effective approach to produce high-value microalgal coproducts.« less

Selective synthesis of human milk fat-style structured triglycerides from microalgal oil in a microfluidic reactor packed with immobilized lipase.

PubMed

Wang, Jun; Liu, Xi; Wang, Xu-Dong; Dong, Tao; Zhao, Xing-Yu; Zhu, Dan; Mei, Yi-Yuan; Wu, Guo-Hua

2016-11-01

Human milk fat-style structured triacylglycerols were produced from microalgal oil in a continuous microfluidic reactor packed with immobilized lipase for the first time. A remarkably high conversion efficiency was demonstrated in the microreactor with reaction time being reduced by 8 times, Michaelis constant decreased 10 times, the lipase reuse times increased 2.25-fold compared to those in a batch reactor. In addition, the content of palmitic acid at sn-2 position (89.0%) and polyunsaturated fatty acids at sn-1, 3 positions (81.3%) are slightly improved compared to the product in a batch reactor. The increase of melting points (1.7°C) and decrease of crystallizing point (3°C) implied higher quality product was produced using the microfluidic technology. The main cost can be reduced from $212.3 to $14.6 per batch with the microreactor. Overall, the microfluidic bioconversion technology is promising for modified functional lipids production allowing for cost-effective approach to produce high-value microalgal coproducts. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis of a drug-like focused library of trisubstituted pyrrolidines using integrated flow chemistry and batch methods.

PubMed

Baumann, Marcus; Baxendale, Ian R; Kuratli, Christoph; Ley, Steven V; Martin, Rainer E; Schneider, Josef

2011-07-11

A combination of flow and batch chemistries has been successfully applied to the assembly of a series of trisubstituted drug-like pyrrolidines. This study demonstrates the efficient preparation of a focused library of these pharmaceutically important structures using microreactor technologies, as well as classical parallel synthesis techniques, and thus exemplifies the impact of integrating innovative enabling tools within the drug discovery process.

Novel approach to investigation of semiconductor MOCVD by microreactor technology

NASA Astrophysics Data System (ADS)

Konakov, S. A.; Krzhizhanovskaya, V. V.

2017-11-01

Metal-Organic Chemical Vapour Deposition is a very complex technology that requires further investigation and optimization. We propose to apply microreactors to (1) replace multiple expensive time-consuming macroscale experiments by just one microreactor deposition with many points on one substrate; (2) to derive chemical reaction rates from individual deposition profiles using theoretical analytical solution. In this paper we also present the analytical solution of a simplified equation describing the deposition rate dependency on temperature. It allows to solve an inverse problem and to obtain detailed information about chemical reaction mechanism of MOCVD process.

Flow microreactor synthesis in organo-fluorine chemistry

PubMed Central

Nagaki, Aiichiro

2013-01-01

Summary Organo-fluorine compounds are the substances of considerable interest in various industrial fields due to their unique physical and chemical properties. Despite increased demand in wide fields of science, synthesis of fluoro-organic compounds is still often faced with problems such as the difficulties in handling of fluorinating reagents and in controlling of chemical reactions. Recently, flow microreactor synthesis has emerged as a new methodology for producing chemical substances with high efficiency. This review outlines the successful examples of synthesis and reactions of fluorine-containing molecules by the use of flow microreactor systems to overcome long-standing problems in fluorine chemistry. PMID:24367443

Flow microreactor synthesis in organo-fluorine chemistry.

PubMed

Amii, Hideki; Nagaki, Aiichiro; Yoshida, Jun-Ichi

2013-12-05

Organo-fluorine compounds are the substances of considerable interest in various industrial fields due to their unique physical and chemical properties. Despite increased demand in wide fields of science, synthesis of fluoro-organic compounds is still often faced with problems such as the difficulties in handling of fluorinating reagents and in controlling of chemical reactions. Recently, flow microreactor synthesis has emerged as a new methodology for producing chemical substances with high efficiency. This review outlines the successful examples of synthesis and reactions of fluorine-containing molecules by the use of flow microreactor systems to overcome long-standing problems in fluorine chemistry.

Micro-Fluidic Chemical Reactor Systems: Development, Scale-Up and Demonstration

DTIC Science & Technology

2002-11-01

B) A ) Figure 1: Gas Phase Microreactor . ( A ) Photograph of device. (B) Top view schematic. (C) Side view across channel. ( D ) Side view along... Microreactor system showing controller, heater power, fluid mixing, and microreactor cards (as in Figure 14) in a PCI chassis... microreactor design used for gas-phase heterogeneous reactions is a microchannel device that can be integrated with a heat exchange layer for highly

An automated microreactor for semi-continuous biosensor measurements.

PubMed

Buffi, Nina; Beggah, Siham; Truffer, Frederic; Geiser, Martial; van Lintel, Harald; Renaud, Philippe; van der Meer, Jan Roelof

2016-04-21

Living bacteria or yeast cells are frequently used as bioreporters for the detection of specific chemical analytes or conditions of sample toxicity. In particular, bacteria or yeast equipped with synthetic gene circuitry that allows the production of a reliable non-cognate signal (e.g., fluorescent protein or bioluminescence) in response to a defined target make robust and flexible analytical platforms. We report here how bacterial cells expressing a fluorescence reporter ("bactosensors"), which are mostly used for batch sample analysis, can be deployed for automated semi-continuous target analysis in a single concise biochip. Escherichia coli-based bactosensor cells were continuously grown in a 13 or 50 nanoliter-volume reactor on a two-layered polydimethylsiloxane-on-glass microfluidic chip. Physiologically active cells were directed from the nl-reactor to a dedicated sample exposure area, where they were concentrated and reacted in 40 minutes with the target chemical by localized emission of the fluorescent reporter signal. We demonstrate the functioning of the bactosensor-chip by the automated detection of 50 μgarsenite-As l(-1) in water on consecutive days and after a one-week constant operation. Best induction of the bactosensors of 6-9-fold to 50 μg l(-1) was found at an apparent dilution rate of 0.12 h(-1) in the 50 nl microreactor. The bactosensor chip principle could be widely applicable to construct automated monitoring devices for a variety of targets in different environments.

Accelerated gas-liquid visible light photoredox catalysis with continuous-flow photochemical microreactors.

PubMed

Straathof, Natan J W; Su, Yuanhai; Hessel, Volker; Noël, Timothy

2016-01-01

In this protocol, we describe the construction and use of an operationally simple photochemical microreactor for gas-liquid photoredox catalysis using visible light. The general procedure includes details on how to set up the microreactor appropriately with inlets for gaseous reagents and organic starting materials, and it includes examples of how to use it to achieve continuous-flow preparation of disulfides or trifluoromethylated heterocycles and thiols. The reported photomicroreactors are modular, inexpensive and can be prepared rapidly from commercially available parts within 1 h even by nonspecialists. Interestingly, typical reaction times of gas-liquid visible light photocatalytic reactions performed in microflow are lower (in the minute range) than comparable reactions performed as a batch process (in the hour range). This can be attributed to the improved irradiation efficiency of the reaction mixture and the enhanced gas-liquid mass transfer in the segmented gas-liquid flow regime.

Microreactor Array Device

NASA Astrophysics Data System (ADS)

Wiktor, Peter; Brunner, Al; Kahn, Peter; Qiu, Ji; Magee, Mitch; Bian, Xiaofang; Karthikeyan, Kailash; Labaer, Joshua

2015-03-01

We report a device to fill an array of small chemical reaction chambers (microreactors) with reagent and then seal them using pressurized viscous liquid acting through a flexible membrane. The device enables multiple, independent chemical reactions involving free floating intermediate molecules without interference from neighboring reactions or external environments. The device is validated by protein expressed in situ directly from DNA in a microarray of ~10,000 spots with no diffusion during three hours incubation. Using the device to probe for an autoantibody cancer biomarker in blood serum sample gave five times higher signal to background ratio compared to standard protein microarray expressed on a flat microscope slide. Physical design principles to effectively fill the array of microreactors with reagent and experimental results of alternate methods for sealing the microreactors are presented.

Conscious coupling: The challenges and opportunities of cascading enzymatic microreactors.

PubMed

Gruber, Pia; Marques, Marco P C; O'Sullivan, Brian; Baganz, Frank; Wohlgemuth, Roland; Szita, Nicolas

2017-07-01

The continuous production of high value or difficult to synthesize products is of increasing interest to the pharmaceutical industry. Cascading reaction systems have already been employed for chemical synthesis with great success, allowing a quick change in reaction conditions and addition of new reactants as well as removal of side products. A cascading system can remove the need for isolating unstable intermediates, increasing the yield of a synthetic pathway. Based on the success for chemical synthesis, the question arises how cascading systems could be beneficial to chemo-enzymatic or biocatalytic synthesis. Microreactors, with their rapid mass and heat transfer, small reaction volumes and short diffusion pathways, are promising tools for the development of such processes. In this mini-review, the authors provide an overview of recent examples of cascaded microreactors. Special attention will be paid to how microreactors are combined and the challenges as well as opportunities that arise from such combinations. Selected chemical reaction cascades will be used to illustrate this concept, before the discussion is widened to include chemo-enzymatic and multi-enzyme cascades. The authors also present the state of the art of online and at-line monitoring for enzymatic microreactor cascades. Finally, the authors review work-up and purification steps and their integration with microreactor cascades, highlighting the potential and the challenges of integrated cascades. © 2017 The Authors. Biotechnology Journal published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microreactor Array Device

PubMed Central

Wiktor, Peter; Brunner, Al; Kahn, Peter; Qiu, Ji; Magee, Mitch; Bian, Xiaofang; Karthikeyan, Kailash; LaBaer, Joshua

2015-01-01

We report a device to fill an array of small chemical reaction chambers (microreactors) with reagent and then seal them using pressurized viscous liquid acting through a flexible membrane. The device enables multiple, independent chemical reactions involving free floating intermediate molecules without interference from neighboring reactions or external environments. The device is validated by protein expressed in situ directly from DNA in a microarray of ~10,000 spots with no diffusion during three hours incubation. Using the device to probe for an autoantibody cancer biomarker in blood serum sample gave five times higher signal to background ratio compared to standard protein microarray expressed on a flat microscope slide. Physical design principles to effectively fill the array of microreactors with reagent and experimental results of alternate methods for sealing the microreactors are presented. PMID:25736721

Scalable microreactors and methods for using same

DOEpatents

Lawal, Adeniyi; Qian, Dongying

2010-03-02

The present invention provides a scalable microreactor comprising a multilayered reaction block having alternating reaction plates and heat exchanger plates that have a plurality of microchannels; a multilaminated reactor input manifold, a collecting reactor output manifold, a heat exchange input manifold and a heat exchange output manifold. The present invention also provides methods of using the microreactor for multiphase chemical reactions.

Application of Microreactor to the Preparation of C-11-Labeled Compounds via O-[11C]Methylation with [11C]CH3I: Rapid Synthesis of [11C]Raclopride.

PubMed

Kawashima, Hidekazu; Kimura, Hiroyuki; Nakaya, Yuta; Tomatsu, Kenji; Arimitsu, Kenji; Nakanishi, Hiroaki; Ozeki, Eiichi; Kuge, Yuji; Saji, Hideo

2015-01-01

A new radiolabeling method using a microreactor was developed for the rapid synthesis of [(11)C]raclopride. A chip bearing a Y-shaped mixing junction with a 200 µm (width)×20 µm (depth)×250 mm (length) flow channel was designed, and the efficiency of O-[11C]methylation was evaluated. Dimethyl sulfoxide solutions containing the O-desmethyl precursor or [11C]CH3I were introduced into separate injection ports by infusion syringes, and the radiochemical yields were measured under various conditions. The decay-corrected radiochemical yield of microreactor-derived [11C]raclopride reached 12% in 20 s at 25 °C, which was observed to increase with increasing temperature. In contrast, batch synthesis at 25 °C produced a yield of 5%: this indicates that this device could effectively achieve O-[11C]methylation in a shorter period of time. The microreactor technique may facilitate simple and efficient routine production of 11C-labeled compounds via O-[11C]methylation with [11C]CH3I.

Parallelization of Catalytic Packed-Bed Microchannels with Pressure-Drop Microstructures for Gas-Liquid Multiphase Reactions

NASA Astrophysics Data System (ADS)

Murakami, Sunao; Ohtaki, Kenichiro; Matsumoto, Sohei; Inoue, Tomoya

2012-06-01

High-throughput and stable treatments are required to achieve the practical production of chemicals with microreactors. However, the flow maldistribution to the paralleled microchannels has been a critical problem in achieving the productive use of multichannel microreactors for multiphase flow conditions. In this study, we newly designed and fabricated a glass four-channel catalytic packed-bed microreactor for the scale-up of gas-liquid multiphase chemical reactions. We embedded microstructures generating high pressure losses at the upstream side of each packed bed, and experimentally confirmed the efficacy of the microstructures in decreasing the maldistribution of the gas-liquid flow to the parallel microchannels.

Microfluidic Reactors for the Controlled Synthesis of Nanoparticles

NASA Astrophysics Data System (ADS)

Erdem, Emine Yegan

Nanoparticles have attracted a lot of attention in the past few decades due to their unique, size-dependent properties. In order to use these nanoparticles in devices or sensors effectively, it is important to maintain uniform properties throughout the system; therefore nanoparticles need to have uniform sizes -- or monodisperse. In order to achieve monodispersity, an extreme control over the reaction conditions is required during their synthesis. These reaction conditions such as temperature, concentration of reagents, residence times, etc. affect the structure of nanoparticles dramatically; therefore when the conditions vary locally in the reaction vessel, different sized nanoparticles form, causing polydispersity. In widely-used batch wise synthesis techniques, large sized reaction vessels are used to mix and heat reagents. In these types of systems, it is very hard to avoid thermal gradients and to achieve rapid mixing times as well as to control residence times. Also it is not possible to make rapid changes in the reaction parameters during the synthesis. The other drawback of conventional methods is that it is not possible to separate the nucleation of nanoparticles from their growth; this leads to combined nucleation and growth and subsequently results in polydisperse size distributions. Microfluidics is an alternative method by which the limitations of conventional techniques can be addressed. Due to the small size, it is possible to control temperature and concentration of reagents precisely as well as to make rapid changes in mixing ratios of reagents or temperature of the reaction zones. There have been several microfluidic reactors -- (microreactors) in literature that were designed to improve the size distribution of nanoparticles. In this work, two novel microfluidic systems were developed for achieving controlled synthesis of nanoparticles. The first microreactor was made out of a chemically robust polymer, polyurethane, and it was used for low temperature nanoparticle synthesis. This microreactor was fabricated by using a CO 2-laser printer, which is an inexpensive method for fabricating microfluidic devices and it is a relatively fast way compared to other fabrication techniques. Iron oxide nanoparticle synthesis was demonstrated using this reactor and size distributions with a standard deviation of 10% was obtained. The second microreactor presented in this work was designed to produce monodisperse nanoparticles by utilizing thermally isolated heated and cooled regions for separating nucleation and growth processes. This microreactor was made out of silicon and it was used to demonstrate the synthesis of TiO 2 nanoparticles. Size distributions with less than 10% standard deviation were achieved. This microreactor also provides a platform for studying the effects of temperature and residence times which is very important to understand the reaction kinetics of nanoparticle synthesis. In this work, two microfluidic techniques for retrieving nanoparticles from the microreactors were also discussed. The first method was based on trapping the aqueous droplet phase inside the microchannel and the second method was utilizing a micropost array to direct droplets from the oil solution to the pure water. As a final step, a printing technique was used to print nanoparticles synthesized inside the microreactors for future applications. This ability is important for achieving smart surfaces that can utilize the properties of nanoparticles for sensing applications in the future.

Applications of immobilized catalysts in continuous flow processes.

PubMed

Kirschning, Andreas; Jas, Gerhard

2004-01-01

As part of the dramatic changes associated with automation in pharmaceutical and agrochemical research laboratories, the search for new technologies has become a major topic in the chemical community. Commonly, high-throughput chemistry is still carried out in batches whereas flow-through processes are rather restricted to production processes, despite the fact that the latter concept allows facile automation, reproducibility, safety, and process reliability. Indeed, methods and technologies are missing that allow rapid transfer from the research level to process development. Continuous flow processes are considered as a universal lever to overcome these restrictions and only recently, joint efforts between synthetic and polymer chemists and chemical engineers have resulted in the first continuous flow devices and microreactors which allow rapid preparation of compounds with minimum workup. Importantly, more and more developments combine the use of immobilized reagents and catalysts with the concept of structured continuous flow reactors. Consequently, the present article focuses on this new research field, which is located at the interface of continuous flow processes and solid-phase-bound catalysts.

Chemical microreactor and method thereof

DOEpatents

Morse, Jeffrey D.; Jankowski, Alan

2005-11-01

A chemical microreactor suitable for generation of hydrogen fuel from liquid sources such as ammonia, methanol, and butane through steam reforming processes when mixed with an appropriate amount of water contains capillary microchannels with integrated resistive heaters to facilitate the occurrence of catalytic steam reforming reactions. One such microreactor employs a packed catalyst capillary microchannel and at least one porous membrane. Another employs a porous membrane with a large surface area or a porous membrane support structure containing a plurality of porous membranes having a large surface area in the aggregate, i.e., greater than about 1 m.sup.2 /cm.sup.3. The packed catalyst capillary microchannels, porous membranes and porous membrane support structures may be formed by a variety of methods.

High mass resolution time of flight mass spectrometer for measuring products in heterogeneous catalysis in highly sensitive microreactors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Andersen, T.; Jensen, R.; Christensen, M. K.

2012-07-15

We demonstrate a combined microreactor and time of flight system for testing and characterization of heterogeneous catalysts with high resolution mass spectrometry and high sensitivity. Catalyst testing is performed in silicon-based microreactors which have high sensitivity and fast thermal response. Gas analysis is performed with a time of flight mass spectrometer with a modified nude Bayard-Alpert ionization gauge as gas ionization source. The mass resolution of the time of flight mass spectrometer using the ion gauge as ionization source is estimated to m/{Delta}m > 2500. The system design is superior to conventional batch and flow reactors with accompanying product detectionmore » by quadrupole mass spectrometry or gas chromatography not only due to the high sensitivity, fast temperature response, high mass resolution, and fast acquisition time of mass spectra but it also allows wide mass range (0-5000 amu in the current configuration). As a demonstration of the system performance we present data from ammonia oxidation on a Pt thin film showing resolved spectra of OH and NH{sub 3}.« less

A novel continuous flow biosynthesis of caffeic acid phenethyl ester from alkyl caffeate and phenethanol in a packed bed microreactor.

PubMed

Wang, Jun; Gu, Shuang-Shuang; Cui, Hong-Sheng; Wu, Xiang-Yang; Wu, Fu-An

2014-04-01

Caffeic acid phenethyl ester (CAPE) is a rare natural ingredient with several biological activity, but the industrial production of CAPE using lipase-catalyzed esterification of caffeic acid (CA) and 2-phenylethanol (PE) in ionic liquids is hindered by low substrate concentrations and a long reaction time. To establish a high-efficiency bioprocess for obtaining CAPE, a novel continuous flow biosynthesis of CAPE from alkyl caffeate and PE in [Bmim][Tf2N] using a packed bed microreactor was successfully carried out. Among the tested alkyl caffeates and lipases, methyl caffeate and Novozym 435, respectively, were selected as the suitable substrate and biocatalyst. Under the optimum conditions selected using response surface methodology, a 93.21% CAPE yield was achieved in 2.5h using a packed bed microreactor, compared to 24h using a batch reactor. The reuse of Novozym 435 for 20 cycles and continuous reaction for 9 days did not result in any decrease in activity. Copyright © 2014 Elsevier Ltd. All rights reserved.

Six-flow operations for catalyst development in Fischer-Tropsch synthesis: Bridging the gap between high-throughput experimentation and extensive product evaluation

NASA Astrophysics Data System (ADS)

Sartipi, Sina; Jansma, Harrie; Bosma, Duco; Boshuizen, Bart; Makkee, Michiel; Gascon, Jorge; Kapteijn, Freek

2013-12-01

Design and operation of a "six-flow fixed-bed microreactor" setup for Fischer-Tropsch synthesis (FTS) is described. The unit consists of feed and mixing, flow division, reaction, separation, and analysis sections. The reactor system is made of five heating blocks with individual temperature controllers, assuring an identical isothermal zone of at least 10 cm along six fixed-bed microreactor inserts (4 mm inner diameter). Such a lab-scale setup allows running six experiments in parallel, under equal feed composition, reaction temperature, and conditions of separation and analysis equipment. It permits separate collection of wax and liquid samples (from each flow line), allowing operation with high productivities of C5+ hydrocarbons. The latter is crucial for a complete understanding of FTS product compositions and will represent an advantage over high-throughput setups with more than ten flows where such instrumental considerations lead to elevated equipment volume, cost, and operation complexity. The identical performance (of the six flows) under similar reaction conditions was assured by testing a same catalyst batch, loaded in all microreactors.

High mass resolution time of flight mass spectrometer for measuring products in heterogeneous catalysis in highly sensitive microreactors

NASA Astrophysics Data System (ADS)

Andersen, T.; Jensen, R.; Christensen, M. K.; Pedersen, T.; Hansen, O.; Chorkendorff, I.

2012-07-01

We demonstrate a combined microreactor and time of flight system for testing and characterization of heterogeneous catalysts with high resolution mass spectrometry and high sensitivity. Catalyst testing is performed in silicon-based microreactors which have high sensitivity and fast thermal response. Gas analysis is performed with a time of flight mass spectrometer with a modified nude Bayard-Alpert ionization gauge as gas ionization source. The mass resolution of the time of flight mass spectrometer using the ion gauge as ionization source is estimated to m/Δm > 2500. The system design is superior to conventional batch and flow reactors with accompanying product detection by quadrupole mass spectrometry or gas chromatography not only due to the high sensitivity, fast temperature response, high mass resolution, and fast acquisition time of mass spectra but it also allows wide mass range (0-5000 amu in the current configuration). As a demonstration of the system performance we present data from ammonia oxidation on a Pt thin film showing resolved spectra of OH and NH3.

High mass resolution time of flight mass spectrometer for measuring products in heterogeneous catalysis in highly sensitive microreactors.

PubMed

Andersen, T; Jensen, R; Christensen, M K; Pedersen, T; Hansen, O; Chorkendorff, I

2012-07-01

We demonstrate a combined microreactor and time of flight system for testing and characterization of heterogeneous catalysts with high resolution mass spectrometry and high sensitivity. Catalyst testing is performed in silicon-based microreactors which have high sensitivity and fast thermal response. Gas analysis is performed with a time of flight mass spectrometer with a modified nude Bayard-Alpert ionization gauge as gas ionization source. The mass resolution of the time of flight mass spectrometer using the ion gauge as ionization source is estimated to m/Δm > 2500. The system design is superior to conventional batch and flow reactors with accompanying product detection by quadrupole mass spectrometry or gas chromatography not only due to the high sensitivity, fast temperature response, high mass resolution, and fast acquisition time of mass spectra but it also allows wide mass range (0-5000 amu in the current configuration). As a demonstration of the system performance we present data from ammonia oxidation on a Pt thin film showing resolved spectra of OH and NH(3).

Method for forming a chemical microreactor

DOEpatents

Morse, Jeffrey D [Martinez, CA; Jankowski, Alan [Livermore, CA

2009-05-19

Disclosed is a chemical microreactor that provides a means to generate hydrogen fuel from liquid sources such as ammonia, methanol, and butane through steam reforming processes when mixed with an appropriate amount of water. The microreactor contains capillary microchannels with integrated resistive heaters to facilitate the occurrence of catalytic steam reforming reactions. Two distinct embodiment styles are discussed. One embodiment style employs a packed catalyst capillary microchannel and at least one porous membrane. Another embodiment style employs a porous membrane with a large surface area or a porous membrane support structure containing a plurality of porous membranes having a large surface area in the aggregate, i.e., greater than about 1 m.sup.2/cm.sup.3. Various methods to form packed catalyst capillary microchannels, porous membranes and porous membrane support structures are also disclosed.

Enzymatic Continuous Flow Synthesis of Thiol-Terminated Poly(δ-Valerolactone) and Block Copolymers.

PubMed

Zhu, Ning; Huang, Weijun; Hu, Xin; Liu, Yihuan; Fang, Zheng; Guo, Kai

2018-04-01

Thiol-terminated poly(δ-valerolactone) is directly synthesized via enzymatic 6-mercapto-1-hexanol initiated ring-opening polymerization in both batch and microreactor. By using Candida antartica Lipase B immobilized tubular reactor, narrowly dispersed poly(δ-valerolactone) with higher thiol fidelity is more efficiently prepared in contrast to the batch reactor. Moreover, the integrated enzyme packed tubular reactor system is established to perform the chain extension experiments. Thiol-terminated poly(δ-valerolactone)-block-poly(ε-caprolactone) and poly(ε-caprolactone)-block-poly(δ-valerolactone) are easily prepared by modulating the monomer introduction sequence. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Molecular Imaging Probe Development using Microfluidics

PubMed Central

Liu, Kan; Wang, Ming-Wei; Lin, Wei-Yu; Phung, Duy Linh; Girgis, Mark D.; Wu, Anna M.; Tomlinson, James S.; Shen, Clifton K.-F.

2012-01-01

In this manuscript, we review the latest advancement of microfluidics in molecular imaging probe development. Due to increasing needs for medical imaging, high demand for many types of molecular imaging probes will have to be met by exploiting novel chemistry/radiochemistry and engineering technologies to improve the production and development of suitable probes. The microfluidic-based probe synthesis is currently attracting a great deal of interest because of their potential to deliver many advantages over conventional systems. Numerous chemical reactions have been successfully performed in micro-reactors and the results convincingly demonstrate with great benefits to aid synthetic procedures, such as purer products, higher yields, shorter reaction times compared to the corresponding batch/macroscale reactions, and more benign reaction conditions. Several ‘proof-of-principle’ examples of molecular imaging probe syntheses using microfluidics, along with basics of device architecture and operation, and their potential limitations are discussed here. PMID:22977436

High density gold nanoparticles immobilized on surface via plasma deposited APTES film for decomposing organic compounds in microchannels

NASA Astrophysics Data System (ADS)

Rao, Xi; Guyon, Cédric; Ognier, Stephanie; Da Silva, Bradley; Chu, Chenglin; Tatoulian, Michaël; Hassan, Ali Abou

2018-05-01

Immobilization of colloidal particles (e.g. gold nanoparticles (AuNps)) on the inner surface of micro-/nano- channels has received a great interest for catalysis. A novel catalytic ozonation setup using a gold-immobilized microchannel reactor was developed in this work. To anchor AuNps, (3-aminopropyl) triethoxysilane (APTES) with functional amine groups was deposited using plasma enhanced chemical vapor deposition (PECVD) process. The results clearly evidenced that PECVD processing exhibited relatively high efficiency for grafting amine groups and further immobilizing AuNPs. The catalytic activity of gold immobilized microchannel was evaluated by pyruvic acid ozonation. The decomposition rate calculated from High Performance Liquid Chromatography (HPLC) indicated a much better catalytic performance of gold in microchannel than that in batch. The results confirmed immobilizing gold nanoparticles on plasma deposited APTES for preparing catalytic microreactors is promising for the wastewater treatment in the future.

Micromotors for "Chemistry-on-the-Fly".

PubMed

Karshalev, Emil; Esteban-Fernández de Ávila, Berta; Wang, Joseph

2018-03-21

This perspective reviews mobile micro/nanomotor scaffolds for performing "chemistry-on-the-fly". Synthetic nano/micromotors offer great versatility and distinct advantages in diverse chemical applications owing to their efficient propulsion and facile surface functionalization that allow these mobile platforms to move and disperse reactive materials across the solution. Such dynamic microreactors have led to accelerated chemical processes, including organic pollutant degradation, metal chelation, biorecognition, redox chemistry, chemical "writing", and a variety of other chemical transformations. Representative examples of such micromotor-enhanced chemical reactions are discussed, focusing on the specific chemical role of these mobile microreactors. The advantages, gaps and limitations of using micromotors as mobile chemical platforms are discussed, concluding with the future prospects of this emerging field. We envision that artificial nano/micromotors will become attractive dynamic tools for speeding up and enhancing "on-the-fly" chemical reactions.

Flash chemistry: flow microreactor synthesis based on high-resolution reaction time control.

PubMed

Yoshida, Jun-ichi

2010-10-01

This article addresses a fascinating aspect of flash chemistry, high-resolution reaction-time control by virtue of a flow microreactor system, and its applications. The length of time that the solution remains inside the reactor is called the residence time. The residence time between the addition of a reagent and that of a quenching agent or the next reagent in a flow microreactor is the reaction time, and the reaction time can be greatly reduced by adjusting the length of a reaction channel in a flow microreactor. This feature is quite effective for conducting reactions involving short-lived reactive intermediates. A reactive species can be generated and transferred to another location to be used in the next reaction before it decomposes by adjusting the residence time in the millisecond to second timescale. The principle of such high-resolution reaction-time control, which can be achieved only by flow microreactors, and its applications to synthetic reactions including Swern-Moffatt-type oxidation, as well as the generation and reactions of aryllithium compounds bearing electrophilic substituents, such as alkoxycarbonyl groups, are presented. Integration of such reactions using integrated flow microreactor systems is also demonstrated. © 2010 The Japan Chemical Journal Forum and Wiley Periodicals, Inc.

Optical fiber-based on-line UV/Vis spectroscopic monitoring of chemical reaction kinetics under high pressure in a capillary microreactor.

PubMed

Benito-Lopez, Fernando; Verboom, Willem; Kakuta, Masaya; Gardeniers, J Han G E; Egberink, Richard J M; Oosterbroek, Edwin R; van den Berg, Albert; Reinhoudt, David N

2005-06-14

With a miniaturized (3 microL volume) fiber-optics based system for on-line measurement by UV/Vis spectroscopy, the reaction rate constants (at different pressures) and the activation volumes (deltaV(not =)) were determined for a nucleophilic aromatic substitution and an aza Diels-Alder reaction in a capillary microreactor.

A novel three-jet microreactor for localized metal-organic chemical vapour deposition of gallium arsenide: design and simulation

NASA Astrophysics Data System (ADS)

Konakov, S. A.; Krzhizhanovskaya, V. V.

2016-08-01

We present a novel three-jet microreactor design for localized deposition of gallium arsenide (GaAs) by low-pressure Metal-Organic Chemical Vapour Deposition (MOCVD) for semiconductor devices, microelectronics and solar cells. Our approach is advantageous compared to the standard lithography and etching technology, since it preserves the nanostructure of the deposited material, it is less time-consuming and less expensive. We designed two versions of reactor geometry with a 10-micron central microchannel for precursor supply and with two side jets of a dilutant to control the deposition area. To aid future experiments, we performed computational modeling of a simplified-geometry (twodimensional axisymmetric) microreactor, based on Navier-Stokes equations for a laminar flow of chemically reacting gas mixture of Ga(CH3)3-AsH3-H2. Simulation results show that we can achieve a high-rate deposition (over 0.3 μm/min) on a small area (less than 30 μm diameter). This technology can be used in material production for microelectronics, optoelectronics, photovoltaics, solar cells, etc.

Theoretical description of spin-selective reactions of radical pairs diffusing in spherical 2D and 3D microreactors

NASA Astrophysics Data System (ADS)

Ivanov, Konstantin L.; Sadovsky, Vladimir M.; Lukzen, Nikita N.

2015-08-01

In this work, we treat spin-selective recombination of a geminate radical pair (RP) in a spherical "microreactor," i.e., of a RP confined in a micelle, vesicle, or liposome. We consider the microreactor model proposed earlier, in which one of the radicals is located at the center of the micelle and the other one undergoes three-dimensional diffusion inside the micelle. In addition, we suggest a two-dimensional model, in which one of the radicals is located at the "pole" of the sphere, while the other one diffuses on the spherical surface. For this model, we have obtained a general analytical expression for the RP recombination yield in terms of the free Green function of two-dimensional diffusion motion. In turn, this Green function is expressed via the Legendre functions and thus takes account of diffusion over a restricted spherical surface and its curvature. The obtained expression allows one to calculate the RP recombination efficiency at an arbitrary magnetic field strength. We performed a comparison of the two models taking the same geometric parameters (i.e., the microreactor radius and the closest approach distance of the radicals), chemical reactivity, magnetic interactions in the RP and diffusion coefficient. Significant difference between the predictions of the two models is found, which is thus originating solely from the dimensionality effect: for different dimensionality of space, the statistics of diffusional contacts of radicals becomes different altering the reaction yield. We have calculated the magnetic field dependence of the RP reaction yield and chemically induced dynamic nuclear polarization of the reaction products at different sizes of the microreactor, exchange interaction, and spin relaxation rates. Interestingly, due to the intricate interplay of diffusional contacts of reactants and spin dynamics, the dependence of the reaction yield on the microreactor radius is non-monotonous. Our results are of importance for (i) interpreting experimental data for magnetic field effects on RP recombination in confined space and (ii) for describing kinetics of chemical reactions, which occur predominantly on the surfaces of biomembranes, i.e., lipid peroxidation reactions.

Theoretical description of spin-selective reactions of radical pairs diffusing in spherical 2D and 3D microreactors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ivanov, Konstantin L., E-mail: ivanov@tomo.nsc.ru; Lukzen, Nikita N.; Novosibirsk State University, Pirogova St. 2, Novosibirsk 630090

2015-08-28

In this work, we treat spin-selective recombination of a geminate radical pair (RP) in a spherical “microreactor,” i.e., of a RP confined in a micelle, vesicle, or liposome. We consider the microreactor model proposed earlier, in which one of the radicals is located at the center of the micelle and the other one undergoes three-dimensional diffusion inside the micelle. In addition, we suggest a two-dimensional model, in which one of the radicals is located at the “pole” of the sphere, while the other one diffuses on the spherical surface. For this model, we have obtained a general analytical expression formore » the RP recombination yield in terms of the free Green function of two-dimensional diffusion motion. In turn, this Green function is expressed via the Legendre functions and thus takes account of diffusion over a restricted spherical surface and its curvature. The obtained expression allows one to calculate the RP recombination efficiency at an arbitrary magnetic field strength. We performed a comparison of the two models taking the same geometric parameters (i.e., the microreactor radius and the closest approach distance of the radicals), chemical reactivity, magnetic interactions in the RP and diffusion coefficient. Significant difference between the predictions of the two models is found, which is thus originating solely from the dimensionality effect: for different dimensionality of space, the statistics of diffusional contacts of radicals becomes different altering the reaction yield. We have calculated the magnetic field dependence of the RP reaction yield and chemically induced dynamic nuclear polarization of the reaction products at different sizes of the microreactor, exchange interaction, and spin relaxation rates. Interestingly, due to the intricate interplay of diffusional contacts of reactants and spin dynamics, the dependence of the reaction yield on the microreactor radius is non-monotonous. Our results are of importance for (i) interpreting experimental data for magnetic field effects on RP recombination in confined space and (ii) for describing kinetics of chemical reactions, which occur predominantly on the surfaces of biomembranes, i.e., lipid peroxidation reactions.« less

Enzymatic synthesis of chiral amino-alcohols by coupling transketolase and transaminase-catalyzed reactions in a cascading continuous-flow microreactor system.

PubMed

Gruber, Pia; Carvalho, Filipe; Marques, Marco P C; O'Sullivan, Brian; Subrizi, Fabiana; Dobrijevic, Dragana; Ward, John; Hailes, Helen C; Fernandes, Pedro; Wohlgemuth, Roland; Baganz, Frank; Szita, Nicolas

2018-03-01

Rapid biocatalytic process development and intensification continues to be challenging with currently available methods. Chiral amino-alcohols are of particular interest as they represent key industrial synthons for the production of complex molecules and optically pure pharmaceuticals. (2S,3R)-2-amino-1,3,4-butanetriol (ABT), a building block for the synthesis of protease inhibitors and detoxifying agents, can be synthesized from simple, non-chiral starting materials, by coupling a transketolase- and a transaminase-catalyzed reaction. However, until today, full conversion has not been shown and, typically, long reaction times are reported, making process modifications and improvement challenging. In this contribution, we present a novel microreactor-based approach based on free enzymes, and we report for the first time full conversion of ABT in a coupled enzyme cascade for both batch and continuous-flow systems. Using the compartmentalization of the reactions afforded by the microreactor cascade, we overcame inhibitory effects, increased the activity per unit volume, and optimized individual reaction conditions. The transketolase-catalyzed reaction was completed in under 10 min with a volumetric activity of 3.25 U ml -1 . Following optimization of the transaminase-catalyzed reaction, a volumetric activity of 10.8 U ml -1 was attained which led to full conversion of the coupled reaction in 2 hr. The presented approach illustrates how continuous-flow microreactors can be applied for the design and optimization of biocatalytic processes. © 2017 The Authors. Biotechnology and Bioengineering Published by Wiley Periodicals, Inc.

FURFURAL YIELD AND DECOMPOSITION IN SODIUM 2,4DIMETHYLBENZENESULFONATE--SULFURIC ACID--WATER SOLUTIONS.

DTIC Science & Technology

Batch-type microreactors (about 1/40 milliliter of reactants) were used to measure furfural yields from acidified xylose solutions containing sodium...It was found that presence of the salt did not affect the quantity of furfural produced, but greatly increased the rate of formation. The regular...increase in rate of furfural formation was directly related to the increase in the rate xylose decomposition, and furfural yields for all salt and acid

A monolithic and flexible fluoropolymer film microreactor for organic synthesis applications.

PubMed

Kim, Jin-Oh; Kim, Heejin; Ko, Dong-Hyeon; Min, Kyoung-Ik; Im, Do Jin; Park, Soo-Young; Kim, Dong-Pyo

2014-11-07

A photocurable and viscous fluoropolymer with chemical stability is a highly desirable material for fabrication of microchemical devices. Lack of a reliable fabrication method, however, limits actual applications for organic reactions. Herein, we report fabrication of a monolithic and flexible fluoropolymer film microreactor and its use as a new microfluidic platform. The fabrication involves facile soft lithography techniques that enable partial curing of thin laminates, which can be readily bonded by conformal contact without any external forces. We demonstrate fabrication of various functional channels (~300 μm thick) such as those embedded with either a herringbone micromixer pattern or a droplet generator. Organic reactions under strongly acidic and basic conditions can be carried out in this film microreactor even at elevated temperature with excellent reproducibility. In particular, the transparent film microreactor with good deformability could be wrapped around a light-emitting lamp for close contact with the light source for efficient photochemical reactions with visible light, which demonstrates easy integration with optical components for functional miniaturized systems.

Limited proteolysis in proteomics using protease-immobilized microreactors.

PubMed

Yamaguchi, Hiroshi; Miyazaki, Masaya; Maeda, Hideaki

2012-01-01

Proteolysis is the key step for proteomic studies integrated with MS analysis. Compared with the conventional method of in-solution digestion, proteolysis by a protease-immobilized microreactor has a number of advantages for proteomic analysis; i.e., rapid and efficient digestion, elimination of a purification step of the digests prior to MS, and high stability against a chemical or thermal denaturant. This chapter describes the preparation of the protease-immobilized microreactors and proteolysis performance of these microreactors. Immobilization of proteases by the formation of a polymeric membrane consisting solely of protease-proteins on the inner wall of the microchannel is performed. This was realized either by a cross-linking reaction in a laminar flow between lysine residues sufficiently present on the protein surfaces themselves or in the case of acidic proteins by mixing them with poly-lysine prior to the crosslink-reaction. The present procedure is simple and widely useful not only for proteases but also for several other enzymes.

Design and Optimization of Coin-Shaped Microreactor Chips for PET Radiopharmaceutical Synthesis

PubMed Central

Elizarov, Arkadij M.; van Dam, R. Michael; Shin, Young Shik; Kolb, Hartmuth C.; Padgett, Henry C.; Stout, David; Shu, Jenny; Huang, Jiang; Daridon, Antoine; Heath, James R.

2010-01-01

An integrated elastomeric microfluidic device, with a footprint the size of a postage stamp, has been designed and optimized for multistep radiosynthesis of PET tracers. Methods The unique architecture of the device is centered around a 5-μL coin-shaped reactor, which yields reaction efficiency and speed from a combination of high reagent concentration, pressurized reactions, and rapid heat and mass transfer. Its novel features facilitate mixing, solvent exchange, and product collection. New mixing mechanisms assisted by vacuum, pressure, and chemical reactions are exploited. Results The architecture of the reported reactor is the first that has allowed batch-mode microfluidic devices to produce radiopharmaceuticals of sufficient quality and quantity to be validated by in vivo imaging. Conclusion The reactor has the potential to produce multiple human doses of 18F-FDG; the most impact, however, is expected in the synthesis of PET radiopharmaceuticals that can be made only with low yields by currently available equipment. PMID:20124050

Concepts for compact mid-IR spectroscopy in photochemistry

NASA Astrophysics Data System (ADS)

Cu-Nguyen, Phuong-Ha; Wang, Ziyu; Zappe, Hans

2016-11-01

Mid-infrared (IR) spectroscopy, typically 3 to 5 µm, is often the technology of choice to monitor the interaction between and concentration of molecules during photochemical reactions. However, classical mid-IR spectrometers are bulky, complex and expensive, making them unsuitable for use in the miniaturized microreactors increasingly being employed for chemical synthesis. We present here the concept for an ultra-miniaturized mid-IR spectrometer directly integrated onto a chemical microreactor to monitor the chemical reaction. The spectrometer is based on micro-machined Fabry-Perot resonator filters realized using pairs of Bragg mirrors to achieve a high spectral resolution. The fabrication of the optical filters is outlined and the measurement of transmittance spectra in the mid-IR range show a good agreement with theory and are thus promising candidates for a fully integrated system.

"Batch" kinetics in flow: online IR analysis and continuous control.

PubMed

Moore, Jason S; Jensen, Klavs F

2014-01-07

Currently, kinetic data is either collected under steady-state conditions in flow or by generating time-series data in batch. Batch experiments are generally considered to be more suitable for the generation of kinetic data because of the ability to collect data from many time points in a single experiment. Now, a method that rapidly generates time-series reaction data from flow reactors by continuously manipulating the flow rate and reaction temperature has been developed. This approach makes use of inline IR analysis and an automated microreactor system, which allowed for rapid and tight control of the operating conditions. The conversion/residence time profiles at several temperatures were used to fit parameters to a kinetic model. This method requires significantly less time and a smaller amount of starting material compared to one-at-a-time flow experiments, and thus allows for the rapid generation of kinetic data. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microfluidic-based photocatalytic microreactor for environmental application: a review of fabrication substrates and techniques, and operating parameters.

PubMed

Das, Susmita; Srivastava, Vimal Chandra

2016-06-08

Photochemical technology with microfluidics is emerging as a new platform in environmental science. Microfluidic technology has various advantages, like better mixing and a shorter diffusion distance for the reactants and products; and uniform distribution of light on the photocatalyst. Depending on the material type and related applications, several fabrication techniques have been adopted by various researchers. Microreactors have been prepared by various techniques, such as lithography, etching, mechanical microcutting technology, etc. Lithography can be classified into photolithography, soft lithography and X-ray lithography techniques whereas the etching process is divided into wet etching (chemical etching) and dry etching (plasma etching) techniques. Several substrates, like polymers, such as polydimethyl-siloxane (PDMS), polymethyle-methacrylate (PMMA), hydrogel, etc.; metals, such as stainless steel, titanium foil, etc.; glass, such as silica capillary, glass slide, etc.; and ceramics have been used for microchannel fabrication. During degradation in a microreactor, the degradation efficiency is affected by few important parameters such as flow rate, initial concentration of the target compound, microreactor dimensions, light intensity, photocatalyst structure and catalyst support. The present paper discusses and critically reviews fabrication techniques and substrates used for microchannel fabrication and critical operating parameters for organics, especially dye degradation in the microreactor. The kinetics of degradation has also been discussed.

I: Hydrodynamic-focusing microreactor II: Mechanically interlocked molecules for functional materials

NASA Astrophysics Data System (ADS)

Coti, Karla Karina

I: Microreactors, a class of microfluidics, offer numerous benefits -- such as small sample requirement, short analysis times and automations -- and have been used to study reactions of chemical and biological reagents. In order to understand the relationship between fast mixing, product regioselectivity, as well as the ability to separate, in time and space, the nanoparticle (NP) formation stages, a microreactor capable of fast and controllable mixing was developed (Chapter 1) based on multi-lamination and hydrodynamic-focusing. By taking advantage of the fast and controllable mixing properties of this novel microreactor one can control the time when chemical reactions commence inside the microchannels. These properties of the microreactor can be exploited to improve the product regioselectivity of a diazo-coupling reaction to attain a product distribution of monoazo to diazo product of ˜1:99, a selectivity unprecedented in both conventional, macroscopic reactors and other microfluidic systems. Additionally, the ability to separate different stages during the NP formation process inside the microreactor, allowed us to study the aggregation of polypyrrole NPs. II: Supramolecular actuators and molecular interlocked molecules, such as catenanes and rotaxanes, have attracted considerable attention because of their sophisticated topology and their application in functional molecular devices. The blending of supramolecular and mechanostereochemistry with mesoporous silica NPs has proven to be a powerful combination, leading to the development of a new class of materials -- mechanized silica nanoparticles ( Chapter 2). These new hybrid materials are designed to release their content in response to an external stimuli and their development is being driven by the need to improve current drug delivery technologies. In an effort to explore how the stimuli-controlled mechanical movement of switchable, bistable [2]rotaxanes -- based on a cyclobis(paraquat-p-phenylene) ring, tetrathiafulvalene and 1,5-dioxynapthalene as the recognition units -- can be exploited to develop new electro-optical liquid crystalline (LC) materials, a novel cholesteric LC bistable [2]rotaxane has been designed (Chapter 3) and its synthesis is underway. Furthermore, the electrochromic behavior of Smectic A LC bistable Rlrotaxanes has been accomplished (Chapter 4) in the condensed LC state as well as within a PMMA polymer matrix.

Design and fabrication of miniaturized PEM fuel cell combined microreactor with self-regulated hydrogen mechanism

NASA Astrophysics Data System (ADS)

Balakrishnan, A.; Frei, M.; Kerzenmacher, S.; Reinecke, H.; Mueller, C.

2015-12-01

In this work we present the design and fabrication of the miniaturized PEM fuel cell combined microreactor system with hydrogen regulation mechanism and testing of prototype microreactor. The system consists of two components (i) fuel cell component and (ii) microreactor component. The fuel cell component represents the miniaturized PEM fuel cell system (combination of screen printed fuel cell assembly and an on-board hydrogen storage medium). Hydrogen production based on catalytic hydrolysis of chemical hydride takes place in the microreactor component. The self-regulated hydrogen mechanism based on the gaseous hydrogen produced from the catalytic hydrolysis of sodium borohydride (NaBH4) gets accumulated as bubbles at the vicinity of the hydrophobic coated hydrogen exhaust holes. When the built up hydrogen bubbles pressure exceeds the burst pressure at the hydrogen exhaust holes the bubble collapses. This collapse causes a surge of fresh NaBH4 solution onto the catalyst surface leading to the removal of the reaction by-products formed at the active sites of the catalyst. The catalyst used in the system is platinum deposited on a base substrate. Nickel foam, carbon porous medium (CPM) and ceramic plate were selected as candidates for base substrate for developing a robust catalyst surface. For the first time the platinum layer fabricated by pulsed electrodeposition and dealloying (EPDD) technique is used for hydrolysis of NaBH4. The major advantages of such platinum catalyst layers are its high surface area and their mechanical stability. Prototype microreactor system with self-regulated hydrogen mechanism is demonstrated.

Applications of Continuous-Flow Photochemistry in Organic Synthesis, Material Science, and Water Treatment.

PubMed

Cambié, Dario; Bottecchia, Cecilia; Straathof, Natan J W; Hessel, Volker; Noël, Timothy

2016-09-14

Continuous-flow photochemistry in microreactors receives a lot of attention from researchers in academia and industry as this technology provides reduced reaction times, higher selectivities, straightforward scalability, and the possibility to safely use hazardous intermediates and gaseous reactants. In this review, an up-to-date overview is given of photochemical transformations in continuous-flow reactors, including applications in organic synthesis, material science, and water treatment. In addition, the advantages of continuous-flow photochemistry are pointed out and a thorough comparison with batch processing is presented.

Enzymatic synthesis of chiral amino‐alcohols by coupling transketolase and transaminase‐catalyzed reactions in a cascading continuous‐flow microreactor system

PubMed Central

Gruber, Pia; Carvalho, Filipe; Marques, Marco P. C.; O'Sullivan, Brian; Subrizi, Fabiana; Dobrijevic, Dragana; Ward, John; Hailes, Helen C.; Fernandes, Pedro; Wohlgemuth, Roland; Baganz, Frank

2017-01-01

Abstract Rapid biocatalytic process development and intensification continues to be challenging with currently available methods. Chiral amino‐alcohols are of particular interest as they represent key industrial synthons for the production of complex molecules and optically pure pharmaceuticals. (2S,3R)‐2‐amino‐1,3,4‐butanetriol (ABT), a building block for the synthesis of protease inhibitors and detoxifying agents, can be synthesized from simple, non‐chiral starting materials, by coupling a transketolase‐ and a transaminase‐catalyzed reaction. However, until today, full conversion has not been shown and, typically, long reaction times are reported, making process modifications and improvement challenging. In this contribution, we present a novel microreactor‐based approach based on free enzymes, and we report for the first time full conversion of ABT in a coupled enzyme cascade for both batch and continuous‐flow systems. Using the compartmentalization of the reactions afforded by the microreactor cascade, we overcame inhibitory effects, increased the activity per unit volume, and optimized individual reaction conditions. The transketolase‐catalyzed reaction was completed in under 10 min with a volumetric activity of 3.25 U ml−1. Following optimization of the transaminase‐catalyzed reaction, a volumetric activity of 10.8 U ml−1 was attained which led to full conversion of the coupled reaction in 2 hr. The presented approach illustrates how continuous‐flow microreactors can be applied for the design and optimization of biocatalytic processes. PMID:28986983

Ultrapyrolytic upgrading of plastic wastes and plastics/heavy oil mixtures to valuable light gas products

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lovett, S.; Berruti, F.; Behie, L.A.

1997-11-01

Viable operating conditions were identified experimentally for maximizing the production of high-value products such as ethylene, propylene, styrene, and benzene, from the ultrapyrolysis of waste plastics. Using both a batch microreactor and a pilot-plant-sized reactor, the key operating variables considered were pyrolysis temperature, product reaction time, and quench time. In the microreactor experiments, polystyrene (PS), a significant component of waste plastics, was pyrolyzed at temperatures ranging from 800 to 965 C, with total reaction times ranging from 500 to 1,000 ms. At a temperature of 965 C and 500 ms, the yields of styrene plus benzene were greater than 95more » wt %. In the pilot-plant experiments, the recently patented internally circulating fluidized bed (ICFB) reactor (Milne et al., US Patent Number 5,370,789, 1994b) was used to ultrapyrolyze low-density polyethylene (LDPE) in addition to LDPE (5% by weight)/heavy oil mixtures at a residence time of 600 ms. Both experiments produced light olefin yields greater than 55 wt % at temperatures above 830 C.« less

Sustainable efficient way for opioid peptide LVV-h7 preparation from enzymatic proteolysis in a microfluidic-based reaction-extraction process with solvent recycling.

PubMed

Elagli, Adil; Belhacene, Kalim; Dhulster, Pascal; Froidevaux, Renato

2016-05-01

LVV-h7 (LVVYPWTQFR) is a bioactive peptide that can be obtained from blood as waste of food industry, more precisely from hemoglobin hydrolysis by pepsin. This opioid peptide belongs to the hemorphins family and have strong physiological effects that bring its use in pharmaceutics and various therapeutic treatments attractive, in particular for substituting its costly chemically synthetized analogous. Hemoglobin hydrolysis by pepsin generates a huge variety of peptides among whose LVV-h7 can be purified by liquid-liquid extraction (LLE). Herein, selective preparation of this peptide is proposed by a microfluidic-based continuous reaction-separation process. Hemoglobin hydrolysis in microreactor was firstly coupled to LVV-h7 LLE in octan-1-ol and then coupled to LVV-h7 back LLE in acidic water. This continuous process allowed to prepare pure LVV-h7, as confirmed by liquid chromatography and mass spectrometry. The microfluidic circuit also allowed octan-1-ol recycling in a closed loop, making this method more sustainable than similar biphasic batch process. Copyright © 2016 Elsevier B.V. All rights reserved.

An Easy-to-Machine Electrochemical Flow Microreactor: Efficient Synthesis of Isoindolinone and Flow Functionalization.

PubMed

Folgueiras-Amador, Ana A; Philipps, Kai; Guilbaud, Sébastien; Poelakker, Jarno; Wirth, Thomas

2017-11-27

Flow electrochemistry is an efficient methodology to generate radical intermediates. An electrochemical flow microreactor has been designed and manufactured to improve the efficiency of electrochemical flow reactions. With this device only little or no supporting electrolytes are needed, making processes less costly and enabling easier purification. This is demonstrated by the facile synthesis of amidyl radicals used in intramolecular hydroaminations to produce isoindolinones. The combination with inline mass spectrometry facilitates a much easier combination of chemical steps in a single flow process. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

An RF-Powered Micro-Reactor for Efficient Extraction and Hydrolysis

NASA Astrophysics Data System (ADS)

Scott, V.

2014-12-01

An RF sample-processing micro-reactor that was developed as part of potential in situ Exploration Missions to inner- and outer-planetary bodies was designed to utilize aqueous solutions subjected to 60 GHz radiation at 730 mW of input power to extract target organic compounds and molecular and inorganic ions as well as to hydrolyze complex polymeric materials. Successful identification and characterization of these molecules relies on the sample-processing techniques utilized alongside state-of-the-art detection and analysis. For mass and power restrictions put on space exploration missions, smaller and more efficient instruments are highly desirable. The RF micro-reactor potentially offers a simplified alternative to the typical gold-standard extractions that often use solvents, chemicals, and conditions that can vary wildly and depend on the targeted molecules. Instead, this instrument uses a single solvent ­— water — that can be "tuned" under the different experimental conditions, leveraging the operating principles of the Sub-Critical Water Extractor. Proof-of-concept experiments examining the hydrolysis of glycosidic and peptide bonds were successful in demonstrating the RF micro-reactor's capabilities. Progress toward coupling the reactor with a micro-scale sample-handling system enabling slurry delivery has been made and preliminary results on heterogeneous reactions and extractions will be presented.

Continuous and rapid synthesis of nanoclusters and nanocrystals using scalable microstructured reactors

NASA Astrophysics Data System (ADS)

Jin, Hyung Dae

Recent advances in nanocrystalline materials production are expected to impact the development of next generation low-cost and/or high efficiency solar cells. For example, semiconductor nanocrystal inks are used to lower the fabrication cost of the absorber layers of the solar cells. In addition, some quantum confined nanocrystals display electron-hole pair generation phenomena with greater than 100% quantum yield, called multiple exciton generation (MEG). These quantum dots could potentially be used to fabricate solar cells that exceed the Schockley-Queisser limit. At present, continuous syntheses of nanoparticles using microreactors have been reported by several groups. Microreactors have several advantages over conventional batch synthesis. One advantage is their efficient heat transfer and mass transport. Another advantage is the drastic reduction in the reaction time, in many cases, down to minutes from hours. Shorter reaction time not only provides higher throughput but also provide better particle size control by avoiding aggregation and by reducing probability of oxidizing precursors. In this work, room temperature synthesis of Au11 nanoclusters and high temperature synthesis of chalcogenide nanocrystals were demonstrated using continuous flow microreactors with high throughputs. A high rate production of phosphine-stabilized Au11 nanoclusters was achieved using a layer-up strategy which involves the use of microlamination architectures; the patterning and bonding of thin layers of material (laminae) to create a multilayered micromixer in the range of 25-250 mum thick was used to step up the production of phosphine-stabilized Au11 nanoclusters. Continuous production of highly monodispersed phosphine-stabilized Au 11 nanoclusters at a rate of about 11.8 [mg/s] was achieved using a microreactor with a size of 1.687cm3. This result is about 30,000 times over conventional batch synthesis according to production rate/per reactor volume. We have elucidated the formation mechanism of CuInSe2 nanocrystals for the development of a continuous flow process for their synthesis. It was found that copper-rich CuInSe2 with a sphalerite structure was formed initially followed by the formation of more ordered CuInSe2 at longer reaction times, along with the formation of Cu2Se and In2Se3. It was found that Cu2Se was formed at a much faster rate than In2Se3 under the same reaction conditions. By adjusting the Cu/In precursor ratio, we were able to develop a very rapid and simple synthesis of CuInSe2 nanocrystals using a continuous flow microreactor with a high throughput per reactor volume. The microreactor has a simple design which uses readily available low cost components. It comprised an inner microtube to precisely control the injection of TOPSe into a larger diameter tube that preheated CuCl and InCl3 hot mixture was pumped through. Rapid injection plays an important role in dividing the nucleation and growth process which is crucial in getting narrow size distribution. The design of this microreactor also has the advantages of alleviating sticking of QDs on the growth channel wall since QDs were formed from the center of the reactor. Furthermore, size-controlled synthesis of CuInSe2 nanocrystals was achieved using this reactor simply by adjusting ratio between coordinating solvents. Semiconductors with a direct bandgap between 1 and 2eV including Cu(In,Ga)Se 2 (1.04--1.6eV) and CuIn(Se,S)2 (1.04--1.53eV) are ideal for single junction cells utilize the visible spectrum. However, half of the solar energy available to the Earth lies in the infrared region. Inorganic QD-based solar cells with a decent efficiency near 1.5 mum have been reported. Therefore, syntheses of narrow gap IV-VI (SnTe, PbS, PbSe, PbTe), II-IV (HgTe, CdXHg1-XTe), and III-V (InAs) QDs have attracted significant attention and these materials have potential uses for a variety of other optical, electronic, and optoelectronic applications. SnTe with an energy gap of 0.18eV at 300K can be used for IR photodetectors, laser diodes, and thermophotovoltaic energy converters. First continuous synthesis of shape-controlled SnTe nanocrystals were also accomplished in this work. SnCl2, and TOPTe were used as reactants successfully in coordinating OA and TOP solvents. Both rod shape and dot shape SnTe nanocrystals with uniform size distributions could be obtained. A blue shift was observed from these SnTe nanocrystals. Production rate at about 5mg/min (300mg/hr) was achieved using a microreactor at a size of 1.78cm3.

Multichannel quench-flow microreactor chip for parallel reaction monitoring.

PubMed

Bula, Wojciech P; Verboom, Willem; Reinhoudt, David N; Gardeniers, Han J G E

2007-12-01

This paper describes a multichannel silicon-glass microreactor which has been utilized to investigate the kinetics of a Knoevenagel condensation reaction under different reaction conditions. The reaction is performed on the chip in four parallel channels under identical conditions but with different residence times. A special topology of the reaction coils overcomes the common problem arising from the difference in pressure drop of parallel channels having different length. The parallelization of reaction coils combined with chemical quenching at specific locations results in a considerable reduction in experimental effort and cost. The system was tested and showed good reproducibility in flow properties and reaction kinetic data generation.

A novel microreactor approach for analysis of ketones and aldehydes in breath.

PubMed

Fu, Xiao-An; Li, Mingxiao; Biswas, Souvik; Nantz, Michael H; Higashi, Richard M

2011-11-21

We report a fabricated microreactor with thousands of micropillars in channels. Each micropillar surface is chemically functionalized to selectively preconcentrate gaseous ketones and aldehydes of exhaled breath and to enhance ultra-trace, rapid analysis by direct-infusion Fourier transform-ion cyclotron resonance (FT-ICR) mass spectrometry (MS). The micropillar reactive coating contains the quaternary ammonium aminooxy salt 2-(aminooxy)ethyl-N,N,N-trimethylammonium iodide (ATM) for capturing trace carbonyl VOCs by means of an oximation reaction. We demonstrate the utility of this approach for detection of C(1) to C(12) aldehydes and ketones in exhaled breath, but the approach is applicable to any gaseous sample.

Six-flow operations for catalyst development in Fischer-Tropsch synthesis: Bridging the gap between high-throughput experimentation and extensive product evaluation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sartipi, Sina, E-mail: S.Sartipi@tudelft.nl, E-mail: J.Gascon@tudelft.nl; Jansma, Harrie; Bosma, Duco

2013-12-15

Design and operation of a “six-flow fixed-bed microreactor” setup for Fischer-Tropsch synthesis (FTS) is described. The unit consists of feed and mixing, flow division, reaction, separation, and analysis sections. The reactor system is made of five heating blocks with individual temperature controllers, assuring an identical isothermal zone of at least 10 cm along six fixed-bed microreactor inserts (4 mm inner diameter). Such a lab-scale setup allows running six experiments in parallel, under equal feed composition, reaction temperature, and conditions of separation and analysis equipment. It permits separate collection of wax and liquid samples (from each flow line), allowing operation with highmore » productivities of C5+ hydrocarbons. The latter is crucial for a complete understanding of FTS product compositions and will represent an advantage over high-throughput setups with more than ten flows where such instrumental considerations lead to elevated equipment volume, cost, and operation complexity. The identical performance (of the six flows) under similar reaction conditions was assured by testing a same catalyst batch, loaded in all microreactors.« less

A microfluidic microreactor for the synthesis of gold nanorods.

PubMed

Day, Daniel; Gu, Min

2009-03-11

A microfluidic microreactor for the synthesis of gold nanorods is fabricated using femtosecond pulse laser microfabrication techniques. Femtosecond pulse lasers are able to etch a wide range of materials that are required for a microreactor, from the photomasks to the microheaters. The heating of the fluid in the microreactor is achieved through the design and fabrication of a microscale heating element incorporated onto the bottom surface of the microreactor which is capable of reaching temperatures greater than 130 degrees C. Computational fluid dynamic simulations of the heating profile of an optimized microreactor show increased heating performance with respect to a serpentine microreactor. The synthesis of gold nanorods is demonstrated in the optimized microreactor, based on a flow rate of 0.5 microg min(-1).

Dose-on-demand production of diverse 18F-radiotracers for preclinical applications using a continuous flow microfluidic system.

PubMed

Matesic, Lidia; Kallinen, Annukka; Greguric, Ivan; Pascali, Giancarlo

2017-09-01

The production of 18 F-radiotracers using continuous flow microfluidics is under-utilized due to perceived equipment limitations. We describe the dose-on-demand principle, whereby the back-to-back production of multiple, diverse 18 F-radiotracers can be prepared on the same day, on the same microfluidic system using the same batch of [ 18 F]fluoride, the same microreactor, the same HPLC column and SPE cartridge to obtain a useful production yield. [ 18 F]MEL050, [ 18 F]Fallypride and [ 18 F]PBR111 were radiolabeled with [ 18 F]fluoride using the Advion NanoTek Microfluidic Synthesis System. The outlet of the microreactor was connected to an automated HPLC injector and following the collection of the product, SPE reformulation produced the 18 F-radiotracer in <10% ethanolic saline. A thorough automated cleaning procedure was implemented to ensure no cross-contamination between radiotracer synthesis. The complete productions for [ 18 F]MEL050 and [ 18 F]Fallypride were performed at total flow rates of 20μL/min, resulting in 40±13% and 25±13% RCY respectively. [ 18 F]PBR111 was performed at 200μL/min to obtain 27±8% RCY. Molar activities for each 18 F-radiotracer were >100GBq/μmol and radiochemical purities were >97%, implying that the cleaning procedure was effective. Using the same initial solution of [ 18 F]fluoride, microreactor, HPLC column and SPE cartridge, three diverse 18 F-radiotracers could be produced in yields sufficient for preclinical studies in a back-to-back fashion using a microfluidic system with no detectable cross-contamination. Crown Copyright © 2017. Published by Elsevier Inc. All rights reserved.

Construction of graphene oxide magnetic nanocomposites-based on-chip enzymatic microreactor for ultrasensitive pesticide detection.

PubMed

Liang, Ru-Ping; Wang, Xiao-Ni; Liu, Chun-Ming; Meng, Xiang-Ying; Qiu, Jian-Ding

2013-11-08

A new strategy for facile construction of graphene oxide magnetic nanocomposites (GO/Fe3O4 MNCs)-based on-chip enzymatic microreactor and ultrasensitive pesticide detection has been proposed. GO/Fe3O4 MNCs were first prepared through an in situ chemical deposition strategy. Then, acetylcholinesterase (AChE) was adsorbed onto the GO/Fe3O4 surface to form GO/Fe3O4/AChE MNCs which was locally packed into PDMS microchannel simply with the help of external magnetic field to form an on-chip enzymatic microreactor. The constructed GO/Fe3O4/AChE MNCs-based enzymatic microreactor not only have the magnetism of Fe3O4 NPs that make them conveniently manipulated by an external magnetic field, but also have the larger surface and excellent biocompatibility of graphene which can incorporate much more AChE molecules and well maintain their biological activity. On the basis of the AChE inhibition principle, a novel on-chip enzymatic microreactor was constructed for analyzing dimethoate which is usually used as a model of organophosphorus pesticides. Under optimal conditions, a linear relationship between the inhibition rates of AChE and the concentration of dimethoate from 1 to 20 μgL(-1) with a detection limit of 0.18 μgL(-1) (S/N=3) was obtained. The developed electrophoretic and magnetic-based chip exhibited excellent reproducibility and stability with no decrease in the activity of enzyme for more than 20 repeated measurements over one week period, which provided a new and promising tool for the analysis of enzyme inhibitors with low cost and excellent performance. Copyright © 2013 Elsevier B.V. All rights reserved.

A high efficiency microfluidic-based photocatalytic microreactor using electrospun nanofibrous TiO2 as a photocatalyst

NASA Astrophysics Data System (ADS)

Meng, Zhaoxu; Zhang, Xu; Qin, Jianhua

2013-05-01

We present a novel microfluidic-based photocatalytic microreactor by using electrospun nanofibrous TiO2 as a photocatalyst for the first time. The microreactor exhibits not only a simple fabrication process, but also much higher photocatalytic activity than that achieved by a TiO2 film microreactor.We present a novel microfluidic-based photocatalytic microreactor by using electrospun nanofibrous TiO2 as a photocatalyst for the first time. The microreactor exhibits not only a simple fabrication process, but also much higher photocatalytic activity than that achieved by a TiO2 film microreactor. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr00775h

Microchemical Pen: An Open Microreactor for Region-Selective Surface Modification.

PubMed

Mao, Sifeng; Sato, Chiho; Suzuki, Yuma; Yang, Jianmin; Zeng, Hulie; Nakajima, Hizuru; Yang, Ming; Lin, Jin-Ming; Uchiyama, Katsumi

2016-10-18

Various micro surface-modification approaches including photolithography, dip-pen lithography and ink-jet systems have been developed and used to extend the functionalities of solid surfaces. While those approaches work in the "open space", push-pull systems which work in solutions have recently drawn considerable attention. However, the confining flows performed by push-pull systems have realized only the dispense process, while microscale, region-selective chemical reactions have remained unattainable. This study reports a microchemical pen that enables region-selective chemical reactions for the micro surface modification/patterning. The chemical pen is based on the principle of microfluidic laminar flows and the resulting mixing of reagents by the mutual diffusion. The tiny diffusion layer performs as the working region. This report represents the first demonstration of an open microreactor in which two different reagents react on a real solid sample. The multifunctional characteristics of the microchemical pen are confirmed by different types of reactions in many research areas, including inorganic chemistry, polymer science, electrochemistry and biological sample treatment. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Acetylcholinesterase-Based Electrochemical Multiphase Microreactor for Detection of Organophosphorous Compounds (Preprint)

DTIC Science & Technology

2007-04-01

target molecules, we are interested in incorporating the existing, liquid AChE sensor chemistry into a multiphase microreactor . The multiphase... microreactor will play a critical role in combining microsensor technology with analytical biochemistry and increase reaction time, sensitivity and... microreactor with a micro-scale gas- liquid interface, 2) to adapt AChE biochemistry into the microreactor in order to develop an electrochemical biosensor for

A PORTABLE MICROREACTOR SYSTEM TO SYNTHESIZE HYDROGEN PEROXIDE - PHASE I

EPA Science Inventory

In the event that vehicles of buildings become contaminated by hazardous chemical or biological materials, a well-studied and effective decontaminant is hydrogen peroxide vapor (HPV).  Unfortunately, the current technology for generating HPV requires 35 weight percent hydro...

Chip-based device for parallel sorting, amplification, detection, and identification of nucleic acid subsequences

DOE Office of Scientific and Technical Information (OSTI.GOV)

Beer, Neil Reginald; Colston, Jr, Billy W.

An apparatus for chip-based sorting, amplification, detection, and identification of a sample having a planar substrate. The planar substrate is divided into cells. The cells are arranged on the planar substrate in rows and columns. Electrodes are located in the cells. A micro-reactor maker produces micro-reactors containing the sample. The micro-reactor maker is positioned to deliver the micro-reactors to the planar substrate. A microprocessor is connected to the electrodes for manipulating the micro-reactors on the planar substrate. A detector is positioned to interrogate the sample contained in the micro-reactors.

A high efficiency microfluidic-based photocatalytic microreactor using electrospun nanofibrous TiO2 as a photocatalyst.

PubMed

Meng, Zhaoxu; Zhang, Xu; Qin, Jianhua

2013-06-07

We present a novel microfluidic-based photocatalytic microreactor by using electrospun nanofibrous TiO2 as a photocatalyst for the first time. The microreactor exhibits not only a simple fabrication process, but also much higher photocatalytic activity than that achieved by a TiO2 film microreactor.

Microreactor of Pd nanoparticles immobilized hollow microspheres for catalytic hydrodechlorination of chlorophenols in water.

PubMed

Lan, Yang; Yang, Li; Zhang, Minchao; Zhang, Wangqing; Wang, Shengnan

2010-01-01

A microreactor of Pd nanoparticles immobilized shell-corona hollow microspheres of poly[styrene-co-2-(acetoacetoxy) ethyl methacrylate-co-acrylamide] has been designed for catalytic hydrodechlorination (HDC) of chlorophenols in the sole solvent of water. The strategy of the combined use of the shell-corona hollow microspheres as microcapsule and catalyst scaffold endues the microreactor several advantages. First, the microreactor can be dispersed in the sole solvent of water and acts as a quasi-homogeneous catalyst for catalytic HDC of chlorophenols. Second, the reactant of chlorophenols can be highly concentrated within the hollow microspheres of the microreactor in the sole solvent of water. Third, the resultant product of phenol can be favorably excreted off the microreactor into water because of the polar difference between the reactant of chlorophenols and the product of phenol. Ascribed to the combined advantages, catalytic HDC of chlorophenols can be performed efficiently within the microreactor in the sole solvent of water at room temperature under atmosphere pressure.

Synthesis of copper nanocolloids using a continuous flow based microreactor

NASA Astrophysics Data System (ADS)

Xu, Lei; Peng, Jinhui; Srinivasakannan, C.; Chen, Guo; Shen, Amy Q.

2015-11-01

The copper (Cu) nanocolloids were prepared by sodium borohydride (NaBH4) reduction of metal salt solutions in a T-shaped microreactor at room temperature. The influence of NaBH4 molar concentrations on copper particle's diameter, morphology, size distribution, and elemental compositions has been investigated by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The ultraviolet-visible spectroscopy (UV-vis) was used to verify the chemical compounds of nanocolloids and estimate the average size of copper nanocolloids. The synthesized copper nanocolloids were uniform in size and non-oxidized. A decrease in the mean diameter of copper nanocolloids was observed with increasing NaBH4 molar concentrations. The maximum mean diameter (4.25 nm) occurred at the CuSO4/NaBH4 molar concentration ratio of 1:2.

Fluorogenic DNA Sequencing in PDMS Microreactors

PubMed Central

Sims, Peter A.; Greenleaf, William J.; Duan, Haifeng; Xie, X. Sunney

2012-01-01

We have developed a multiplex sequencing-by-synthesis method combining terminal-phosphate labeled fluorogenic nucleotides (TPLFNs) and resealable microreactors. In the presence of phosphatase, the incorporation of a non-fluorescent TPLFN into a DNA primer by DNA polymerase results in a fluorophore. We immobilize DNA templates within polydimethylsiloxane (PDMS) microreactors, sequentially introduce one of the four identically labeled TPLFNs, seal the microreactors, allow template-directed TPLFN incorporation, and measure the signal from the fluorophores trapped in the microreactors. This workflow allows sequencing in a manner akin to pyrosequencing but without constant monitoring of each microreactor. With cycle times of <10 minutes, we demonstrate 30 base reads with ∼99% raw accuracy. “Fluorogenic pyrosequencing” combines benefits of pyrosequencing, such as rapid turn-around, native DNA generation, and single-color detection, with benefits of fluorescence-based approaches, such as highly sensitive detection and simple parallelization. PMID:21666670

A high efficiency microreactor with Pt/ZnO nanorod arrays on the inner wall for photodegradation of phenol.

PubMed

Zhang, Quan; Zhang, Qinghong; Wang, Hongzhi; Li, Yaogang

2013-06-15

A high efficiency microreactor with Pt coated ZnO (Pt/ZnO) nanorod arrays on the inner wall was successfully fabricated by pumping a Pt sol into the microchannel containing preformed ZnO nanorod arrays. Phenol was selected as a persistent organic pollutant to evaluate the photocatalytic performance of the microreactors. The microreactor which was coated by Pt sol for 5 min showed the best photocatalytic performance compared with other Pt/ZnO nanorod array-modified microreactors. The presence of Pt nanoparticles on the surfaces of ZnO nanorods promoted the separation of photoinduced electron-hole pairs and thus enhanced the photocatalytic activity. In addition, the recyclable property of the microcreator was investigated. It was found that the microreactor displayed higher durability during the continuous photocatalytic process. Copyright © 2013 Elsevier B.V. All rights reserved.

Operando characterization of catalysts through use of a portable microreactor

DOE PAGES

Zhao, Shen; Li, Yuanyuan; Stavitski, Eli; ...

2015-10-09

To provide new understandings of the mechanisms of catalytic reactions, improved methods are needed than can monitor changes in the electronic, structural and chemical properties of catalysts, doing so in the operando conditions in which catalysts work. We describe here a microreactor-based approach that integrates the capabilities of advanced x-ray, electron, optical and gas-phase compositional analysis techniques in operando conditions. For several exemplary catalytic systems, we demonstrate how this approach enables characterization of three major factors contributing to structure-property correlations evidenced in heterogeneously catalyzed reactions, namely: the atomic structure and elemental compositions of nanocatalysts; the physiochemical properties of the supportmore » and catalyst-support interfaces; and the gas and surface-phase chemistry occurring under operando conditions. We highlight the generality of the approach as well as outline opportunities for future developments.« less

An Optically Accessible Pyrolysis Microreactor

NASA Astrophysics Data System (ADS)

Baraban, Joshua H.; David, Donald E.; Ellison, Barney; Daily, John W.

2016-06-01

We report an optically accessible pyrolysis micro-reactor suitable for in situ laser spectroscopic measurements. A radiative heating design allows for completely unobstructed views of the micro-reactor along two axes. The maximum temperature demonstrated here is only 1300 K (as opposed to 1700 K for the usual SiC micro-reactor) because of the melting point of fused silica, but alternative transparent materials will allow for higher temperatures. Laser induced fluorescence measurements on nitric oxide are presented as a proof of principle for spectroscopic characterization of pyrolysis conditions. (This work has been published in J. H. Baraban, D. E. David, G. B. Ellison, and J. W. Daily. An Optically Accessible Pyrolysis Micro-Reactor. Review of Scientific Instruments, 87(1):014101, 2016.)

The silicon-glass microreactor with embedded sensors—technology and results of preliminary qualitative tests, toward intelligent microreaction plant

NASA Astrophysics Data System (ADS)

Knapkiewicz, P.

2013-03-01

The technology and preliminary qualitative tests of silicon-glass microreactors with embedded pressure and temperature sensors are presented. The concept of microreactors for leading highly exothermic reactions, e.g. nitration of hydrocarbons, and design process-included computer-aided simulations are described in detail. The silicon-glass microreactor chip consisting of two micromixers (multistream micromixer), reaction channels, cooling/heating chambers has been proposed. The microreactor chip was equipped with a set of pressure and temperature sensors and packaged. Tests of mixing quality, pressure drops in channels, heat exchange efficiency and dynamic behavior of pressure and temperature sensors were documented. Finally, two applications were described.

A dual-core double emulsion platform for osmolarity-controlled microreactor triggered by coalescence of encapsulated droplets.

PubMed

Guan, Xuewei; Hou, Likai; Ren, Yukun; Deng, Xiaokang; Lang, Qi; Jia, Yankai; Hu, Qingming; Tao, Ye; Liu, Jiangwei; Jiang, Hongyuan

2016-05-01

Droplet-based microfluidics has provided a means to generate multi-core double emulsions, which are versatile platforms for microreactors in materials science, synthetic biology, and chemical engineering. To provide new opportunities for double emulsion platforms, here, we report a glass capillary microfluidic approach to first fabricate osmolarity-responsive Water-in-Oil-in-Water (W/O/W) double emulsion containing two different inner droplets/cores and to then trigger the coalescence between the encapsulated droplets precisely. To achieve this, we independently control the swelling speed and size of each droplet in the dual-core double emulsion by controlling the osmotic pressure between the inner droplets and the collection solutions. When the inner two droplets in one W/O/W double emulsion swell to the same size and reach the instability of the oil film interface between the inner droplets, core-coalescence happens and this coalescence process can be controlled precisely. This microfluidic methodology enables the generation of highly monodisperse dual-core double emulsions and the osmolarity-controlled swelling behavior provides new stimuli to trigger the coalescence between the encapsulated droplets. Such swelling-caused core-coalescence behavior in dual-core double emulsion establishes a novel microreactor for nanoliter-scale reactions, which can protect reaction materials and products from being contaminated or released.

A dual-core double emulsion platform for osmolarity-controlled microreactor triggered by coalescence of encapsulated droplets

PubMed Central

Guan, Xuewei; Hou, Likai; Ren, Yukun; Deng, Xiaokang; Lang, Qi; Jia, Yankai; Hu, Qingming; Tao, Ye; Liu, Jiangwei; Jiang, Hongyuan

2016-01-01

Droplet-based microfluidics has provided a means to generate multi-core double emulsions, which are versatile platforms for microreactors in materials science, synthetic biology, and chemical engineering. To provide new opportunities for double emulsion platforms, here, we report a glass capillary microfluidic approach to first fabricate osmolarity-responsive Water-in-Oil-in-Water (W/O/W) double emulsion containing two different inner droplets/cores and to then trigger the coalescence between the encapsulated droplets precisely. To achieve this, we independently control the swelling speed and size of each droplet in the dual-core double emulsion by controlling the osmotic pressure between the inner droplets and the collection solutions. When the inner two droplets in one W/O/W double emulsion swell to the same size and reach the instability of the oil film interface between the inner droplets, core-coalescence happens and this coalescence process can be controlled precisely. This microfluidic methodology enables the generation of highly monodisperse dual-core double emulsions and the osmolarity-controlled swelling behavior provides new stimuli to trigger the coalescence between the encapsulated droplets. Such swelling-caused core-coalescence behavior in dual-core double emulsion establishes a novel microreactor for nanoliter-scale reactions, which can protect reaction materials and products from being contaminated or released. PMID:27279935

Inverse problem analysis for identification of reaction kinetics constants in microreactors for biodiesel synthesis

NASA Astrophysics Data System (ADS)

Pontes, P. C.; Naveira-Cotta, C. P.

2016-09-01

The theoretical analysis for the design of microreactors in biodiesel production is a complicated task due to the complex liquid-liquid flow and mass transfer processes, and the transesterification reaction that takes place within these microsystems. Thus, computational simulation is an important tool that aids in understanding the physical-chemical phenomenon and, consequently, in determining the suitable conditions that maximize the conversion of triglycerides during the biodiesel synthesis. A diffusive-convective-reactive coupled nonlinear mathematical model, that governs the mass transfer process during the transesterification reaction in parallel plates microreactors, under isothermal conditions, is here described. A hybrid numerical-analytical solution via the Generalized Integral Transform Technique (GITT) for this partial differential system is developed and the eigenfunction expansions convergence rates are extensively analyzed and illustrated. The heuristic method of Particle Swarm Optimization (PSO) is applied in the inverse analysis of the proposed direct problem, to estimate the reaction kinetics constants, which is a critical step in the design of such microsystems. The results present a good agreement with the limited experimental data in the literature, but indicate that the GITT methodology combined with the PSO approach provide a reliable computational algorithm for direct-inverse analysis in such reactive mass transfer problems.

Triple-channel microreactor for biphasic gas-liquid reactions: Photosensitized oxygenations.

PubMed

Maurya, Ram Awatar; Park, Chan Pil; Kim, Dong-Pyo

2011-01-01

A triple-channel microreactor fabricated by means of a soft-lithography technique was devised for efficient biphasic gas-liquid reactions. The excellent performance of the microreactor was demonstrated by carrying out photosensitized oxygenations of α-terpinene, citronellol, and allyl alcohols.

An optically accessible pyrolysis microreactor

NASA Astrophysics Data System (ADS)

Baraban, J. H.; David, D. E.; Ellison, G. Barney; Daily, J. W.

2016-01-01

We report an optically accessible pyrolysis micro-reactor suitable for in situ laser spectroscopic measurements. A radiative heating design allows for completely unobstructed views of the micro-reactor along two axes. The maximum temperature demonstrated here is only 1300 K (as opposed to 1700 K for the usual SiC micro-reactor) because of the melting point of fused silica, but alternative transparent materials will allow for higher temperatures. Laser induced fluorescence measurements on nitric oxide are presented as a proof of principle for spectroscopic characterization of pyrolysis conditions.

An optically accessible pyrolysis microreactor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baraban, J. H.; Ellison, G. Barney; David, D. E.

2016-01-15

We report an optically accessible pyrolysis micro-reactor suitable for in situ laser spectroscopic measurements. A radiative heating design allows for completely unobstructed views of the micro-reactor along two axes. The maximum temperature demonstrated here is only 1300 K (as opposed to 1700 K for the usual SiC micro-reactor) because of the melting point of fused silica, but alternative transparent materials will allow for higher temperatures. Laser induced fluorescence measurements on nitric oxide are presented as a proof of principle for spectroscopic characterization of pyrolysis conditions.

Triple-channel microreactor for biphasic gas–liquid reactions: Photosensitized oxygenations

PubMed Central

Maurya, Ram Awatar; Park, Chan Pil

2011-01-01

Summary A triple-channel microreactor fabricated by means of a soft-lithography technique was devised for efficient biphasic gas–liquid reactions. The excellent performance of the microreactor was demonstrated by carrying out photosensitized oxygenations of α-terpinene, citronellol, and allyl alcohols. PMID:21915221

Patterning of colloidal particles in the galvanic microreactor

NASA Astrophysics Data System (ADS)

Jan, Linda

A Cu-Au galvanic microreactor is used to demonstrate the autonomous patterning of two-dimensional colloidal crystals with spatial and orientational order which are adherent to the electrode substrate. The microreactor is comprised of a patterned array of copper and gold microelectrodes in a coplanar arrangement that is immersed in a dilute hydrochloric acid solution in which colloidal polystyrene microspheres are suspended. During the electrochemical dissolution of copper, polystyrene colloids are transported to the copper electrodes. The spatial arrangement of the electrodes determines whether the colloids initiate aggregation at the edges or centers of the copper electrodes. Depending on the microreactor parameters, two-dimensional colloidal crystals can form and adhere to the electrode. This thesis investigates the mechanisms governing the autonomous particle motion, the directed particle trajectory (inner- versus edge-aggregation) as affected by the spatial patterning of the electrodes, and the adherence of the colloidal particles onto the substrate. Using in situ current density measurements, particle velocimetry, and order-of-magnitude arguments, it is shown that particle motion is governed by bulk fluid motion and electrophoresis induced by the electrochemical reactions. Bulk electrolyte flow is most likely driven by electrochemical potential gradients of reaction products formed during the inhomogeneous copper dissolution, particularly due to localized high current density at the electrode junction. Preferential aggregation of the colloidal particles resulting in inner- and edge-aggregation is influenced by changes to the flow pattern in response to difference in current density profiles as affected by the spatial patterning of the electrode. Finally, by determining the onset of particle cementation through particle tracking analysis, and by monitoring the deposition of reaction products through the observation of color changes of the galvanic electrodes in situ, it is shown that particle cementation coincides with the precipitation and deposition of reaction products. The precipitation process is caused by shifts in the chemical equilibria of the microreactor due to changes in the composition of the electrolyte during the reactions, which can be used to control particle cementation. The corrosion driven transport, deposition and adherence of colloidal particles at corrosion sites have implications for the development of autonomous self-healing materials.

Droplet-based microreactor for synthesis of water-soluble Ag₂S quantum dots.

PubMed

Shu, Yun; Jiang, Peng; Pang, Dai-Wen; Zhang, Zhi-Ling

2015-07-10

A droplet-based microreactor was used for synthesis of water-soluble Ag2S quantum dots (QDs). Monodispersed Ag2S nanoparticles with a surface of carboxylic acid-terminated were synthesized in the droplet microreactor. The x-ray powder diffraction results indicated products were monoclinic Ag2S nanocrystals. Furthermore, different-sized Ag2S QDs that were near-infrared-emitting or visible-emitting were continuously stably synthesized in droplet microreactors at different temperatures. We believe we offer a new method for obtaining different-sized Ag2S nanoparticles.

Design of a Metal Oxide-Organic Framework (MoOF) Foam Microreactor: Solar-Induced Direct Pollutant Degradation and Hydrogen Generation.

PubMed

Zhu, Liangliang; Fu Tan, Chuan; Gao, Minmin; Ho, Ghim Wei

2015-12-16

A macroporous carbon network combined with mesoporous catalyst immobilization by a template method gives a metal-oxide-organic framework (MoOF) foam microreactor that readily soaks up pollutants and localizes solar energy in itself, leading to effective degradation of water pollutants (e.g., methyl orange (MO) and also hydrogen generation. The cleaned-up water can be removed from the microreactor simply by compression, and the microreactor used repeatedly. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Droplet-based microreactor for synthesis of water-soluble Ag2S quantum dots

NASA Astrophysics Data System (ADS)

Shu, Yun; Jiang, Peng; Pang, Dai-Wen; Zhang, Zhi-Ling

2015-07-01

A droplet-based microreactor was used for synthesis of water-soluble Ag2S quantum dots (QDs). Monodispersed Ag2S nanoparticles with a surface of carboxylic acid-terminated were synthesized in the droplet microreactor. The x-ray powder diffraction results indicated products were monoclinic Ag2S nanocrystals. Furthermore, different-sized Ag2S QDs that were near-infrared-emitting or visible-emitting were continuously stably synthesized in droplet microreactors at different temperatures. We believe we offer a new method for obtaining different-sized Ag2S nanoparticles.

Generation and reactions of oxiranyllithiums by use of a flow microreactor system.

PubMed

Nagaki, Aiichiro; Takizawa, Eiji; Yoshida, Jun-ichi

2010-12-17

A flow microreactor system consisting of micromixers and microtubes provides an effective reactor for the generation and reactions of aryloxiranyllithiums without decomposition by virtue of short residence time and efficient temperature control. The deprotonation of styrene oxides with sBuLi can be conducted by using the flow microreactor system at -78 or -68 °C (whereas much lower temperatures (< -100 °C) are needed for the same reactions conducted under macrobatch conditions). The resulting α-aryloxiranyllithiums were allowed to react with electrophiles in the flow microreactor system at the same temperature. The sequential introduction of various electrophiles onto 2,3-diphenyloxiranes was also achieved by using an integrated flow microreactor, which serves as a powerful system for the stereoselective synthesis of tetrasubstituted epoxides.

Vinyl functionalized silica hybrid monolith-based trypsin microreactor for on line digestion and separation via thiol-ene "click" strategy.

PubMed

Chen, Yingzhuang; Wu, Minghuo; Wang, Keyi; Chen, Bo; Yao, Shouzhuo; Zou, Hanfa; Nie, Lihua

2011-11-04

A novel thiol-ene "click" strategy for the preparation of monolithic trypsin microreactor was proposed. The hybrid organic-inorganic monolithic capillary column with ene-functionality was fabricated by sol-gel process using tetramethoxysilane (TMOS) and γ-methacryloxypropyltrimethoxysilane (γ-MAPS) as precursors. The disulfide bonds of trypsin were reduced to form free thiol groups. Then the trypsin containing free thiol groups was attached on the γ-MAPS hybrid monolithic column with ene-functionality via thiol-ene click chemistry to form a trypsin microreactor. The activity of the trypsin microreactor was characterized by detecting the substrate (Nα-p-tosyl-L-arginine methyl ester hydrochloride, TAME) and the product (Nα-p-tosyl-L-arginine, TA) with on-line capillary zone electrophoresis. After investigating various synthesizing conditions, it was found that the microreactor with poly(N,N'-methylenebisacrylamide) as spacer can deliver the highest activity, yielding a rapid reaction rate. After repeatedly sampling and analyzing for 100 times, the monolithic trypsin microreactor still remained 87.5% of its initial activity. It was demonstrated that thiol-ene "click" strategy for the construction of enzyme microreactor is a promising method for the highly selective immobilization of proteins under mild conditions, especially enzymes with free thiol radicals. Copyright © 2011 Elsevier B.V. All rights reserved.

Application of magnetohydrodynamic actuation to continuous flow chemistry.

PubMed

West, Jonathan; Karamata, Boris; Lillis, Brian; Gleeson, James P; Alderman, John; Collins, John K; Lane, William; Mathewson, Alan; Berney, Helen

2002-11-01

Continuous flow microreactors with an annular microchannel for cyclical chemical reactions were fabricated by either bulk micromachining in silicon or by rapid prototyping using EPON SU-8. Fluid propulsion in these unusual microchannels was achieved using AC magnetohydrodynamic (MHD) actuation. This integrated micropumping mechanism obviates the use of moving parts by acting locally on the electrolyte, exploiting its inherent conductive nature. Both silicon and SU-8 microreactors were capable of MHD actuation, attaining fluid velocities of the order of 300 microm s(-1) when using a 500 mM KCl electrolyte. The polymerase chain reaction (PCR), a thermocycling process, was chosen as an illustrative example of a cyclical chemistry. Accordingly, temperature zones were provided to enable a thermal cycle during each revolution. With this approach, fluid velocity determines cycle duration. Here, we report device fabrication and performance, a model to accurately describe fluid circulation by MHD actuation, and compatibility issues relating to this approach to chemistry.

IR spectroscopic studies in microchannel structures

NASA Astrophysics Data System (ADS)

Guber, A. E.; Bier, W.

1998-06-01

By means of the various microengineering methods available, microreaction systems can be produced among others. These microreactors consist of microchannels, where chemical reactions take place under defined conditions. For optimum process control, continuous online analytics is envisaged in the microchannels. For this purpose, a special analytical module has been developed. It may be applied for IR spectroscopic studies at any point of the microchannel.

Microfluidic radiolabeling of biomolecules with PET radiometals

PubMed Central

Zeng, Dexing; Desai, Amit V.; Ranganathan, David; Wheeler, Tobias D.; Kenis, Paul J. A.; Reichert, David E.

2012-01-01

Introduction A robust, versatile and compact microreactor has been designed, fabricated and tested for the labeling of bifunctional chelate conjugated biomolecules (BFC-BM) with PET radiometals. Methods The developed microreactor was used to radiolabel a chelate, either 1,4,7,10-Tetraazacyclododecane-1,4,7,10-tetraacetic acid (DOTA) or 1,4,7-triazacyclononane-1,4,7-triacetic acid (NOTA) that had been conjugated to cyclo(Arg-Gly-Asp-DPhe-Lys) peptide, with both 64Cu and 68Ga respectively. The microreactor radiolabeling conditions were optimized by varying temperature, concentration and residence time. Results Direct comparisons between the microreactor approach and conventional methods showed improved labeling yields and increased reproducibility with the microreactor under identical labeling conditions, due to enhanced mass and heat transfer at the microscale. More importantly, over 90% radiolabeling yields (incorporation of radiometal) were achieved with a 1:1 stoichiometry of bifunctional chelate biomolecule conjugate (BFC-BM) to radiometal in the microreactor, which potentially obviates extensive chromatographic purification that is typically required to remove the large excess of unlabeled biomolecule in radioligands prepared using conventional methods. Moreover, higher yields for radiolabeling of DOTA-functionalized BSA protein (Bovine Serum Albumin) were observed with 64Cu/68Ga using the microreactor, which demonstrates the ability to label both small and large molecules. Conclusions A robust, reliable, compact microreactor capable of chelating radiometals with common chelates has been developed and validated. Based on our radiolabeling results, the reported microfluidic approach overall outperforms conventional radiosynthetic methods, and is a promising technology for the radiometal labeling of commonly utilized BFC-BM in aqueous solutions. PMID:23078875

Microfluidic radiolabeling of biomolecules with PET radiometals.

PubMed

Zeng, Dexing; Desai, Amit V; Ranganathan, David; Wheeler, Tobias D; Kenis, Paul J A; Reichert, David E

2013-01-01

A robust, versatile and compact microreactor has been designed, fabricated and tested for the labeling of bifunctional chelate conjugated biomolecules (BFC-BM) with PET radiometals. The developed microreactor was used to radiolabel a chelate, either 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid (DOTA) or 1,4,7-triazacyclononane-1,4,7-triacetic acid (NOTA) that had been conjugated to cyclo(Arg-Gly-Asp-DPhe-Lys) peptide, with both ⁶⁴Cu and ⁶⁸Ga respectively. The microreactor radiolabeling conditions were optimized by varying temperature, concentration and residence time. Direct comparisons between the microreactor approach and conventional methods showed improved labeling yields and increased reproducibility with the microreactor under identical labeling conditions, due to enhanced mass and heat transfer at the microscale. More importantly, over 90% radiolabeling yields (incorporation of radiometal) were achieved with a 1:1 stoichiometry of bifunctional chelate biomolecule conjugate (BFC-BM) to radiometal in the microreactor, which potentially obviates extensive chromatographic purification that is typically required to remove the large excess of unlabeled biomolecule in radioligands prepared using conventional methods. Moreover, higher yields for radiolabeling of DOTA-functionalized BSA protein (Bovine Serum Albumin) were observed with ⁶⁴Cu/⁶⁸Ga using the microreactor, which demonstrates the ability to label both small and large molecules. A robust, reliable, compact microreactor capable of chelating radiometals with common chelates has been developed and validated. Based on our radiolabeling results, the reported microfluidic approach overall outperforms conventional radiosynthetic methods, and is a promising technology for the radiometal labeling of commonly utilized BFC-BM in aqueous solutions. Copyright © 2013 Elsevier Inc. All rights reserved.

A convenient enantioselective CBS-reduction of arylketones in flow-microreactor systems.

PubMed

De Angelis, Sonia; De Renzo, Maddalena; Carlucci, Claudia; Degennaro, Leonardo; Luisi, Renzo

2016-05-04

A convenient, versatile, and green CBS-asymmetric reduction of aryl and heteroaryl ketones has been developed by using the microreactor technology. The study demonstrates that it is possible to handle borane solution safely within microreactors and that the reaction performs well using 2-MeTHF as a greener solvent.

Membrane microreactors: gas-liquid reactions made easy.

PubMed

Noël, Timothy; Hessel, Volker

2013-03-01

Getting phases together: Membrane microreactors provide new opportunities for gas-liquid reactions. The advantages of this microreactor concept are a large interfacial area, a greater flexibility with regard to flow rates, and the opportunity to immobilize a catalyst on the membrane. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Flash crystallization kinetics of methane (sI) hydrate in a thermoelectrically-cooled microreactor.

PubMed

Chen, Weiqi; Pinho, Bruno; Hartman, Ryan L

2017-09-12

The crystallization kinetics of methane (sI) hydrate were investigated in a thermoelectrically-cooled microreactor with in situ Raman spectroscopy. Step-wise and precise control of the temperature allowed acquisition of reproducible data within minutes, while the nucleation of methane hydrates can take up to 24 h in traditional batch reactors. The propagation rates of methane hydrate (from 3.1-196.3 μm s -1 ) at the gas-liquid interface were measured for different Reynolds' numbers (0.7-68.9), pressures (30.0-80.9 bar), and sub-cooling temperatures (1.0-4.0 K). The precise measurement of the propagation rates and their subsequent analyses revealed a transition from mixed heat-transfer-crystallization-rate-limited to mixed heat-transfer-mass-transfer-crystallization-rate-limited kinetics. A theoretical model, based on heat transfer, mass transfer, and intrinsic crystallization kinetics, was derived for the first time to understand the non-linear relationship between the propagation rate and sub-cooling temperature. The molecular diffusivity of methane within a stagnant film (ahead of the propagation front) was discovered to follow Stokes-Einstein, while calculated Hatta (0.50-0.68), Lewis (128-207), and beta (0.79-116) numbers also confirmed that the diffusive flux influences crystal growth. Understanding methane hydrate crystal growth is important to the atmospheric, oceanic, and planetary sciences and to energy production, storage, and transportation. Our discoveries could someday advance the science of other multiphase, high-pressure, and sub-cooled crystallizations.

Flow-through polymerase chain reaction inside a seamless 3D helical microreactor fabricated utilizing a silicone tube and a paraffin mold.

PubMed

Wu, Wenming; Trinh, Kieu The Loan; Lee, Nae Yoon

2015-03-07

We introduce a new strategy for fabricating a seamless three-dimensional (3D) helical microreactor utilizing a silicone tube and a paraffin mold. With this method, various shapes and sizes of 3D helical microreactors were fabricated, and a complicated and laborious photolithographic process, or 3D printing, was eliminated. With dramatically enhanced portability at a significantly reduced fabrication cost, such a device can be considered to be the simplest microreactor, developed to date, for performing the flow-through polymerase chain reaction (PCR).

Immobilization of Phenylalanine Ammonia‐Lyase on Single‐Walled Carbon Nanotubes for Stereoselective Biotransformations in Batch and Continuous‐Flow Modes

PubMed Central

Bartha‐Vári, Judith H.; Toşa, Monica I.; Irimie, Florin‐Dan; Weiser, Diána; Boros, Zoltán; Vértessy, Beáta G.

2015-01-01

Abstract Carboxylated single‐walled carbon nanotubes (SwCNTCOOH) were used as a support for the covalent immobilization of phenylalanine ammonia‐lyase (PAL) from parsley by two different methods. The nanostructured biocatalysts (SwCNTCOOH‐PALI and SwCNTCOOH‐PALII) with low diffusional limitation were tested in the batch‐mode kinetic resolution of racemic 2‐amino‐3‐(thiophen‐2‐yl)propanoic acid (1) to yield a mixture of (R)‐1 and (E)‐3‐(thiophen‐2‐yl)acrylic acid (2) and in ammonia addition to 2 to yield enantiopure (S)‐1. SwCNTCOOH‐PALII was a stable biocatalyst (>90 % of the original activity remained after six cycles with 1 and after three cycles in 6 m NH3 with 2). The study of ammonia addition to 2 in a continuous‐flow microreactor filled with SwCNTCOOH‐PALII (2 m NH3, pH 10.0, 15 bar) between 30–80 °C indicated no significant loss of activity over 72 h up to 60 °C. SwCNTCOOH‐PALII in the continuous‐flow system at 30 °C was more productive (specific reaction rate, r flow=2.39 μmol min−1 g−1) than in the batch reaction (r batch=1.34 μmol min−1 g−1). PMID:26925171

The development of flow-through bio-catalyst microreactors from silica micro structured fibers for lipid transformations.

PubMed

Anuar, Sabiqah Tuan; Villegas, Carla; Mugo, Samuel M; Curtis, Jonathan M

2011-06-01

This study demonstrates the utility of a flow-through enzyme immobilized silica microreactor for lipid transformations. A silica micro structured fiber (MSF) consisting of 168 channels of internal diameter 4-5 μm provided a large surface area for the covalent immobilization of Candida antartica lipase. The specific activity of the immobilized lipase was determined by hydrolysis of p-nitrophenyl butyrate and calculated to be 0.81 U/mg. The catalytic performance of the lipase microreactor was demonstrated by the efficient ethanolysis of canola oil. The parameters affecting the performance of the MSF microreactor, including temperature and reaction flow rate, were investigated. Characterization of the lipid products exiting the microreactor was performed by non-aqueous reversed-phased liquid chromatography (NARP-LC) with evaporative light scattering detector (ELSD) and by comprehensive two-dimensional gas chromatography (GC x GC). Under optimized conditions of 1 μL/min flow rate of 5 mg/mL trioleoylglycerol (TO) in ethanol and 50 °C reaction temperature, 2-monooleoylglycerol was the main product at > 90% reaction yield. The regioselectivity of the Candida antartica lipase immobilized MSF microreactor in the presence of ethanol was found to be comparable to that obtained under conventional conditions. The ability of these reusable flow-through microreactors to regioselectively form monoacylglycerides in high yield from triacylglycerides demonstrate their potential use in small-scale lipid transformations or analytical lipids profiling.

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions.

PubMed

Laborde-Boutet, Cedric; McCaffrey, William C

2017-02-21

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method to visualize the behavior of petroleum samples under process conditions. The experimental setup relies on a custom-built micro-reactor fitted with a sapphire window at the bottom, which is placed over the objective of an inverted microscope equipped with a cross-polarizer module. Using reflection microscopy enables the visualization of opaque samples, such as petroleum vacuum residues, or asphaltenes. The combination of the sapphire window from the micro-reactor with the cross-polarizer module of the microscope on the light path allows high-contrast imaging of isotropic and anisotropic media. While observations are carried out, the micro-reactor can be heated to the temperature range of cracking reactions (up to 450 °C), can be subjected to H2 pressure relevant to hydroconversion reactions (up to 16 MPa), and can stir the sample by magnetic coupling. Observations are typically carried out by taking snapshots of the sample under cross-polarized light at regular time intervals. Image analyses may not only provide information on the temperature, pressure, and reactive conditions yielding phase separation, but may also give an estimate of the evolution of the chemical (absorption/reflection spectra) and physical (refractive index) properties of the sample before the onset of phase separation.

Quantitative determination of enzyme activity in single cells by scanning microelectrode coupled with a nitrocellulose film-covered microreactor by means of a scanning electrochemical microscope.

PubMed

Zhang, Xiaoli; Sun, Fuchan; Peng, Xuewei; Jin, Wenrui

2007-02-01

An electrochemical method for quantitative determination of enzyme activity in single cells was developed by scanning a microelectrode (ME) over a nitrocellulose film-covered microreactor with micropores by means of a scanning electrochemical microscope (SECM). Peroxidase (PO) in neutrophils was chosen as the model system. The microreactor consisted of a microwell with a solution and a nitrocellulose film with micropores. A single cell perforated by digitonin was injected into the microwell. After the perforated cell was lysed and allowed to dry, physiological buffer saline (PBS) containing hydroquinone (H2Q) and H2O2 as substrates of the enzyme-catalyzed reaction was added in the microwell. The microwell containing the extract of the lysed cell and the enzyme substrates was covered with Parafilm to prevent evaporation. The solution in the microwell was incubated for 20 min. In this case, the released PO from the cell converted H2Q into benzoquinone (BQ). Then, the Parafilm was replaced by a nitrocellulose film with micropores to fabricate the microreactor. The microreactor was placed in an electrochemical cell containing PBS, H2Q, and H2O2. After a 10-microm-radius Au ME was inserted into the electrochemical cell and approached down to the microreactor, the ME was scanned along the central line across the microreactor by means of a SECM. The scan curve with a peak was obtained by detecting BQ that diffused out from the microreactor through the micropores on the nitrocellulose film. PO activity could be quantified on the basis of the peak current on the scan curve using a calibration curve. This method had two obvious advantages: no electrode fouling and no oxygen interference.

Bio-inspired immobilization of metal oxides on monolithic microreactor for continuous Knoevenagel reaction.

PubMed

Song, Wentong; Shi, Da; Tao, Shengyang; Li, Zhaoliang; Wang, Yuchao; Yu, Yongxian; Qiu, Jieshan; Ji, Min; Wang, Xinkui

2016-11-01

A facile method is reported to construct monolithic microreactor with high catalytic performance for Knoevenagel reaction. The microreactor is based on hierarchically porous silica (HPS) which has interconnected macro- and mesopores. Then the HPS is surface modified by pyrogallol (PG) polymer. Al(NO3)3 and Mg(NO3)2 are loaded on the surface of HPS through coordination with -OH groups of PG. After thermal treatment, Al(NO3)3 and Mg(NO3)2 are converted Al2O3 and MgO. The as-synthesized catalytic microreactor shows a high and stable performance in Knoevenagel reaction. The microreactor possess large surface area and interconnected pore structures which are beneficial for reactions. Moreover, this economic, facile and eco-friendly surface modification method can be used in loading more metal oxides for more reactions. Copyright © 2016 Elsevier Inc. All rights reserved.

Product selectivity control induced by using liquid-liquid parallel laminar flow in a microreactor.

PubMed

Amemiya, Fumihiro; Matsumoto, Hideyuki; Fuse, Keishi; Kashiwagi, Tsuneo; Kuroda, Chiaki; Fuchigami, Toshio; Atobe, Mahito

2011-06-07

Product selectivity control based on a liquid-liquid parallel laminar flow has been successfully demonstrated by using a microreactor. Our electrochemical microreactor system enables regioselective cross-coupling reaction of aldehyde with allylic chloride via chemoselective cathodic reduction of substrate by the combined use of suitable flow mode and corresponding cathode material. The formation of liquid-liquid parallel laminar flow in the microreactor was supported by the estimation of benzaldehyde diffusion coefficient and computational fluid dynamics simulation. The diffusion coefficient for benzaldehyde in Bu(4)NClO(4)-HMPA medium was determined to be 1.32 × 10(-7) cm(2) s(-1) by electrochemical measurements, and the flow simulation using this value revealed the formation of clear concentration gradient of benzaldehyde in the microreactor channel over a specific channel length. In addition, the necessity of the liquid-liquid parallel laminar flow was confirmed by flow mode experiments.

Polyamidoamine dendrimer as a spacer for the immobilization of glucose oxidase in capillary enzyme microreactor.

PubMed

Wang, Siming; Su, Ping; Hongjun, E; Yang, Yi

2010-10-15

Polyamidoamine dendrimer (PAMAM) is one of a number of dendritic polymers with precise molecular structure, highly geometric symmetry, and a large number of terminal groups. In this study, different generations of PAMAM (G0-G4) were introduced onto the inner wall of fused-silica capillaries by microwave irradiation and a new type of glucose oxidase (GOx) capillary enzyme microreactor was developed based on enzyme immobilization in the prepared PAMAM-grafted fused-silica capillaries. The optimal enzymolysis conditions for beta-d-glucose in the microreactor were evaluated by capillary zone electrophoresis. In addition, the enzymolysis efficiencies of different generations of PAMAM-GOx capillary enzyme microreactor were compared. The results indicate that enzymolysis efficiency increased with increasing generations of PAMAM. The experimental results provide the possibility for the development and application of an online immobilized capillary enzyme microreactor. Crown Copyright 2010. Published by Elsevier Inc. All rights reserved.

A high-power ultrasonic microreactor and its application in gas-liquid mass transfer intensification.

PubMed

Dong, Zhengya; Yao, Chaoqun; Zhang, Xiaoli; Xu, Jie; Chen, Guangwen; Zhao, Yuchao; Yuan, Quan

2015-02-21

The combination of ultrasound and microreactor is an emerging and promising area, but the report of designing high-power ultrasonic microreactor (USMR) is still limited. This work presents a robust, high-power and highly efficient USMR by directly coupling a microreactor plate with a Langevin-type transducer. The USMR is designed as a longitudinal half wavelength resonator, for which the antinode plane of the highest sound intensity is located at the microreactor. According to one dimension design theory, numerical simulation and impedance analysis, a USMR with a maximum power of 100 W and a resonance frequency of 20 kHz was built. The strong and uniform sound field in the USMR was then applied to intensify gas-liquid mass transfer of slug flow in a microfluidic channel. Non-inertial cavitation with multiple surface wave oscillation was excited on the slug bubbles, enhancing the overall mass transfer coefficient by 3.3-5.7 times.

Synthesis of branched polymers under continuous-flow microprocess: an improvement of the control of macromolecular architectures.

PubMed

Bally, Florence; Serra, Christophe A; Brochon, Cyril; Hadziioannou, Georges

2011-11-15

Polymerization reactions can benefit from continuous-flow microprocess in terms of kinetics control, reactants mixing or simply efficiency when high-throughput screening experiments are carried out. In this work, we perform for the first time the synthesis of branched macromolecular architecture through a controlled/'living' polymerization technique, in tubular microreactor. Just by tuning process parameters, such as flow rates of the reactants, we manage to generate a library of polymers with various macromolecular characteristics. Compared to conventional batch process, polymerization kinetics shows a faster initiation step and more interestingly an improved branching efficiency. Due to reduced diffusion pathway, a characteristic of microsystems, it is thus possible to reach branched polymers exhibiting a denser architecture, and potentially a higher functionality for later applications. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Plasma microreactor in supercritical xenon and its application to diamondoid synthesis

NASA Astrophysics Data System (ADS)

Oshima, F.; Stauss, S.; Ishii, C.; Pai, D. Z.; Terashima, K.

2012-10-01

The generation of plasmas in a microreactor is demonstrated in xenon from atmospheric pressure up to supercritical conditions. Ac high voltage at a frequency of 15 kHz was applied across a 25-µm discharge gap between a tungsten wire and a fused silica micro-capillary tube in a coaxial configuration. Using this continuous flow supercritical fluid microreactor, it was possible to synthesize diamantane and other diamondoids up to nonamantane, using adamantane as a precursor and seed. It is anticipated that plasmas generated in supercritical fluid microreactors may not only allow faster fabrication of diamondoids, but also offer opportunities for the fabrication of other nanomaterials.

DNA-directed trypsin immobilization on a polyamidoamine dendrimer-modified capillary to form a renewable immobilized enzyme microreactor.

PubMed

Wu, Nan; Wang, Siming; Yang, Ye; Song, Jiayi; Su, Ping; Yang, Yi

2018-07-01

A novel type of trypsin capillary microreactor was developed based on a DNA-directed immobilization (DDI) technique applied to a fused-silica capillary modified with polyamidoamine (PAMAM) dendrimers. Trypsin binding to the inner wall of the capillary was confirmed by confocal laser scanning microscopy. The properties of the trypsin-DNA conjugated, PAMAM-modified capillary microreactor were investigated by monitoring hydrolysis of Nα-benzoyl- L -arginine ethyl ester. Through the hybridization and dehybridization of the DNA, the inner wall of the capillary functionalized with trypsin can be regenerated, thus indicating the renewability of this enzyme microreactor. In addition, these results demonstrated that introduction of PAMAM enabled higher amounts of trypsin to be immobilized, markedly improving the enzymolysis efficiency, compared with traditional modified capillaries. The digestion performance of the trypsin capillary microreactor was further evaluated by digesting cytochrome C, and a peptide numbers of 8, and a sequence coverage of 59% were obtained. This renewable and efficient immobilized trypsin capillary microreactor combines advantages of both DDI technology and PAMAM, and is potentially adaptable to high-throughput enzyme assays in biochemical and clinical research. Copyright © 2018. Published by Elsevier B.V.

Influence of surface heterogeneity in electroosmotic flows—Implications in chromatography, fluid mixing, and chemical reactions in microdevices

NASA Astrophysics Data System (ADS)

Adrover, Alessandra; Giona, Massimiliano; Pagnanelli, Francesca; Toro, Luigi

2007-04-01

We analyze the influence of surface heterogeneity, inducing a random ζ-potential at the walls in electroosmotic incompressible flows. Specifically, we focus on how surface heterogeneity modifies the physico-chemical processes (transport, chemical reaction, mixing) occurring in microchannel and microreactors. While the macroscopic short-time features associated with solute transport (e.g. chromatographic patterns) do not depend significantly on ζ-potential heterogeneity, spatial randomness in the surface ζ-potential modifies the spectral properties of the advection-diffusion operator, determining different long-term properties of transport/reaction phenomena compared to the homogeneous case. Examples of physical relevance (chromatography, infinitely fast reactions) are addressed.

Rapid Multistep Synthesis of 1,2,4-Oxadiazoles in a Single Continuous Microreactor Sequence

PubMed Central

Grant, Daniel; Dahl, Russell; Cosford, Nicholas D. P.

2009-01-01

A general method for the synthesis of bis-substituted 1,2,4-oxadiazoles from readily available arylnitriles and activated carbonyls in a single continuous microreactor sequence is described. The synthesis incorporates three sequential microreactors to produce 1,2,4-oxadiazoles in ~30 min in quantities (40–80 mg) sufficient for full characterization and rapid library supply. PMID:18687005

Fischer-Tropsch synthesis from a low H/sub 2/:CO gas in a dry fluidized-bed system. Volume 2. Development of microreactor systems for unsteady-state Fischer-Tropsch synthesis. Final technical report. [408 references

DOE Office of Scientific and Technical Information (OSTI.GOV)

Whiting, G.K.; Liu, Y.A.; Squires, A.M.

1986-10-01

Vibrofluidized microreactor systems have been developed for studies of unsteady-state Fischer-Tropsch synthesis. This development is aimed at preventing carbon deposition on a fused-iron catalyst in a novel reactor called the ''heat tray.'' This reactor involves a supernatant gas flowing over a shallow fluidized bed of catalyst particles. Three systems were built: (1) a vibrofluidized-bed microreactor system for obtaining baseline carbon deposition information under industrially important reaction conditions; (2) a sliding-plug vibrofluidized-bed microreactor system for rapid switching of feed gases in the F-T synthesis; and (3) a cold-flow microreactor model for studying the gas mixing characteristics of the sliding-plug vibrofluidized-bed microreactor.more » The results show that catalyst defluidization occurred under steady-state synthesis conditions below 395 C using a feed gas of H/sub 2//CO ratio of 2:1 or less. Above 395 C, the probability of hydrocarbon chain growth (..cap alpha.. < 0.50 to prevent accumulation of high-molecular-weight species that cause defluidization. Carbon deposition was rapid above 395 C when a feed gas of H/sub 2//CO ratio of 2:1 or less was used. Cold-flow microreactor model studies show that rapid (on the order of seconds), quantitative switching of feed gases over a vibrofluidized bed of catalyst could be achieved. Vibrofluidization of the catalyst bed induced little backmixing of feed gas over the investigated flow-rate range of 417 to 1650 actual mm/sup 3//s. Further, cold-flow microreactor model studies showed intense solid mixing when a bed of fused-iron catalyst (150 to 300 microns) was vibrofluidized at 24 cycles per second with a peak-to-peak amplitude of 4 mm. The development of the microreactor systems provided an easy way of accurately determining integral fluid-bed kinetics in a laboratory reactor. 408 refs., 156 figs., 27 tabs.« less

Reaction Rates Of Olivine Carbonation - An Experimental Study Using Synthetic Fluid Inclusions As Micro-Reactors

NASA Astrophysics Data System (ADS)

Sendula, E.; Lamadrid, H. M.; Bodnar, R. J.

2017-12-01

Ultramafic and mafic rocks (e.g. peridotites, serpentinites and basalts) are being considered as possible targets for CO2 sequestration via mineral carbonation. The determination of reaction kinetics and the factors that control mineralization are important in order to understand and predict fluid-rock reactions between the injected CO2 and the host rocks. Here we present results of experiments focused on determining the reaction rates of carbonation of olivine as a function of initial CO2 concentration (20 mol% and 11 mol%) in the aqueous solution and temperature (100°C and 50°C). We used a recently developed experimental method (Lamadrid et al., 2017) that uses synthetic fluid inclusions as micro-reactors. The micro-reactor technique coupled with non-destructive Raman spectroscopy allows us to monitor the reaction progress in situ and in real time, by quantifying the amount of CO2 consumed in the reaction as a function of time. Results show a measurable decrease of CO2 density in the fluid inclusions as a result of the reaction between the CO2-bearing aqueous phase and olivine. Magnesite formation begins within several hours at 100°C and most of the CO2 was consumed within two days. At 50°C, however, magnesite nucleation and precipitation required weeks to months to begin, and the reaction rates were about an order of magnitude slower than in the experiments at 100°C. No significant differences were observed in the reaction rates as a function of initial CO2 concentration. The application of the synthetic fluid inclusion technique as micro-reactors coupled with non-destructive analytical techniques is a promising tool to monitor rates of fluid-rock reactions in situ and in real time, allowing detailed micron-scale investigations. The technique can be applied to a wide variety of chemical systems, host minerals, reaction products, fluid densities, temperatures, and different starting fluid compositions.

Coaxial microreactor for particle synthesis

DOEpatents

Bartsch, Michael; Kanouff, Michael P; Ferko, Scott M; Crocker, Robert W; Wally, Karl

2013-10-22

A coaxial fluid flow microreactor system disposed on a microfluidic chip utilizing laminar flow for synthesizing particles from solution. Flow geometries produced by the mixing system make use of hydrodynamic focusing to confine a core flow to a small axially-symmetric, centrally positioned and spatially well-defined portion of a flow channel cross-section to provide highly uniform diffusional mixing between a reactant core and sheath flow streams. The microreactor is fabricated in such a way that a substantially planar two-dimensional arrangement of microfluidic channels will produce a three-dimensional core/sheath flow geometry. The microreactor system can comprise one or more coaxial mixing stages that can be arranged singly, in series, in parallel or nested concentrically in parallel.

Synthesis of Monodisperse Chitosan Nanoparticles and in Situ Drug Loading Using Active Microreactor.

PubMed

Kamat, Vivek; Marathe, Ila; Ghormade, Vandana; Bodas, Dhananjay; Paknikar, Kishore

2015-10-21

Chitosan nanoparticles are promising drug delivery vehicles. However, the conventional method of unregulated mixing during ionic gelation limits their application because of heterogeneity in size and physicochemical properties. Therefore, a detailed theoretical analysis of conventional and active microreactor models was simulated. This led to design and fabrication of a polydimethylsiloxane microreactor with magnetic micro needles for the synthesis of monodisperse chitosan nanoparticles. Chitosan nanoparticles synthesized conventionally, using 0.5 mg/mL chitosan, were 250 ± 27 nm with +29.8 ± 8 mV charge. Using similar parameters, the microreactor yielded small size particles (154 ± 20 nm) at optimized flow rate of 400 μL/min. Further optimization at 0.4 mg/mL chitosan concentration yielded particles (130 ± 9 nm) with higher charge (+39.8 ± 5 mV). The well-controlled microreactor-based mixing generated highly monodisperse particles with tunable properties including antifungal drug entrapment (80%), release rate, and effective activity (MIC, 1 μg/mL) against Candida.

Modeling of methanol decomposition on Pt/CeO2/ZrO2 catalyst in a packed bed microreactor

NASA Astrophysics Data System (ADS)

Pohar, Andrej; Belavič, Darko; Dolanc, Gregor; Hočevar, Stanko

2014-06-01

Methanol decomposition on Pt/CeO2/ZrO2 catalyst is studied inside a packed bed microreactor in the temperature range of 300-380 °C. The microreactor is fabricated using low-temperature co-fired ceramic (LTCC) technology, which is well suited for the production of relatively complex three-dimensional structures. It is packed with 2 wt% Pt-CeO2 catalyst, which is deposited onto ZrO2 spherical particles. A 1D mathematical model, which incorporates diffusion, convection and mass transfer through the boundary layer to the catalyst particles, as well as a 3D computational fluid dynamics model, are developed to describe the methanol decomposition process inside the packed bed. The microreactor exhibits reliable operation and no catalyst deactivation was observed during three months of experimentation. A comparison between the 1D mathematical model and the 3D model, considering the full 3D geometry of the microreactor is made and the differences between the models are identified and evaluated.

Microreactor-based mixing strategy suppresses product inhibition to enhance sugar yields in enzymatic hydrolysis for cellulosic biofuel production.

PubMed

Chakraborty, Saikat; Singh, Prasun Kumar; Paramashetti, Pawan

2017-08-01

A novel microreactor-based energy-efficient process of using complete convective mixing in a macroreactor till an optimal mixing time followed by no mixing in 200-400μl microreactors enhances glucose and reducing sugar yields by upto 35% and 29%, respectively, while saving 72-90% of the energy incurred on reactor mixing in the enzymatic hydrolysis of cellulose. Empirical exponential relations are provided for determining the optimal mixing time, during which convective mixing in the macroreactor promotes mass transport of the cellulase enzyme to the solid Avicel substrate, while the latter phase of no mixing in the microreactor suppresses product inhibition by preventing the inhibitors (glucose and cellobiose) from homogenizing across the reactor. Sugar yield increases linearly with liquid to solid height ratio (r h ), irrespective of substrate loading and microreactor size, since large r h allows the inhibitors to diffuse in the liquid away from the solids, thus reducing product inhibition. Copyright © 2017 Elsevier Ltd. All rights reserved.

Biofluidic Intelligent Processors for Preparative Manipulations of Biological Warfare Agents at the Attomole Level

DTIC Science & Technology

2005-11-01

micromixing and microreactor concept. OPA by itself is non- fluorescent, but it reacts with primary amine groups in the presence of β-mercaptoethanol to form...hybrid microchannel/nanopore-membrane devices can serve as efficient micromixers and microreactors, and (2) microscopic kinetics can be obtained from...single image measurements. An immediate application which extended from the micromixing and microreactor concept was microsensing. Calcium ions

High quantum yield ZnO quantum dots synthesizing via an ultrasonication microreactor method.

PubMed

Yang, Weimin; Yang, Huafang; Ding, Wenhao; Zhang, Bing; Zhang, Le; Wang, Lixi; Yu, Mingxun; Zhang, Qitu

2016-11-01

Green emission ZnO quantum dots were synthesized by an ultrasonic microreactor. Ultrasonic radiation brought bubbles through ultrasonic cavitation. These bubbles built microreactor inside the microreactor. The photoluminescence properties of ZnO quantum dots synthesized with different flow rate, ultrasonic power and temperature were discussed. Flow rate, ultrasonic power and temperature would influence the type and quantity of defects in ZnO quantum dots. The sizes of ZnO quantum dots would be controlled by those conditions as well. Flow rate affected the reaction time. With the increasing of flow rate, the sizes of ZnO quantum dots decreased and the quantum yields first increased then decreased. Ultrasonic power changed the ultrasonic cavitation intensity, which affected the reaction energy and the separation of the solution. With the increasing of ultrasonic power, sizes of ZnO quantum dots first decreased then increased, while the quantum yields kept increasing. The effect of ultrasonic temperature on the photoluminescence properties of ZnO quantum dots was influenced by the flow rate. Different flow rate related to opposite changing trend. Moreover, the quantum yields of ZnO QDs synthesized by ultrasonic microreactor could reach 64.7%, which is higher than those synthesized only under ultrasonic radiation or only by microreactor. Copyright © 2016 Elsevier B.V. All rights reserved.

Proteolytic Digestion and TiO2 Phosphopeptide Enrichment Microreactor for Fast MS Identification of Proteins.

PubMed

Deng, Jingren; Lazar, Iulia M

2016-04-01

The characterization of phosphorylation state(s) of a protein is best accomplished by using isolated or enriched phosphoprotein samples or their corresponding phosphopeptides. The process is typically time-consuming as, often, a combination of analytical approaches must be used. To facilitate throughput in the study of phosphoproteins, a microreactor that enables a novel strategy for performing fast proteolytic digestion and selective phosphopeptide enrichment was developed. The microreactor was fabricated using 100 μm i.d. fused-silica capillaries packed with 1-2 mm beds of C18 and/or TiO2 particles. Proteolytic digestion-only, phosphopeptide enrichment-only, and sequential proteolytic digestion/phosphopeptide enrichment microreactors were developed and tested with standard protein mixtures. The protein samples were adsorbed on the C18 particles, quickly digested with a proteolytic enzyme infused over the adsorbed proteins, and further eluted onto the TiO2 microreactor for enrichment in phosphopeptides. A number of parameters were optimized to speed up the digestion and enrichments processes, including microreactor dimensions, sample concentrations, digestion time, flow rates, buffer compositions, and pH. The effective time for the steps of proteolytic digestion and enrichment was less than 5 min. For simple samples, such as standard protein mixtures, this approach provided equivalent or better results than conventional bench-top methods, in terms of both enzymatic digestion and selectivity. Analysis times and reagent costs were reduced ~10- to 15-fold. Preliminary analysis of cell extracts and recombinant proteins indicated the feasibility of integration of these microreactors in more advanced workflows amenable for handling real-world biological samples. Graphical Abstract ᅟ.

Proteolytic Digestion and TiO2 Phosphopeptide Enrichment Microreactor for Fast MS Identification of Proteins

NASA Astrophysics Data System (ADS)

Deng, Jingren; Lazar, Iulia M.

2016-04-01

The characterization of phosphorylation state(s) of a protein is best accomplished by using isolated or enriched phosphoprotein samples or their corresponding phosphopeptides. The process is typically time-consuming as, often, a combination of analytical approaches must be used. To facilitate throughput in the study of phosphoproteins, a microreactor that enables a novel strategy for performing fast proteolytic digestion and selective phosphopeptide enrichment was developed. The microreactor was fabricated using 100 μm i.d. fused-silica capillaries packed with 1-2 mm beds of C18 and/or TiO2 particles. Proteolytic digestion-only, phosphopeptide enrichment-only, and sequential proteolytic digestion/phosphopeptide enrichment microreactors were developed and tested with standard protein mixtures. The protein samples were adsorbed on the C18 particles, quickly digested with a proteolytic enzyme infused over the adsorbed proteins, and further eluted onto the TiO2 microreactor for enrichment in phosphopeptides. A number of parameters were optimized to speed up the digestion and enrichments processes, including microreactor dimensions, sample concentrations, digestion time, flow rates, buffer compositions, and pH. The effective time for the steps of proteolytic digestion and enrichment was less than 5 min. For simple samples, such as standard protein mixtures, this approach provided equivalent or better results than conventional bench-top methods, in terms of both enzymatic digestion and selectivity. Analysis times and reagent costs were reduced ~10- to 15-fold. Preliminary analysis of cell extracts and recombinant proteins indicated the feasibility of integration of these microreactors in more advanced workflows amenable for handling real-world biological samples.

Sample Handling and Chemical Kinetics in an Acoustically Levitated Drop Microreactor

PubMed Central

2009-01-01

Accurate measurement of enzyme kinetics is an essential part of understanding the mechanisms of biochemical reactions. The typical means of studying such systems use stirred cuvettes, stopped-flow apparatus, microfluidic systems, or other small sample containers. These methods may prove to be problematic if reactants or products adsorb to or react with the container’s surface. As an alternative approach, we have developed an acoustically-levitated drop reactor eventually intended to study enzyme-catalyzed reaction kinetics related to free radical and oxidative stress chemistry. Microliter-scale droplet generation, reactant introduction, maintenance, and fluid removal are all important aspects in conducting reactions in a levitated drop. A three capillary bundle system has been developed to address these needs. We report kinetic measurements for both luminol chemiluminescence and the reaction of pyruvate with nicotinamide adenine dinucleotide, catalyzed by lactate dehydrogenase, to demonstrate the feasibility of using a levitated drop in conjunction with the developed capillary sample handling system as a microreactor. PMID:19769373

Quantitative Insights into the Fast Pyrolysis of Extracted Cellulose, Hemicelluloses, and Lignin

PubMed Central

Windt, Michael; Ziegler, Bernhard; Appelt, Jörn; Saake, Bodo; Meier, Dietrich; Bridgwater, Anthony

2017-01-01

Abstract The transformation of lignocellulosic biomass into bio‐based commodity chemicals is technically possible. Among thermochemical processes, fast pyrolysis, a relatively mature technology that has now reached a commercial level, produces a high yield of an organic‐rich liquid stream. Despite recent efforts to elucidate the degradation paths of biomass during pyrolysis, the selectivity and recovery rates of bio‐compounds remain low. In an attempt to clarify the general degradation scheme of biomass fast pyrolysis and provide a quantitative insight, the use of fast pyrolysis microreactors is combined with spectroscopic techniques (i.e., mass spectrometry and NMR spectroscopy) and mixtures of unlabeled and 13C‐enriched materials. The first stage of the work aimed to select the type of reactor to use to ensure control of the pyrolysis regime. A comparison of the chemical fragmentation patterns of “primary” fast pyrolysis volatiles detected by using GC‐MS between two small‐scale microreactors showed the inevitable occurrence of secondary reactions. In the second stage, liquid fractions that are also made of primary fast pyrolysis condensates were analyzed by using quantitative liquid‐state 13C NMR spectroscopy to provide a quantitative distribution of functional groups. The compilation of these results into a map that displays the distribution of functional groups according to the individual and main constituents of biomass (i.e., hemicelluloses, cellulose and lignin) confirmed the origin of individual chemicals within the fast pyrolysis liquids. PMID:28644517

Quantitative Insights into the Fast Pyrolysis of Extracted Cellulose, Hemicelluloses, and Lignin.

PubMed

Carrier, Marion; Windt, Michael; Ziegler, Bernhard; Appelt, Jörn; Saake, Bodo; Meier, Dietrich; Bridgwater, Anthony

2017-08-24

The transformation of lignocellulosic biomass into bio-based commodity chemicals is technically possible. Among thermochemical processes, fast pyrolysis, a relatively mature technology that has now reached a commercial level, produces a high yield of an organic-rich liquid stream. Despite recent efforts to elucidate the degradation paths of biomass during pyrolysis, the selectivity and recovery rates of bio-compounds remain low. In an attempt to clarify the general degradation scheme of biomass fast pyrolysis and provide a quantitative insight, the use of fast pyrolysis microreactors is combined with spectroscopic techniques (i.e., mass spectrometry and NMR spectroscopy) and mixtures of unlabeled and 13 C-enriched materials. The first stage of the work aimed to select the type of reactor to use to ensure control of the pyrolysis regime. A comparison of the chemical fragmentation patterns of "primary" fast pyrolysis volatiles detected by using GC-MS between two small-scale microreactors showed the inevitable occurrence of secondary reactions. In the second stage, liquid fractions that are also made of primary fast pyrolysis condensates were analyzed by using quantitative liquid-state 13 C NMR spectroscopy to provide a quantitative distribution of functional groups. The compilation of these results into a map that displays the distribution of functional groups according to the individual and main constituents of biomass (i.e., hemicelluloses, cellulose and lignin) confirmed the origin of individual chemicals within the fast pyrolysis liquids. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

Energy Analysis of n-Dodecane Combustion in a Hetero/Homogeneous Heat-Recirculating Microreactor for Portable Power Applications

NASA Astrophysics Data System (ADS)

Waits, C. M.; Tolmachoff, E. D.; Allmon, W. R.; Zecher-Freeman, N. E.

2016-11-01

An energy analysis is presented for n-dodecane/air combustion in a heat recirculating Inconel microreactor under vacuum conditions. Microreactor channels are partially coated with platinum enabling operating with coupled heterogeneous and homogeneous reactions. The radiant efficiency, important for thermophotovoltaic energy conversion, was found to decrease from 57% to 52% over 5 different runs covering 377 min of operation. A similar decrease in combustion efficiency was observed with 6%-8% energy lost to incomplete combustion and 5%- 6% lost through sensible heat in the exhaust. The remaining thermal loss is from unusable radiation and conduction through inlet and outlet tubing. Changes in the Inconel microreactor geometry and emissivity properties were observed.

Tailor-made resealable micro(bio)reactors providing easy integration of in situ sensors

NASA Astrophysics Data System (ADS)

Viefhues, Martina; Sun, Shiwen; Valikhani, Donya; Nidetzky, Bernd; Vrouwe, Elwin X.; Mayr, Torsten; Bolivar, Juan M.

2017-06-01

Flow microreactors utilizing immobilized enzymes are of great interest in biocatalysis development. Most of the common devices are permanently closed, single-use systems, which allow limited physical and chemical surface modifications and evaluation methods. In this paper we will present resealable flowcells that overcome these limitations and moreover allow a quick and easy integration of sensor systems, because of the use of modular building blocks. The devices were utilized to study the enzyme activity of glucose oxidase immobilized on chemically modified glass surfaces under flow conditions, employing integrated optical oxygen sensors for on-line monitoring.

Electron-transfer-initiated benzoin- and Stetter-like reactions in packed-bed reactors for process intensification.

PubMed

Zaghi, Anna; Ragno, Daniele; Di Carmine, Graziano; De Risi, Carmela; Bortolini, Olga; Giovannini, Pier Paolo; Fantin, Giancarlo; Massi, Alessandro

2016-01-01

A convenient heterogeneous continuous-flow procedure for the polarity reversal of aromatic α-diketones is presented. Propaedeutic batch experiments have been initially performed to select the optimal supported base capable to initiate the two electron-transfer process from the carbamoyl anion of the N , N -dimethylformamide (DMF) solvent to the α-diketone and generate the corresponding enediolate active species. After having identified the 2- tert -butylimino-2-diethylamino-1,3-dimethylperhydro-1,3,2-diazaphosphorine on polystyrene (PS-BEMP) as the suitable base, packed-bed microreactors (pressure-resistant stainless-steel columns) have been fabricated and operated to accomplish the chemoselective synthesis of aroylated α-hydroxy ketones and 2-benzoyl-1,4-diones (benzoin- and Stetter-like products, respectively) with a good level of efficiency and with a long-term stability of the packing material (up to five days).

Electron-transfer-initiated benzoin- and Stetter-like reactions in packed-bed reactors for process intensification

PubMed Central

Zaghi, Anna; Ragno, Daniele; Di Carmine, Graziano; De Risi, Carmela; Bortolini, Olga; Giovannini, Pier Paolo; Fantin, Giancarlo

2016-01-01

A convenient heterogeneous continuous-flow procedure for the polarity reversal of aromatic α-diketones is presented. Propaedeutic batch experiments have been initially performed to select the optimal supported base capable to initiate the two electron-transfer process from the carbamoyl anion of the N,N-dimethylformamide (DMF) solvent to the α-diketone and generate the corresponding enediolate active species. After having identified the 2-tert-butylimino-2-diethylamino-1,3-dimethylperhydro-1,3,2-diazaphosphorine on polystyrene (PS-BEMP) as the suitable base, packed-bed microreactors (pressure-resistant stainless-steel columns) have been fabricated and operated to accomplish the chemoselective synthesis of aroylated α-hydroxy ketones and 2-benzoyl-1,4-diones (benzoin- and Stetter-like products, respectively) with a good level of efficiency and with a long-term stability of the packing material (up to five days). PMID:28144342

Determination of the Microscopic Structure of Surface and Overlayers, Adsorbate-Adsorbate Interaction Energies, and Rates of Surface Processes.

DTIC Science & Technology

1982-12-28

molecular beam-surface scattering, high pressure microreactor , heterogeneous catalysis. :116. AmTRAC? ’CAuI1ae 4111, 8ee 1 111 It oesey -1lP d ify by...Crystallography.. . ..... ....................... 4 11. Design and Construction of a High Pressure Catalvtic Microreactor ... microreactor has been designed and constructed. This micro- reactor will be a useful adjunct to the molecular beam machine since in the former overall

A low perfusion rate microreactor for continuous monitoring of enzyme characteristics: application to glucose oxidase

PubMed Central

Venema, K.; van Berkel, W. J. H.; Korf, J.

2007-01-01

This report describes a versatile and robust microreactor for bioactive proteins physically immobilized on a polyether sulfone filter. The potential of the reactor is illustrated with glucose oxidase immobilized on a filter with a cut-off value of 30 kDa. A flow-injection system was used to deliver the reactants and the device was linked on-line to an electrochemical detector. The microreactor was used for on-line preparation of apoglucose oxidase in strong acid and its subsequent reactivation with flavin adenine dinucleotide. In addition we describe a miniaturized version of the microreactor used to assess several characteristics of femtomole to attomole amounts of glucose oxidase. A low negative potential over the electrodes was used when ferrocene was the mediator in combination with horseradish peroxidase, ensuring the absence of oxidation of electro-active compounds in biological fluids. A low backpressure at very low flow rates is an advantage, which increases the sensitivity. A variety of further applications of the microreactor are suggested. Figure Preparation of apoGOx and restoration of enzyme activity using a soluton of FAD PMID:17909761

Immobilized Pepsin Microreactor for Rapid Peptide Mapping with Nanoelectrospray Ionization Mass Spectrometry

NASA Astrophysics Data System (ADS)

Long, Ying; Wood, Troy D.

2015-01-01

Most enzymatic microreactors for protein digestion are based on trypsin, but proteins with hydrophobic segments may be difficult to digest because of the paucity of Arg and Lys residues. Microreactors based on pepsin, which is less specific than trypsin, can overcome this challenge. Here, an integrated immobilized pepsin microreactor (IPMR)/nanoelectrospray emitter is examined for its potential for peptide mapping. For myoglobin, equivalent sequence coverage is obtained in a thousandth the time of solution digestion with better sequence coverage. While sequence coverage of cytochrome c is lesser than solution in this short duration, more highly-charged peptic peptides are produced and a number of peaks are unidentified at low-resolution, suggesting that high-resolution mass spectrometry is needed to take full advantage of integrated IPMR/nanoelectrospray devices.

Gallium-containing polymer brush film as efficient supported Lewis acid catalyst in a glass microreactor.

PubMed

Munirathinam, Rajesh; Ricciardi, Roberto; Egberink, Richard J M; Huskens, Jurriaan; Holtkamp, Michael; Wormeester, Herbert; Karst, Uwe; Verboom, Willem

2013-01-01

Polystyrene sulfonate polymer brushes, grown on the interior of the microchannels in a microreactor, have been used for the anchoring of gallium as a Lewis acid catalyst. Initially, gallium-containing polymer brushes were grown on a flat silicon oxide surface and were characterized by FTIR, ellipsometry, and X-ray photoelectron spectroscopy (XPS). XPS revealed the presence of one gallium per 2-3 styrene sulfonate groups of the polymer brushes. The catalytic activity of the Lewis acid-functionalized brushes in a microreactor was demonstrated for the dehydration of oximes, using cinnamaldehyde oxime as a model substrate, and for the formation of oxazoles by ring closure of ortho-hydroxy oximes. The catalytic activity of the microreactor could be maintained by periodic reactivation by treatment with GaCl3.

Chemical imaging of molecular changes in a hydrated single cell by dynamic secondary ion mass spectrometry and super-resolution microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hua, Xin; Szymanski, Craig; Wang, Zhaoying

2016-01-01

Chemical imaging of single cells is important in capturing biological dynamics. Single cell correlative imaging is realized between structured illumination microscopy (SIM) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) using System for Analysis at the Liquid Vacuum Interface (SALVI), a multimodal microreactor. SIM characterized cells and guided subsequent ToF-SIMS analysis. Dynamic ToF-SIMS provided time- and space-resolved cell molecular mapping. Lipid fragments were identified in the hydrated cell membrane. Principal component analysis was used to elucidate chemical component differences among mouse lung cells that uptake zinc oxide nanoparticles. Our results provided submicron chemical spatial mapping for investigations of cell dynamics atmore » the molecular level.« less

Gallium-containing polymer brush film as efficient supported Lewis acid catalyst in a glass microreactor

PubMed Central

Munirathinam, Rajesh; Ricciardi, Roberto; Egberink, Richard J M; Huskens, Jurriaan; Holtkamp, Michael; Wormeester, Herbert; Karst, Uwe

2013-01-01

Summary Polystyrene sulfonate polymer brushes, grown on the interior of the microchannels in a microreactor, have been used for the anchoring of gallium as a Lewis acid catalyst. Initially, gallium-containing polymer brushes were grown on a flat silicon oxide surface and were characterized by FTIR, ellipsometry, and X-ray photoelectron spectroscopy (XPS). XPS revealed the presence of one gallium per 2–3 styrene sulfonate groups of the polymer brushes. The catalytic activity of the Lewis acid-functionalized brushes in a microreactor was demonstrated for the dehydration of oximes, using cinnamaldehyde oxime as a model substrate, and for the formation of oxazoles by ring closure of ortho-hydroxy oximes. The catalytic activity of the microreactor could be maintained by periodic reactivation by treatment with GaCl3. PMID:24062830

Let the substrate flow, not the enzyme: Practical immobilization of d-amino acid oxidase in a glass microreactor for effective biocatalytic conversions.

PubMed

Bolivar, Juan M; Tribulato, Marco A; Petrasek, Zdenek; Nidetzky, Bernd

2016-11-01

Exploiting enzymes for chemical synthesis in flow microreactors necessitates their reuse for multiple rounds of conversion. To achieve this goal, immobilizing the enzymes on microchannel walls is a promising approach, but practical methods for it are lacking. Using fusion to a silica-binding module to engineer enzyme adsorption to glass surfaces, we show convenient immobilization of d-amino acid oxidase on borosilicate microchannel plates. In confocal laser scanning microscopy, channel walls appeared uniformly coated with target protein. The immobilized enzyme activity was in the range expected for monolayer coverage of the plain surface with oxidase (2.37 × 10(-5)  nmol/mm(2) ). Surface attachment of the enzyme was completely stable under flow. The operational half-life of the immobilized oxidase (25°C, pH 8.0; soluble catalase added) was 40 h. Enzymatic oxidation of d-Met into α-keto-γ-(methylthio)butyric acid was characterized in single-pass and recycle reactor configurations, employing in-line measurement of dissolved O2 , and off-line determination of the keto-acid product. Reaction-diffusion time-scale analysis for different flow conditions showed that the heterogeneously catalyzed reaction was always slower than diffusion of O2 to the solid surface (DaII  ≤ 0.3). Potential of the microreactor for intensifying O2 -dependent biotransformations restricted by mass transfer in conventional reactors is thus revealed. Biotechnol. Bioeng. 2016;113: 2342-2349. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

A biofilm microreactor system for simultaneous electrochemical and nuclear magnetic resonance techniques.

PubMed

Renslow, R S; Babauta, J T; Majors, P D; Mehta, H S; Ewing, R J; Ewing, T W; Mueller, K T; Beyenal, H

2014-01-01

Nuclear magnetic resonance (NMR) techniques are ideally suited for the study of biofilms and for probing their microenvironments because these techniques allow for noninvasive interrogation and in situ monitoring with high resolution. By combining NMR with simultaneous electrochemical techniques, it is possible to sustain and study live biofilms respiring on electrodes. Here, we describe a biofilm microreactor system, including a reusable and a disposable reactor, that allows for simultaneous electrochemical and NMR techniques (EC-NMR) at the microscale. Microreactors were designed with custom radio frequency resonator coils, which allowed for NMR measurements of biofilms growing on polarized gold electrodes. For an example application of this system we grew Geobacter sulfurreducens biofilms on electrodes. EC-NMR was used to investigate growth medium flow velocities and depth-resolved acetate concentration inside the biofilm. As a novel contribution we used Monte Carlo error analysis to estimate the standard deviations of the acetate concentration measurements. Overall, we found that the disposable EC-NMR microreactor provided a 9.7 times better signal-to-noise ratio over the reusable reactor. The EC-NMR biofilm microreactor system can ultimately be used to correlate extracellular electron transfer rates with metabolic reactions and explore extracellular electron transfer mechanisms.

Cell-free protein synthesis in PDMS-glass hybrid microreactor

NASA Astrophysics Data System (ADS)

Yamamoto, Takatoki; Fujii, Teruo; Nojima, Takahiko; Hong, Jong W.; Endo, Isao

2000-08-01

A living cell has numerous kinds of proteins while only thousands of that have been identified as of now. In order to discover and produce various proteins that are applicable to biotechnological, pharmaceutical and medical applications, cell-free protein synthesis is one of the most useful and promising techniques. In this study, we developed an inexpensive microreactor with temperature control capability for protein synthesis. The microreactor consists of a sandwich of glass-based chip and PDMS(polydimethylsiloxane) chip. The thermo control system, which is composed of a heater and a temperature sensor, is fabricated with an ITO (Indium Tin Oxide) resistive material on a glass substrate by ordinary microfabrication method based on photolithography and etching techniques. The reactor chamber and flow channels are fabricated by injection micromolding of PDMS. Since one can use thermo control system on a glass substrate repeatedly by replacing only the easily-fabricated and low-cost PDMS reactor chamber, this microreactor is quite cost effective. As a demonstration, a DNA template of a GFP (Green Fluorescent Protein) is transcribed and translated using cell-free extract prepared from Escherichia coli. As a result, GFP was successfully synthesized in the present microreactor.

Microreactor-Assisted Nanomaterial Deposition for Photovoltaic Thin-Film Production

DOE Office of Scientific and Technical Information (OSTI.GOV)

None

2009-03-01

This factsheet describes a research project whose goal is to develop and demonstrate a scalable microreactor-assisted nanomaterial deposition pilot platform for the production, purification, functionalization, and solution deposition of nanomaterials for PV applications.

Design of a prototype flow microreactor for synthetic biology in vitro.

PubMed

Boehm, Christian R; Freemont, Paul S; Ces, Oscar

2013-09-07

As a reference platform for in vitro synthetic biology, we have developed a prototype flow microreactor for enzymatic biosynthesis. We report the design, implementation, and computer-aided optimisation of a three-step model pathway within a microfluidic reactor. A packed bed format was shown to be optimal for enzyme compartmentalisation after experimental evaluation of several approaches. The specific substrate conversion efficiency could significantly be improved by an optimised parameter set obtained by computational modelling. Our microreactor design provides a platform to explore new in vitro synthetic biology solutions for industrial biosynthesis.

Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering

PubMed Central

Kehres, Jan; Pedersen, Thomas; Masini, Federico; Andreasen, Jens Wenzel; Nielsen, Martin Meedom; Diaz, Ana; Nielsen, Jane Hvolbæk; Hansen, Ole

2016-01-01

The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles. PMID:26917133

Silver nanocluster catalytic microreactors for water purification

NASA Astrophysics Data System (ADS)

Da Silva, B.; Habibi, M.; Ognier, S.; Schelcher, G.; Mostafavi-Amjad, J.; Khalesifard, H. R. M.; Tatoulian, M.; Bonn, D.

2016-07-01

A new method for the elaboration of a novel type of catalytic microsystem with a high specific area catalyst is developed. A silver nanocluster catalytic microreactor was elaborated by doping a soda-lime glass with a silver salt. By applying a high power laser beam to the glass, silver nanoclusters are obtained at one of the surfaces which were characterized by BET measurements and AFM. A microfluidic chip was obtained by sealing the silver coated glass with a NOA 81 microchannel. The catalytic activity of the silver nanoclusters was then tested for the efficiency of water purification by using catalytic ozonation to oxidize an organic pollutant. The silver nanoclusters were found to be very stable in the microreactor and efficiently oxidized the pollutant, in spite of the very short residence times in the microchannel. This opens the way to study catalytic reactions in microchannels without the need of introducing the catalyst as a powder or manufacturing complex packed bed microreactors.

The use of a microreactor for rapid screening of the reaction conditions and investigation of the photoluminescence mechanism of carbon dots.

PubMed

Lu, Yue; Zhang, Ling; Lin, Hengwei

2014-04-07

A microreactor is applied and reported, for the first time, in the field of research of carbon dots (CDs), including rapid screening of the reaction conditions and investigation of the photoluminescence (PL) mechanism. Various carbonaceous precursors and solvents were selected and hundreds of reaction conditions were screened (ca. 15 min on average per condition). Through analyzing the screened conditions, tunable PL emission maxima, from about 330 to 550 nm with respectable PL quantum yields, were achieved. Moreover, the relationship between different developmental stages of the CDs and the PL properties was explored by using the microreactor. The PL emission was observed to be independent of the composition, carbonization extent, and morphology/size of the CDs. This study unambiguously presents that a microreactor could serve as a promising tool for the research of CDs. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Micro reactor integrated μ-PEM fuel cell system: a feed connector and flow field free approach

NASA Astrophysics Data System (ADS)

Balakrishnan, A.; Mueller, C.; Reinecke, H.

2013-12-01

A system level microreactor concept for hydrogen generation with Sodium Borohydride (NaBH4) is demonstrated. The uniqueness of the system is the transport and distribution feature of fuel (hydrogen) to the anode of the fuel cell without any external feed connectors and flow fields. The approach here is to use palladium film instead of feed connectors and the flow fields; palladium's property to adsorb and desorb the hydrogen at ambient and elevated condition. The proof of concept is demonstrated with a polymethyl methacrylate (PMMA) based complete system integration which includes microreactor, palladium transport layer and the self-breathing polymer electrolyte membrane (PEM) fuel cell. The hydrolysis of NaBH4 was carried out in the presence of platinum supported by nickel (NiPt). The prototype functionality is tested with NaBH4 chemical hydride. The characterization of the integrated palladium layer and fuel cell is tested with constant and switching load. The presented integrated fuel cell is observed to have a maximum power output and current of 60 mW and 280 mA respectively.

In situ photoelectrochemical/photocatalytic study of a dye discoloration in a microreactor system using TiO2 thin films.

PubMed

Montero-Ocampo, C; Gago, A; Abadias, G; Gombert, B; Alonso-Vante, N

2012-11-01

In this work, we report in situ studies of UV photoelectrocatalytic discoloration of a dye (indigo carmine) by a TiO(2) thin film in a microreactor to demonstrate the driving force of the applied electrode potential and the dye flow rate toward dye discoloration kinetics. TiO(2) 65-nm-thick thin films were deposited by PVD magnetron sputtering technique on a conducting glass substrate of fluorinated tin oxide. A microreactor to measure the discoloration rate, the electrode potential, and the photocurrent in situ, was developed. The dye solutions, before and after measurements in the microreactor, were analyzed by Raman spectroscopy. The annealed TiO(2) thin films had anatase structure with preferential orientation (101). The discoloration rate of the dye increased with the applied potential to TiO(2) electrode. Further, acceleration of the photocatalytic reaction was achieved by utilizing dye flow recirculation to the microreactor. In both cases the photoelectrochemical/photocatalytic discoloration kinetics of the dye follows the Langmuir-Hinshelwood model, with first-order kinetics. The feasibility of dye discoloration on TiO(2) thin film electrodes, prepared by magnetron sputtering using a flow microreactor system, has been clearly demonstrated. The discoloration rate is enhanced by applying a positive potential (E (AP)) and/or increasing the flow rate. The fastest discoloration and shortest irradiation time (50 min) produced 80% discoloration with an external anodic potential of 0.931 V and a flow rate of 12.2 mL min(-1).

Chemical and Toxicological Fate of Fumonisin B1 during Extrusion Processing of Corn Grits

USDA-ARS?s Scientific Manuscript database

Two batches of flaking corn grits were prepared by growing Fusarium verticillioides to contain low and high levels of fumonisin B1 (FB1), Batch-1 at 9.7 ppm and Batch-2 at 50 ppm FB1 as determined by HPLC. These two batches were extruded (Batch-1E; Batch-2E) or extruded with 10% w/w glucose supplem...

Production Methods in Industrial Microbiology.

ERIC Educational Resources Information Center

Gaden, Elmer L., Jr.

1981-01-01

Compares two methods (batch and continuous) in which microorganisms are used to produce industrial chemicals. Describes batch and continuous stirred-tank reactors and offers reasons why the batch method may be preferred. (JN)

Lithographically fabricated silicon microreactor for operando QEXAFS studies in exhaust gas catalysis during simulation of a standard driving cycle

NASA Astrophysics Data System (ADS)

Doronkin, D. E.; Baier, S.; Sheppard, T.; Benzi, F.; Grunwaldt, J.-D.

2016-05-01

Selective catalytic reduction of NOx by ammonia over Cu-ZSM-5 was monitored by operando QEXAFS during simulation of the New European Driving Cycle. The required fast temperature transients were realized using a novel silicon microreactor, enabling simultaneous spectroscopic and kinetic analysis by X-ray absorption spectroscopy (XAS) and mass spectrometry (MS). Periods of high temperature were correlated to an increase in both N2 production and change of coordination of Cu sites. This operando approach using Si microreactors can be applied to other heterogeneous catalytic systems involving fast temperature transients.

Chip-based sequencing nucleic acids

DOEpatents

Beer, Neil Reginald

2014-08-26

A system for fast DNA sequencing by amplification of genetic material within microreactors, denaturing, demulsifying, and then sequencing the material, while retaining it in a PCR/sequencing zone by a magnetic field. One embodiment includes sequencing nucleic acids on a microchip that includes a microchannel flow channel in the microchip. The nucleic acids are isolated and hybridized to magnetic nanoparticles or to magnetic polystyrene-coated beads. Microreactor droplets are formed in the microchannel flow channel. The microreactor droplets containing the nucleic acids and the magnetic nanoparticles are retained in a magnetic trap in the microchannel flow channel and sequenced.

Bioinspired Design of Alcohol Dehydrogenase@nano TiO₂ Microreactors for Sustainable Cycling of NAD⁺/NADH Coenzyme.

PubMed

Lin, Sen; Sun, Shiyong; Wang, Ke; Shen, Kexuan; Ma, Biaobiao; Ren, Yuquan; Fan, Xiaoyu

2018-02-24

The bioinspired design and construction of enzyme@capsule microreactors with specific cell-like functionality has generated tremendous interest in recent years. Inspired by their fascinating complexity, scientists have endeavored to understand the essential aspects of a natural cell and create biomimicking microreactors so as to immobilize enzymes within the hierarchical structure of a microcapsule. In this study, simultaneous encapsulation of alcohol dehydrogenase (ADH) was achieved during the preparation of microcapsules by the Pickering emulsion method using amphiphilic modified TiO₂ nanoparticles (NPs) as building blocks for assembling the photocatalytic microcapsule membrane. The ADH@TiO₂ NP microreactors exhibited dual catalytic functions, i.e., spatially confined enzymatic catalysis and the membrane-associated photocatalytic oxidation under visible light. The sustainable cycling of nicotinamide adenine dinucleotide (NAD) coenzyme between NADH and NAD⁺ was realized by enzymatic regeneration of NADH from NAD⁺ reduction, and was provided in a form that enabled further photocatalytic oxidation to NAD⁺ under visible light. This bioinspired ADH@TiO₂ NP microreactor allowed the linking of a semiconductor mineral-based inorganic photosystem to enzymatic reactions. This is a first step toward the realization of sustainable biological cycling of NAD⁺/NADH coenzyme in synthetic functional microsystems operating under visible light irradiation.

Cellulose Nanofibril Based-Aerogel Microreactors: A High Efficiency and Easy Recoverable W/O/W Membrane Separation System

PubMed Central

Zhang, Fang; Ren, Hao; Dou, Jing; Tong, Guolin; Deng, Yulin

2017-01-01

Hereby we report a novel cellulose nanofirbril aerogel-based W/O/W microreactor system that can be used for fast and high efficient molecule or ions extraction and separation. The ultra-light cellulose nanofibril based aerogel microspheres with high porous structure and water storage capacity were prepared. The aerogel microspheres that were saturated with stripping solution were dispersed in an oil phase to form a stable water-in-oil (W/O) suspension. This suspension was then dispersed in large amount of external waste water to form W/O/W microreactor system. Similar to a conventional emulsion liquid membrane (ELM), the molecules or ions in external water can quickly transport to the internal water phase. However, the microreactor is also significantly different from traditional ELM: the water saturated nanocellulose cellulose aerogel microspheres can be easily removed by filtration or centrifugation after extraction reaction. The condensed materials in the filtrated aerogel particles can be squeezed and washed out and aerogel microspheres can be reused. This novel process overcomes the key barrier step of demulsification in traditional ELM process. Our experimental indicates the novel microreactor was able to extract 93% phenol and 82% Cu2+ from external water phase in a few minutes, suggesting its great potential for industrial applications. PMID:28059153

Screening of neuraminidase inhibitors from traditional Chinese medicines by integrating capillary electrophoresis with immobilized enzyme microreactor.

PubMed

Zhao, Haiyan; Chen, Zilin

2014-05-02

A simple and effective neuraminidase-immobilized capillary microreactor was fabricated by glutaraldehyde cross-linking technology for screening the neuraminidase inhibitors from traditional Chinese medicines. The substrate and product were separated by CE in short-end injection mode within 2 min. Dual-wavelength ultraviolet detection was employed to eliminate the interference from the screened compounds. The parameters relating to the separation efficiency and the activity of immobilized neuraminidase were systematically evaluated. The activity of the immobilized neuraminidase remained 90% after 30 days storage at 4°C. The immobilized NA microreactor could be continuously used for more than 200 runs. The Michaelis-Menten constant of neuraminidase was determined by the microreactor as 136.6 ± 10.8 μM. In addition, six in eighteen natural products were found as potent inhibitors and the inhibition potentials were ranked in the following order: bavachinin>bavachin>baicalein>baicalin>chrysin and vitexin. The half-maximal inhibitory concentrations were 59.52 ± 4.12, 65.28 ± 1.07, 44.79 ± 1.21 and 31.62 ± 2.04 for baicalein, baicalin, bavachin and bavachinin, respectively. The results demonstrated that the neuraminidase-immobilized capillary microreactor was a very effective tool for screening neuraminidase inhibitors from traditional Chinese medicines. Copyright © 2014 Elsevier B.V. All rights reserved.

Cellulose Nanofibril Based-Aerogel Microreactors: A High Efficiency and Easy Recoverable W/O/W Membrane Separation System

NASA Astrophysics Data System (ADS)

Zhang, Fang; Ren, Hao; Dou, Jing; Tong, Guolin; Deng, Yulin

2017-01-01

Hereby we report a novel cellulose nanofirbril aerogel-based W/O/W microreactor system that can be used for fast and high efficient molecule or ions extraction and separation. The ultra-light cellulose nanofibril based aerogel microspheres with high porous structure and water storage capacity were prepared. The aerogel microspheres that were saturated with stripping solution were dispersed in an oil phase to form a stable water-in-oil (W/O) suspension. This suspension was then dispersed in large amount of external waste water to form W/O/W microreactor system. Similar to a conventional emulsion liquid membrane (ELM), the molecules or ions in external water can quickly transport to the internal water phase. However, the microreactor is also significantly different from traditional ELM: the water saturated nanocellulose cellulose aerogel microspheres can be easily removed by filtration or centrifugation after extraction reaction. The condensed materials in the filtrated aerogel particles can be squeezed and washed out and aerogel microspheres can be reused. This novel process overcomes the key barrier step of demulsification in traditional ELM process. Our experimental indicates the novel microreactor was able to extract 93% phenol and 82% Cu2+ from external water phase in a few minutes, suggesting its great potential for industrial applications.

Batch compositions for cordierite ceramics

DOEpatents

Hickman, David L.

1994-07-26

Ceramic products consisting principally of cordierite and a method for making them are provided, the method employing batches comprising a mineral component and a chemical component, the mineral component comprising clay and talc and the chemical component consisting essentially of a combination of the powdered oxides, hydroxides, or hydrous oxides of magnesium, aluminum and silicon. Ceramics made by extrusion and firing of the batches can exhibit low porosity, high strength and low thermal expansion coefficients.

Microfluidic labeling of biomolecules with radiometals for use in nuclear medicine.

PubMed

Wheeler, Tobias D; Zeng, Dexing; Desai, Amit V; Önal, Birce; Reichert, David E; Kenis, Paul J A

2010-12-21

Radiometal-based radiopharmaceuticals, used as imaging and therapeutic agents in nuclear medicine, consist of a radiometal that is bound to a targeting biomolecule (BM) using a bifunctional chelator (BFC). Conventional, macroscale radiolabeling methods use an excess of the BFC-BM conjugate (ligand) to achieve high radiolabeling yields. Subsequently, to achieve maximal specific activity (minimal amount of unlabeled ligand), extensive chromatographic purification is required to remove unlabeled ligand, often resulting in longer synthesis times and loss of imaging sensitivity due to radioactive decay. Here we describe a microreactor that overcomes the above issues through integration of efficient mixing and heating strategies while working with small volumes of concentrated reagents. As a model reaction, we radiolabel 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid (DOTA) conjugated to the peptide cyclo(Arg-Gly-Asp-DPhe-Lys) with (64)Cu(2+). We show that the microreactor (made from polydimethylsiloxane and glass) can withstand 260 mCi of activity over 720 hours and retains only minimal amounts of (64)Cu(2+) (<5%) upon repeated use. A direct comparison between the radiolabeling yields obtained using the microreactor and conventional radiolabeling methods shows that improved mixing and heat transfer in the microreactor leads to higher yields for identical reaction conditions. Most importantly, by using small volumes (~10 µL) of concentrated solutions of reagents (>50 µM), yields of over 90% can be achieved in the microreactor when using a 1:1 stoichiometry of radiometal to BFC-BM. These high yields eliminate the need for use of excess amounts of often precious BM and obviate the need for a chromatographic purification process to remove unlabeled ligand. The results reported here demonstrate the potential of microreactor technology to improve the production of patient-tailored doses of radiometal-based radiopharmaceuticals in the clinic.

Study on the photocatalytic reaction kinetics in a TiO2 nanoparticles coated microreactor integrated microfluidics device.

PubMed

Liu, Ai-Lin; Li, Zhong-Qiu; Wu, Zeng-Qiang; Xia, Xing-Hua

2018-05-15

For study of the photocatalytic reaction kinetics in a confined microsystem, a photocatalysis microreactor integrated on a microfluidic device has been fabricated using an on-line UV/vis detector. The performance of the photocatalysis microreactor is evaluated by the photocatalytic degradation of Rhodamine B chosen as model target by using commercial titanium dioxide (Degussa P25, TiO 2 ) nanoparticles as a photocatalyst. Results show that the photocatalytic reaction occurs via the Langmuir-Hinshelwood mechanism and the photocatalysis kinetics in the confined microsystem (r = 0.359 min -1 ) is about 10 times larger than that in macrosystem (r = 0.033 min -1 ). In addition, the photocatalysis activity of the immobilized TiO 2 nanoparticles in the microreactor exhibits good stability under flowing conditions. The present microchip device offers an interesting platform for screening of photocatalysts and exploration of photocatalysis mechanisms and kinetics. Copyright © 2018 Elsevier B.V. All rights reserved.

Streptavidin-functionalized capillary immune microreactor for highly efficient chemiluminescent immunoassay.

PubMed

Yang, Zhanjun; Zong, Chen; Ju, Huangxian; Yan, Feng

2011-11-07

A streptavidin functionalized capillary immune microreactor was designed for highly efficient flow-through chemiluminescent (CL) immunoassay. The functionalized capillary could be used as both a support for highly efficient immobilization of antibody and a flow cell for flow-through immunoassay. The functionalized inner wall and the capture process were characterized using scanning electron microscopy. Compared to conventional packed tube or thin-layer cell immunoreactor, the proposed microreactor showed remarkable properties such as lower cost, simpler fabrication, better practicality and wider dynamic range for fast CL immunoassay with good reproducibility and stability. Using α-fetoprotein as model analyte, the highly efficient CL flow-through immunoassay system showed a linear range of 3 orders of magnitude from 0.5 to 200 ng mL(-1) and a low detection limit of 0.1 ng mL(-1). The capillary immune microreactor could make up the shortcoming of conventional CL immunoreactors and provided a promising alternative for highly efficient flow-injection immunoassay. Copyright © 2011 Elsevier B.V. All rights reserved.

Multiple reuses of Rhodococcus ruber TH3 free cells to produce acrylamide in a membrane dispersion microreactor.

PubMed

Li, Jiahui; Liu, Junqi; Chen, Jie; Wang, Yujun; Luo, Guangsheng; Yu, Huimin

2015-01-01

In this work, multiple reuses of Rhodococcus ruber TH3 free cells for the hydration of acrylonitrile to produce acrylamide in a membrane dispersion microreactor were carried out. Through using a centrifuge, the reactions reached 39.9, 39.5, 38.6 and 38.0wt% of the final acrylamide product concentration respectively within 35min in a four cycle reuse of free cells. In contrast, using a stirring tank, free cells could only be used once with the same addition speed of acrylonitrile with a microreactor. Through observing the dissolution behavior of acrylonitrile microdroplets in a free cell solution using a coaxial microfluidic device and microscope, it was found that the acrylonitrile microdroplets with a diameter of 75μm were rarely observed within a length of 2cm channel within 10s, which illustrated that the microreactor can intensify the reaction rate to reduce the inhibition of acrylonitrile and acrylamide. Copyright © 2015 Elsevier Ltd. All rights reserved.

40 CFR 98.128 - Definitions.

Code of Federal Regulations, 2013 CFR

2013-07-01

... processing. An isolated intermediate is usually a product of chemical synthesis. Storage of an isolated... withdrawal of product do not occur simultaneously in a batch operation. Batch emission episode means a... process operations. By-product means a chemical that is produced coincidentally during the production of...

40 CFR 98.128 - Definitions.

Code of Federal Regulations, 2012 CFR

2012-07-01

... stored before subsequent processing. An isolated intermediate is usually a product of chemical synthesis... withdrawal of product do not occur simultaneously in a batch operation. Batch emission episode means a... process operations. By-product means a chemical that is produced coincidentally during the production of...

40 CFR 98.128 - Definitions.

Code of Federal Regulations, 2014 CFR

2014-07-01

... processing. An isolated intermediate is usually a product of chemical synthesis. Storage of an isolated... withdrawal of product do not occur simultaneously in a batch operation. Batch emission episode means a... process operations. By-product means a chemical that is produced coincidentally during the production of...

High-rate synthesis of phosphine-stabilized undecagold nanoclusters using a multilayered micromixer.

PubMed

Jin, Hyung Dae; Garrison, Anna; Tseng, T; Paul, Brian K; Chang, Chih-Hung

2010-11-05

Growth in the potential applications of nanomaterials has led to a focus on the development of new manufacturing approaches for these materials. In particular, an increased demand due to the unique properties of nanomaterials requires a substantial yield of high-performance materials and a simultaneous reduction in the environmental impact of these processes. In this paper, a high-rate production of phosphine-stabilized undecagold nanoclusters was achieved using a layer-up strategy which involves the use of microlamination architectures; the patterning and bonding of thin layers of material (laminae) to create a multilayered micromixer in the range of 25-250 µm thick was used to step up the production of phosphine-stabilized undecagold nanoclusters. The continuous production of highly monodispersed phosphine-stabilized undecagold nanoclusters at a rate of about 11.8 (mg s(-1)) was achieved using a microreactor with a size of 1.687 cm(3). This result is about 500 times over conventional batch syntheses based on the production rate per reactor volume.

High-rate synthesis of phosphine-stabilized undecagold nanoclusters using a multilayered micromixer

NASA Astrophysics Data System (ADS)

Jin, Hyung Dae; Garrison, Anna; Tseng, T.; Paul, Brian K.; Chang, Chih-Hung

2010-11-01

Growth in the potential applications of nanomaterials has led to a focus on the development of new manufacturing approaches for these materials. In particular, an increased demand due to the unique properties of nanomaterials requires a substantial yield of high-performance materials and a simultaneous reduction in the environmental impact of these processes. In this paper, a high-rate production of phosphine-stabilized undecagold nanoclusters was achieved using a layer-up strategy which involves the use of microlamination architectures; the patterning and bonding of thin layers of material (laminae) to create a multilayered micromixer in the range of 25-250 µm thick was used to step up the production of phosphine-stabilized undecagold nanoclusters. The continuous production of highly monodispersed phosphine-stabilized undecagold nanoclusters at a rate of about 11.8 (mg s - 1) was achieved using a microreactor with a size of 1.687 cm3. This result is about 500 times over conventional batch syntheses based on the production rate per reactor volume.

FUGITIVE EMISSION SOURCES AND BATCH OPERATIONS IN SYNTHETIC ORGANIC CHEMICAL PRODUCTION

EPA Science Inventory

This survey report was developed for the EPA for use in assessing the potential magnitude of fugitive volatile organic compound (VOC) emissions from agitator seals, cooling towers and batch operations in the production of 378 designated chemicals. The information presented in thi...

Paper-based microreactor integrating cell culture and subsequent immunoassay for the investigation of cellular phosphorylation.

PubMed

Lei, Kin Fong; Huang, Chia-Hao

2014-12-24

Investigation of cellular phosphorylation and signaling pathway has recently gained much attention for the study of pathogenesis of cancer. Related conventional bioanalytical operations for this study including cell culture and Western blotting are time-consuming and labor-intensive. In this work, a paper-based microreactor has been developed to integrate cell culture and subsequent immunoassay on a single paper. The paper-based microreactor was a filter paper with an array of circular zones for running multiple cell cultures and subsequent immunoassays. Cancer cells were directly seeded in the circular zones without hydrogel encapsulation and cultured for 1 day. Subsequently, protein expressions including structural, functional, and phosphorylated proteins of the cells could be detected by their specific antibodies, respectively. Study of the activation level of phosphorylated Stat3 of liver cancer cells stimulated by IL-6 cytokine was demonstrated by the paper-based microreactor. This technique can highly reduce tedious bioanalytical operation and sample and reagent consumption. Also, the time required by the entire process can be shortened. This work provides a simple and rapid screening tool for the investigation of cellular phosphorylation and signaling pathway for understanding the pathogenesis of cancer. In addition, the operation of the paper-based microreactor is compatible to the molecular biological training, and therefore, it has the potential to be developed for routine protocol for various research areas in conventional bioanalytical laboratories.

40 CFR 63.1323 - Batch process vents-methods and procedures for group determination.

Code of Federal Regulations, 2010 CFR

2010-07-01

... accepted chemical engineering principles, measurable process parameters, or physical or chemical laws or... recovering monomer, reaction products, by-products, or solvent from a stripper operated in batch mode, and the primary condenser recovering monomer, reaction products, by-products, or solvent from a...

Integrated Microreactor for Chemical and Biochemical Applications

NASA Technical Reports Server (NTRS)

Schwesinger, N.; Dressler, L.; Frank, Th.; Wurmus, H.

1995-01-01

A completely integrated microreactor was developed that allows for the processing of very small amounts of chemical solutions. The entire system comprises several pumps and valves arranged in different branches as well as a mixing unit and a reaction chamber. The streaming path of each branch contains two valves and one pump each. The pumps are driven by piezoelectric elements mounted on thin glass membranes. Each pump is about 3.5 mm x 3.5 mm x 0.7 mm. A pumping rate up to 25 microliters per hour can be achieved. The operational voltage ranges between 40 and 200 V. A volume stroke up to 1.5 millimeter is achievable from the membrane structures. The valves are designed as passive valves. Sealing is by thin metal films. The dimension of a valve unit is 0.8 x 0.8. 07 mm. The ends of the separate streaming branches are arranged to meet in one point. This point acts as the beginning of a mixer unit which contains several fork-shaped channels. The arrangement of these channels allows for the division of the whole liquid stream into partial streams and their reuniting. A homogeneous mixing of solutions and/or gases can be observed after having passed about 10 of the fork elements. A reaction chamber is arranged behind the mixing unit to support the chemical reaction of special fluids. This unit contains heating elements placed outside of the chamber. The complete system is arranged in a modular structure and is built up of silicon. It comprises three silicon wafers bonded together by applying the silicon direct bonding technology. The silicon structures are made only by wet chemical etching processes. The fluid connections to the outside are realized using standard injection needles glued into v-shaped structures on the silicon wafers. It is possible to integrate other components, like sensors or electronic circuits using silicon as the basic material.

Miniaturized flow system based on enzyme modified PMMA microreactor for amperometric determination of glucose.

PubMed

Cerdeira Ferreira, Luís Marcos; da Costa, Eric Tavares; do Lago, Claudimir Lucio; Angnes, Lúcio

2013-09-15

This paper describes the development of a microfluidic system having as main component an enzymatic reactor constituted by a microchannel assembled in poly(methyl methacrylate) (PMMA) substrate connected to an amperometric detector. A CO2 laser engraving machine was used to make the channels, which in sequence were thermally sealed. The internal surfaces of the microchannels were chemically modified with polyethyleneimine (PEI), which showed good effectiveness for the immobilization of the glucose oxidase enzyme using glutaraldehyde as crosslinking agent, producing a very effective microreactor for the detection of glucose. The hydrogen peroxide generated by the enzymatic reaction was detected in an electrochemical flow cell localized outside of the reactor using a platinum disk as the working electrode. The proposed system was applied to the differential amperometric determination of glucose content in soft drinks showing good repeatability (DPR=1.72%, n=50), low detection limit (1.40×10(-6)molL(-1)), high sampling frequency (calculated as 345 samples h(-1)), and relatively good stability for long-term use. The results were in close agreement with those obtained by the classical spectrophotometric method utilized to quantify glucose in biological fluids. Copyright © 2013 Elsevier B.V. All rights reserved.

Ceramic microsystem incorporating a microreactor with immobilized biocatalyst for enzymatic spectrophotometric assays.

PubMed

Baeza, Mireia; López, Carmen; Alonso, Julián; López-Santín, Josep; Alvaro, Gregorio

2010-02-01

Low-temperature cofired ceramics (LTCC) technology is a versatile fabrication technique used to construct microflow systems. It permits the integration of several unitary operations (pretreatment, separation, (bio)chemical reaction, and detection stage) of an analytical process in a modular or monolithic way. Moreover, because of its compatibility with biological material, LTCC is adequate for analytical applications based on enzymatic reactions. Here we present the design, construction, and evaluation of a LTCC microfluidic system that integrates a microreactor (internal volume, 24.28 microL) with an immobilized beta-galactosidase from Escherichia coli (0.479 activity units) and an optical flow cell to measure the product of the enzymatic reaction. The enzyme was immobilized on a glyoxal-agarose support, maintaining its activity along the time of the study. As a proof of concept, the LTCC-beta-galactosidase system was tested by measuring the conversion of ortho-nitrophenyl beta-D-galactopyranoside, the substrate usually employed for activity determinations. Once packed in a monolithically integrated microcolumn, the miniaturized flow system was characterized, the operational conditions optimized (flow rate and injection volume), and its performance successfully evaluated by determining the beta-galactosidase substrate concentration at the millimolar level.

Recent changes in patenting behavior in microprocess technology and its possible use for gas-liquid reactions and the oxidation of glucose.

PubMed

Dencic, Ivana; Hessel, Volker; de Croon, Mart H J M; Meuldijk, Jan; van der Doelen, Christianus W J; Koch, Kasper

2012-02-13

The miniaturization of continuous processes has been of increasing interest in the past decade, and microreaction technology and flow chemistry have moved from academic and industrial research to commercial applications. With industry taking up such innovations, this trend is also reflected in the patenting behavior of companies active in this area. This review is a continuation of the review paper on microreactor patents published by Hessel et al. and indicates major changes in patenting trends since 2006. Moreover, a different patent database search algorithm is presented, which complements the algorithm explained in the previous review. In addition, the preservation of intellectual property is analyzed for multiphase reactions and particularly solid-catalyzed gas-liquid reactions in microreactors, which play an important role in the chemical and pharmaceutical industries and are reactions that benefit largely from microprocessing. Among other results, we show that the number of patents has increased in this field, with solid-catalyst design and deposition, control of the flow pattern, and ensured stable flow as the main challenges. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Lithographically fabricated silicon microreactor for in situ characterization of heterogeneous catalysts—Enabling correlative characterization techniques

NASA Astrophysics Data System (ADS)

Baier, S.; Rochet, A.; Hofmann, G.; Kraut, M.; Grunwaldt, J.-D.

2015-06-01

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The silicon microreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy. Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor for in situ studies.

Lithographically fabricated silicon microreactor for in situ characterization of heterogeneous catalysts—Enabling correlative characterization techniques.

PubMed

Baier, S; Rochet, A; Hofmann, G; Kraut, M; Grunwaldt, J-D

2015-06-01

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The silicon microreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy. Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor for in situ studies.

Chitosan-microreactor: a versatile approach for heterogeneous organic synthesis in microfluidics.

PubMed

Basavaraju, K C; Sharma, Siddharth; Singh, Ajay K; Im, Do Jin; Kim, Dong-Pyo

2014-07-01

Microreactors have been proven to be efficient tools for a variety of homogeneous organic transformations due to their mixing efficiency, which results in very fast reactions, better heat and mass transfer, and simple scale-up. However, in heterogeneous catalytic reactions each catalyst needs an individual substrate as support. Herein, a versatile approach to immobilize metal catalysts on chitosan as a common substrate is presented. Chitosan, accommodating many metal catalysts, is grafted onto the microchannel surface as nanobrush. The versatility, catalytic efficiency, and stability/durability of the microreactor are demonstrated for a number of organic transformations involving various metal compounds as catalysts. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A biphasic oxidation of alcohols to aldehydes and ketones using a simplified packed-bed microreactor

PubMed Central

Bogdan, Andrew

2009-01-01

Summary We demonstrate the preparation and characterization of a simplified packed-bed microreactor using an immobilized TEMPO catalyst shown to oxidize primary and secondary alcohols via the biphasic Anelli-Montanari protocol. Oxidations occurred in high yields with great stability over time. We observed that plugs of aqueous oxidant and organic alcohol entered the reactor as plugs but merged into an emulsion on the packed-bed. The emulsion coalesced into larger plugs upon exiting the reactor, leaving the organic product separate from the aqueous by-products. Furthermore, the microreactor oxidized a wide range of alcohols and remained active in excess of 100 trials without showing any loss of catalytic activity. PMID:19478910

Investigation of chemical and spin dynamics in micellized radical pairs by time-resolved stimulated nuclear polarization. Theory and experiment

NASA Astrophysics Data System (ADS)

Parnachev, A. P.; Bagryanskaya, E. G.; Tarasov, V. F.; Lukzen, N. N.; Sagdeev, R. Z.

1995-10-01

A numerical solution of the stochastic Liouville equation for a microreactor model is applied to the theoretical treatment of time-resolved stimulated nuclear polarization data, obtained during the investigation of micellized radical pairs, conducted in two different modes. Escape rate constants and relaxation parameters of radical pairs formed in the photolysis of methyldeoxybenzoin and benzoin in alkyl sulfate micelles of different sizes have been obtained. The conditions of the S-T 0 quantum oscillations in SNP kinetics have been determined.

Externally controlled pressure and temperature microreactor for in situ x-ray diffraction, visual and spectroscopic reaction investigations under supercritical and subcritical conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Diefenbacher, Jason; McKelvy, Michael; Chizmeshya, Andrew V.G.

2005-01-01

A microreactor has been developed for in situ, spectroscopic investigations of materials and reaction processes with full external pressure and temperature control from ambient conditions to 400 deg. C and 310 bar. The sample chamber is in direct contact with an external manifold, whereby gases, liquids or fluids can be injected and their activities controlled prior to and under investigation conditions. The microreactor employs high strength, single crystal moissanite windows which allow direct probe beam interaction with a sample to investigate in situ reaction processes and other materials properties. The relatively large volume of the cell, along with full opticalmore » accessibility and external temperature and pressure control, make this reaction cell well suited for experimental investigations involving any combination of gas, fluid, and solid interactions. The microreactor's capabilities are demonstrated through an in situ x-ray diffraction study of the conversion of a meta-serpentine sample to magnesite under high pressure and temperature. Serpentine is one of the mineral candidates for the implementation of mineral carbonation, an intriguing carbon sequestration candidate technology.« less

Externally controlled pressure and temperature microreactor for in situ x-ray diffraction, visual and spectroscopic reaction investigations under supercritical and subcritial conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Diefenbacher, J.; McKelvy, M.; Chizemeshya, A.V.

2010-07-13

A microreactor has been developed for in situ, spectroscopic investigations of materials and reaction processes with full external pressure and temperature control from ambient conditions to 400 C and 310 bar. The sample chamber is in direct contact with an external manifold, whereby gases, liquids or fluids can be injected and their activities controlled prior to and under investigation conditions. The microreactor employs high strength, single crystal moissanite windows which allow direct probe beam interaction with a sample to investigate in situ reaction processes and other materials properties. The relatively large volume of the cell, along with full optical accessibilitymore » and external temperature and pressure control, make this reaction cell well suited for experimental investigations involving any combination of gas, fluid, and solid interactions. The microreactor's capabilities are demonstrated through an in situ x-ray diffraction study of the conversion of a meta-serpentine sample to magnesite under high pressure and temperature. Serpentine is one of the mineral candidates for the implementation of mineral carbonation, an intriguing carbon sequestration candidate technology.« less

Novel monolithic enzymatic microreactor based on single-enzyme nanoparticles for highly efficient proteolysis and its application in multidimensional liquid chromatography.

PubMed

Gao, Mingxia; Zhang, Peng; Hong, Guangfeng; Guan, Xia; Yan, Guoquan; Deng, Chunhui; Zhang, Xiangmin

2009-10-30

In this work, a novel and facile monolithic enzymatic microreactor was prepared in the fused-silica capillary via a two-step procedure including surface acryloylation and in situ aqueous polymerization/immobilization to encapsulate a single enzyme, and its application to fast protein digestion through a direct matrix-assisted laser desorption/ionization time-of-flight mass spectrometer (MALDI-TOF-MS) analysis was demonstrated. At first, vinyl groups on the protein surface were generated by a mild acryloylation with N-acryloxysuccinimide in alkali buffer. Then, acryloylated enzyme was encapsulated into polyacrylates by free-radical copolymerization with acrylamide as the monomer, N,N'-methylenebisacrylamide as the cross-linker, and N,N,N',N'-tetramethylethylenediamine/ammonium persulfate as the initiator. Finally, polymers were immobilized onto the activated inner wall of capillaries via the reaction of vinyl groups. Capability of the enzyme-immobilized monolithic microreactor was demonstrated by myoglobin and bovine serum albumin as model proteins. The digestion products were characterized using MALDI-TOF-MS with sequence coverage of 94% and 29% observed. This microreactor was also applied to the analysis of fractions through two-dimensional separation of weak anion exchange/reversed-phase liquid chromatography of human liver extract. After a database search, 16 unique peptides corresponding to 3 proteins were identified when two RPLC fractions of human liver extract were digested by the microreactor. This opens a route for its future application in top-down proteomic analysis.

Flexible metal patterning in glass microfluidic structures using femtosecond laser direct-write ablation followed by electroless plating

NASA Astrophysics Data System (ADS)

Xu, Jian; Midorikawa, Katsumi; Sugioka, Koji

2014-03-01

A simple and flexible technique for integrating metal micropatterns into glass microfluidic structures based on threedimensional femtosecond laser microfabrication is presented. Femtosecond laser direct writing followed by thermal treatment and successive chemical etching allows us to fabricate three-dimensional microfluidic structures such as microchannels and microreservoirs inside photosensitive glass. Then, the femtosecond laser direct-write ablation followed by electroless metal plating enables space-selective deposition of patterned metal films on desired locations of internal walls of the fabricated microfluidic structures. The developed technique is applied to integrate a metal microheater into a glass microchannel to control the temperature of liquid samples in the channel, which can be used as a microreactor for enhancement of chemical reactions.

Synthesis of tin monosulfide (SnS) nanoparticles using surfactant free microemulsion (SFME) with the single microemulsion scheme

NASA Astrophysics Data System (ADS)

Tarkas, Hemant S.; Marathe, Deepak M.; Mahajan, Mrunal S.; Muntaser, Faisal; Patil, Mahendra B.; Tak, Swapnil R.; Sali, Jaydeep V.

2017-02-01

Synthesis of monomorphic, SnS nanoparticles without using a capping agent is a difficult task with chemical route of synthesis. This paper reports on synthesis of tin monosulfide (SnS) nanopartilces with dimension in the quantum-dot regime using surfactant free microemulsion with single microemulsion scheme. This has been achieved by reaction in microreactors in the CME (C: chlorobenzene, M: methanol and E: ethylene glycol) microemulsion system. This is an easy and controllable chemical route for synthesis of SnS nanoparticles. Nanoparticle diameter showed prominent dependence on microemulsion concentration and marginal dependence on microemulsion temperature in the temperature range studied. The SnS nanoparticles formed with this method form stable dispersion in Tolune.

40 CFR 63.1323 - Batch process vents-methods and procedures for group determination.

Code of Federal Regulations, 2014 CFR

2014-07-01

... accepted chemical engineering principles, measurable process parameters, or physical or chemical laws or... paragraph (b)(5) of this section. Engineering assessment may be used to estimate emissions from a batch... defined in paragraph (b)(5) of this section, through engineering assessment, as defined in paragraph (b)(6...

40 CFR 63.1323 - Batch process vents-methods and procedures for group determination.

Code of Federal Regulations, 2011 CFR

2011-07-01

... accepted chemical engineering principles, measurable process parameters, or physical or chemical laws or... paragraph (b)(5) of this section. Engineering assessment may be used to estimate emissions from a batch... defined in paragraph (b)(5) of this section, through engineering assessment, as defined in paragraph (b)(6...

40 CFR 63.1323 - Batch process vents-methods and procedures for group determination.

Code of Federal Regulations, 2013 CFR

2013-07-01

... accepted chemical engineering principles, measurable process parameters, or physical or chemical laws or... paragraph (b)(5) of this section. Engineering assessment may be used to estimate emissions from a batch... defined in paragraph (b)(5) of this section, through engineering assessment, as defined in paragraph (b)(6...

40 CFR 63.1323 - Batch process vents-methods and procedures for group determination.

Code of Federal Regulations, 2012 CFR

2012-07-01

... accepted chemical engineering principles, measurable process parameters, or physical or chemical laws or... paragraph (b)(5) of this section. Engineering assessment may be used to estimate emissions from a batch... defined in paragraph (b)(5) of this section, through engineering assessment, as defined in paragraph (b)(6...

B827 Chemical Synthhesis Project - Industrial Control System Integration - Statement of Work & Specification with Attachments 1-14

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wade, F. E.

The Chemical Synthesis Pilot Process at the Lawrence Livermore National Laboratory (LLNL) Site 300 827 Complex will be used to synthesize small quantities of material to support research and development. The project will modernize and increase current capabilities for chemical synthesis at LLNL. The primary objective of this project is the conversion of a non-automated hands-on process to a remoteoperation process, while providing enhanced batch process step control, stored recipe-specific parameter sets, process variable visibility, monitoring, alarm and warning handling, and comprehensive batch record data logging. This Statement of Work and Specification provides the industrial-grade process control requirements for themore » chemical synthesis batching control system, hereafter referred to as the “Control System” to be delivered by the System Integrator.« less

An Organotypic Liver System for Tumor Progression

DTIC Science & Technology

2006-04-01

a physiologically relevant microreactor that has proved suitable for organotypic liver culture to investigate metastatic seeding. The sub-millimeter...metastasis. Our objective is to utilize a physiologically relevant microreactor that has proved suitable for organotypic liver culture (3) to...C Yates, D B Stolz, L Griffith, A Wells (2004) Direct Visualization of Prostate Cancer Progression Utilizing a Bioreactor. American Association

Lithographically fabricated silicon microreactor for in situ characterization of heterogeneous catalysts—Enabling correlative characterization techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baier, S.; Rochet, A.; Hofmann, G.

2015-06-15

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The silicon microreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy. Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor formore » in situ studies.« less

Colliding-Droplet Microreactor: Rapid On-Demand Inertial Mixing and Metal-Catalyzed Aqueous Phase Oxidation Processes.

PubMed

Davis, Ryan D; Jacobs, Michael I; Houle, Frances A; Wilson, Kevin R

2017-11-21

In-depth investigations of the kinetics of aqueous chemistry occurring in microdroplet environments require experimental techniques that allow a reaction to be initiated at a well-defined point in time and space. Merging microdroplets of different reactants is one such approach. The mixing dynamics of unconfined (airborne) microdroplets have yet to be studied in detail, which is an essential step toward widespread use and application of merged droplet microreactors for monitoring chemical reactions. Here, we present an on-demand experimental approach for initiating chemical reactions in and characterizing the mixing dynamics of colliding airborne microdroplets (40 ± 5 μm diameter) using a streak-based fluorescence microscopy technique. The advantages of this approach include the ability to generate two well-controlled monodisperse microdroplet streams and collide (and thus mix) the microdroplets with high spatial and temporal control while consuming small amounts of sample (<0.1 μL/s). Mixing times are influenced not only by the velocity at which microdroplets collide but also the geometry of the collision (i.e., head-on vs off-center collision). For head-on collisions, we achieve submillisecond mixing times ranging from ∼900 μs at a collision velocity of 0.1 m/s to <200 μs at ∼6 m/s. For low-velocity (<1 m/s) off-center collisions, mixing times were consistent with the head-on cases. For high-velocity (i.e., > 1 m/s) off-center collisions, mixing times increased by as much as a factor of 6 (e.g., at ∼6 m/s, mixing times increased from <200 μs for head-on collisions to ∼1200 μs for highly off-center collisions). At collision velocities >7 m/s, droplet separation and fragmentation occurred, resulting in incomplete mixing. These results suggest a limited range of collision velocities over which complete and rapid mixing can be achieved when using airborne merged microdroplets to, e.g., study reaction kinetics when reaction times are short relative to typical bulk reactor mixing times. We benchmark our reactor using an aqueous-phase oxidation reaction: iron-catalyzed hydroxyl radical production from hydrogen peroxide (Fenton's reaction) and subsequent aqueous-phase oxidation of organic species in solution. Kinetic simulations of our measurements show that quantitative agreement can be obtained using known bulk-phase kinetics for bimolecular reactions in our colliding-droplet microreactor.

Colliding-Droplet Microreactor: Rapid On-Demand Inertial Mixing and Metal-Catalyzed Aqueous Phase Oxidation Processes

DOE PAGES

Davis, Ryan D.; Jacobs, Michael I.; Houle, Frances A.; ...

2017-10-30

In-depth investigations of the kinetics of aqueous chemistry occurring in microdroplet environments require experimental techniques that allow a reaction to be initiated at a well-defined point in time and space. Merging microdroplets of different reactants is one such approach. The mixing dynamics of unconfined (airborne) microdroplets have yet to be studied in detail, which is an essential step toward widespread use and application of merged droplet microreactors for monitoring chemical reactions. Here, we present an on-demand experimental approach for initiating chemical reactions in and characterizing the mixing dynamics of colliding airborne microdroplets (40 ± 5 μm diameter) using a streak-basedmore » fluorescence microscopy technique. The advantages of this approach include the ability to generate two well-controlled monodisperse microdroplet streams and collide (and thus mix) the microdroplets with high spatial and temporal control while consuming small amounts of sample (<0.1 μL/s). Mixing times are influenced not only by the velocity at which microdroplets collide but also the geometry of the collision (i.e., head-on vs off-center collision). For head-on collisions, we achieve submillisecond mixing times ranging from ~900 μs at a collision velocity of 0.1 m/s to <200 μs at ~6 m/s. For low-velocity (<1 m/s) off-center collisions, mixing times were consistent with the head-on cases. For high-velocity (i.e., > 1 m/s) off-center collisions, mixing times increased by as much as a factor of 6 (e.g., at ~6 m/s, mixing times increased from <200 μs for head-on collisions to ~1200 μs for highly off-center collisions). At collision velocities >7 m/s, droplet separation and fragmentation occurred, resulting in incomplete mixing. These results suggest a limited range of collision velocities over which complete and rapid mixing can be achieved when using airborne merged microdroplets to, e.g., study reaction kinetics when reaction times are short relative to typical bulk reactor mixing times. We benchmark our reactor using an aqueous-phase oxidation reaction: iron-catalyzed hydroxyl radical production from hydrogen peroxide (Fenton's reaction) and subsequent aqueous-phase oxidation of organic species in solution. In conclusion, kinetic simulations of our measurements show that quantitative agreement can be obtained using known bulk-phase kinetics for bimolecular reactions in our colliding-droplet microreactor.« less

Colliding-Droplet Microreactor: Rapid On-Demand Inertial Mixing and Metal-Catalyzed Aqueous Phase Oxidation Processes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Davis, Ryan D.; Jacobs, Michael I.; Houle, Frances A.

In-depth investigations of the kinetics of aqueous chemistry occurring in microdroplet environments require experimental techniques that allow a reaction to be initiated at a well-defined point in time and space. Merging microdroplets of different reactants is one such approach. The mixing dynamics of unconfined (airborne) microdroplets have yet to be studied in detail, which is an essential step toward widespread use and application of merged droplet microreactors for monitoring chemical reactions. Here, we present an on-demand experimental approach for initiating chemical reactions in and characterizing the mixing dynamics of colliding airborne microdroplets (40 ± 5 μm diameter) using a streak-basedmore » fluorescence microscopy technique. The advantages of this approach include the ability to generate two well-controlled monodisperse microdroplet streams and collide (and thus mix) the microdroplets with high spatial and temporal control while consuming small amounts of sample (<0.1 μL/s). Mixing times are influenced not only by the velocity at which microdroplets collide but also the geometry of the collision (i.e., head-on vs off-center collision). For head-on collisions, we achieve submillisecond mixing times ranging from ~900 μs at a collision velocity of 0.1 m/s to <200 μs at ~6 m/s. For low-velocity (<1 m/s) off-center collisions, mixing times were consistent with the head-on cases. For high-velocity (i.e., > 1 m/s) off-center collisions, mixing times increased by as much as a factor of 6 (e.g., at ~6 m/s, mixing times increased from <200 μs for head-on collisions to ~1200 μs for highly off-center collisions). At collision velocities >7 m/s, droplet separation and fragmentation occurred, resulting in incomplete mixing. These results suggest a limited range of collision velocities over which complete and rapid mixing can be achieved when using airborne merged microdroplets to, e.g., study reaction kinetics when reaction times are short relative to typical bulk reactor mixing times. We benchmark our reactor using an aqueous-phase oxidation reaction: iron-catalyzed hydroxyl radical production from hydrogen peroxide (Fenton's reaction) and subsequent aqueous-phase oxidation of organic species in solution. In conclusion, kinetic simulations of our measurements show that quantitative agreement can be obtained using known bulk-phase kinetics for bimolecular reactions in our colliding-droplet microreactor.« less

Biphasic microreactor for efficient membrane protein pretreatment with a combination of formic acid assisted solubilization, on-column pH adjustment, reduction, alkylation, and tryptic digestion.

PubMed

Zhao, Qun; Liang, Yu; Yuan, Huiming; Sui, Zhigang; Wu, Qi; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

2013-09-17

Combining good dissolving ability of formic acid (FA) for membrane proteins and excellent complementary retention behavior of proteins on strong cation exchange (SCX) and strong anion exchange (SAX) materials, a biphasic microreactor was established to pretreat membrane proteins at microgram and even nanogram levels. With membrane proteins solubilized by FA, all of the proteomics sample processing procedures, including protein preconcentration, pH adjustment, reduction, and alkylation, as well as tryptic digestion, were integrated into an "SCX-SAX" biphasic capillary column. To evaluate the performance of the developed microreactor, a mixture of bovine serum albumin, myoglobin, and cytochrome c was pretreated. Compared with the results obtained by the traditional in-solution process, the peptide recovery (93% vs 83%) and analysis throughput (3.5 vs 14 h) were obviously improved. The microreactor was further applied for the pretreatment of 14 μg of membrane proteins extracted from rat cerebellums, and 416 integral membrane proteins (IMPs) (43% of total protein groups) and 103 transmembrane peptides were identified by two-dimensional nanoliquid chromatography-electrospray ionization tandem mass spectrometry (2D nano-LC-ESI-MS/MS) in triplicate analysis. With the starting sample preparation amount decreased to as low as 50 ng, 64 IMPs and 17 transmembrane peptides were identified confidently, while those obtained by the traditional in-solution method were 10 and 1, respectively. All these results demonstrated that such an "SCX-SAX" based biphasic microreactor could offer a promising tool for the pretreatment of trace membrane proteins with high efficiency and throughput.

Design and characterization of a prototype enzyme microreactor: quantification of immobilized transketolase kinetics.

PubMed

Matosevic, S; Lye, G J; Baganz, F

2010-01-01

In this work, we describe the design of an immobilized enzyme microreactor (IEMR) for use in transketolase (TK) bioconversion process characterization. The prototype microreactor is based on a 200-microm ID fused silica capillary for quantitative kinetic analysis. The concept is based on the reversible immobilization of His(6)-tagged enzymes via Ni-NTA linkage to surface derivatized silica. For the initial microreactor design, the mode of operation is a stop-flow analysis which promotes higher degrees of conversion. Kinetics for the immobilized TK-catalysed synthesis of L-erythrulose from substrates glycolaldehyde (GA) and hydroxypyruvate (HPA) were evaluated based on a Michaelis-Menten model. Results show that the TK kinetic parameters in the IEMR (V(max(app)) = 0.1 +/- 0.02 mmol min(-1), K(m(app)) = 26 +/- 4 mM) are comparable with those measured in free solution. Furthermore, the k(cat) for the microreactor of 4.1 x 10(5) s(-1) was close to the value for the bioconversion in free solution. This is attributed to the controlled orientation and monolayer surface coverage of the His(6)-immobilized TK. Furthermore, we show quantitative elution of the immobilized TK and the regeneration and reuse of the derivatized capillary over five cycles. The ability to quantify kinetic parameters of engineered enzymes at this scale has benefits for the rapid and parallel evaluation of evolved enzyme libraries for synthetic biology applications and for the generation of kinetic models to aid bioconversion process design and bioreactor selection as a more efficient alternative to previously established microwell-based systems for TK bioprocess characterization.

Catalyst for microelectromechanical systems microreactors

DOEpatents

Morse, Jeffrey D [Martinez, CA; Sopchak, David A [Livermore, CA; Upadhye, Ravindra S [Pleasanton, CA; Reynolds, John G [San Ramon, CA; Satcher, Joseph H [Patterson, CA; Gash, Alex E [Brentwood, CA

2010-06-29

A microreactor comprising a silicon wafer, a multiplicity of microchannels in the silicon wafer, and a catalyst coating the microchannels. In one embodiment the catalyst coating the microchannels comprises a nanostructured material. In another embodiment the catalyst coating the microchannels comprises an aerogel. In another embodiment the catalyst coating the microchannels comprises a solgel. In another embodiment the catalyst coating the microchannels comprises carbon nanotubes.

Catalyst for microelectromechanical systems microreactors

DOEpatents

Morse, Jeffrey D [Martinez, CA; Sopchak, David A [Livermore, CA; Upadhye, Ravindra S [Pleasanton, CA; Reynolds, John G [San Ramon, CA; Satcher, Joseph H [Patterson, CA; Gash, Alex E [Brentwood, CA

2011-11-15

A microreactor comprising a silicon wafer, a multiplicity of microchannels in the silicon wafer, and a catalyst coating the microchannels. In one embodiment the catalyst coating the microchannels comprises a nanostructured material. In another embodiment the catalyst coating the microchannels comprises an aerogel. In another embodiment the catalyst coating the microchannels comprises a solgel. In another embodiment the catalyst coating the microchannels comprises carbon nanotubes.

Real-time spectroscopic monitoring of photocatalytic activity promoted by graphene in a microfluidic reactor

PubMed Central

Li, Yifan; Lin, Beichen; Ge, Likai; Guo, Hongchen; Chen, Xinyi; Lu, Miao

2016-01-01

Photocatalytic microreactors have been utilized as rapid, versatile platforms for the characterization of photocatalysts. In this work, a photocatalytic microreactor integrated with absorption spectroscopy was proposed for the real-time monitoring of photocatalytic activity using different catalysts. The validity of this method was investigated by the rapid screening on the photocatalytic performance of a titanium oxide (TiO2)-decorated graphene oxide (GO) sheet for the degradation of methylene blue under monochromatic visible irradiation. The sampling interval time could be minimized to 10 s for achieving real-time detection. The best photocatalytic activity was observed for an optimized TiO2/GO weight mixing ratio of 7:11, with a reaction rate constant up to 0.067 min−1. The addition of GO into TiO2 enhances photocatalytic activity and adsorption of MB molecules. The synthetic reaction rate constant was up to approximately 0.11 min−1, which was also the highest among the catalysts. The microreactor exhibited good sensitivity and reproducibility without weakening the performance of the photocatalysts. Consequently, the photocatalytic microreactor is promising as a simple, portable, and rapid screening tool for new photocatalysts. PMID:27346555

Synthesis of CuInSe2 nanocrystals using a continuous hot-injection microreactor

NASA Astrophysics Data System (ADS)

Jin, Hyung Dae; Chang, Chih-Hung

2012-10-01

A very rapid and simple synthesis of CuInSe2 nanocrystals (NCs) was successfully performed using a continuous hot-injection microreactor with a high throughput per reactor volume. It was found that copper-rich CuInSe2 with a sphalerite structure was formed initially followed by the formation of more ordered CuInSe2 at longer reaction times along with the formation of Cu2Se and In2Se3. Binary syntheses were performed and the results show a much faster formation rate of Cu2Se than In2Se3. The rate limiting step in the formation of CuInSe2 is forming the In2Se3 intermediate. Rapid synthesis of stoichiometric CuInSe2 NCs using a continuous-flow microreactor was accomplished by properly adjusting the Cu/In precursor ratio. Tuning the ratio of coordinating solvents can cause size differences from 2.6 to 4.1 nm, bandgaps from 1.1 to 1.3 eV, and different production yields of NCs. The highest production yield as determined by weight was achieved up to 660 mg/h using a microreactor with a small volume of 3.2 cm3.

Continuous-flow biosynthesis of Au-Ag bimetallic nanoparticles in a microreactor

NASA Astrophysics Data System (ADS)

Liu, Hongyu; Huang, Jiale; Sun, Daohua; Odoom-Wubah, Tareque; Li, Jun; Li, Qingbiao

2014-11-01

Herein, a microfluidic biosynthesis of Au-Ag bimetallic nanoparticle (NP) in a tubular microreactor, based on simultaneous reduction of HAuCl4 and AgNO3 precursors in the presence of Cacumen Platycladi ( C. Platycladi) extract was studied. The flow velocity profile was numerically analyzed with computational fluid dynamics. Au-Ag bimetallic NPs with Ag/Au molar ratios of 1:1 and 2:1 were synthesized, respectively. The alloy formation, morphology, structure, and size were investigated by UV-Vis spectra analysis, transmission electron microscopy (TEM), high resolution TEM, scanning TEM, and energy-dispersive X-ray analysis. In addition, the effects of volumetric flow rate, reaction temperature, and concentration of C. Platycladi extract and NaOH on the properties of the as-synthesized Au-Ag bimetallic NPs were investigated. The results indicated that these factors could not only affect the molar ratios of the two elements in the Au-Ag bimetallic NPs, but also affect particle size which can be adjusted from 3.3 to 5.6 nm. The process was very rapid and green, since a microreactor was employed with no additional synthetic reagents used. This work is anticipated to provide useful parameters for continuous-flow biosynthesis of bimetallic NPs in microreactors.

Real-time spectroscopic monitoring of photocatalytic activity promoted by graphene in a microfluidic reactor

NASA Astrophysics Data System (ADS)

Li, Yifan; Lin, Beichen; Ge, Likai; Guo, Hongchen; Chen, Xinyi; Lu, Miao

2016-06-01

Photocatalytic microreactors have been utilized as rapid, versatile platforms for the characterization of photocatalysts. In this work, a photocatalytic microreactor integrated with absorption spectroscopy was proposed for the real-time monitoring of photocatalytic activity using different catalysts. The validity of this method was investigated by the rapid screening on the photocatalytic performance of a titanium oxide (TiO2)-decorated graphene oxide (GO) sheet for the degradation of methylene blue under monochromatic visible irradiation. The sampling interval time could be minimized to 10 s for achieving real-time detection. The best photocatalytic activity was observed for an optimized TiO2/GO weight mixing ratio of 7:11, with a reaction rate constant up to 0.067 min-1. The addition of GO into TiO2 enhances photocatalytic activity and adsorption of MB molecules. The synthetic reaction rate constant was up to approximately 0.11 min-1, which was also the highest among the catalysts. The microreactor exhibited good sensitivity and reproducibility without weakening the performance of the photocatalysts. Consequently, the photocatalytic microreactor is promising as a simple, portable, and rapid screening tool for new photocatalysts.

Development of an enzymatic microreactor based on microencapsulated laccase with off-line capillary electrophoresis for measurement of oxidation reactions.

PubMed

Roman-Gusetu, Georgiana; Waldron, Karen C; Rochefort, Dominic

2009-11-20

Microencapsulation is used here as a new technique to immobilize enzymes in a microreactor coupled off-line to capillary electrophoresis (CE), allowing the determination of enzymatic reaction products. The redox enzyme laccase was encapsulated using the method of interfacial cross-linking of poly(ethyleneimine) (PEI). The 50 microm diameter capsules were slurry packed from a suspension into a capillary-sized reactor made easily and quickly from a short length of 530 microm diameter fused-silica tubing. The volume of the bed of laccase microcapsules in the microreactor was in the order of 1.1 microL through which 50 microL of the substrate o-phenylenediamine (OPD) was flowed. The oxidation product 2,3-diaminophenazine (DAP) and the remaining OPD were quantified by CE in a pH 2.5 phosphate buffer. Peak migration time reproducibility was in the order of 0.4% RSD and peak area reproducibility was less than 1.7% RSD within the same day. Using the OPD peak area calibration curve, a conversion efficiency of 48% was achieved for a 2-min oxidation reaction in the microreactor.

Uniform integration of gold nanoparticles in PDMS microfluidics with 3D micromixing

NASA Astrophysics Data System (ADS)

SadAbadi, H.; Packirisamy, M.; Wuthrich, R.

2015-09-01

The integration of gold nanoparticles (AuNPs) on the surface of polydimethylsiloxane (PDMS) microfluidics for biosensing applications is a challenging task. In this paper we address this issue by integration of pre-synthesized AuNPs (in a microreactor) into a microfluidic system. This method explored the affinity of AuNPs toward the PDMS surface so that the pre-synthesized particles will be adsorbed onto the channel walls. AuNPs were synthesized inside a microreactor before integration. In order to improve the size uniformity of the synthesized AuNPs and also to provide full mixing of reactants, a 3D-micromixer was designed, fabricated and then integrated with the microreactor in a single platform. SEM and UV/Vis spectroscopy were used to characterize the AuNPs on the PDMS surface.

Searching CA Condensates, On-Line and Batch.

ERIC Educational Resources Information Center

Kaminecki, Ronald M.; And Others

Batch mode processing is compared, using cost-effectiveness, with on-line processing for computer-aided searching of chemical abstracts. Consideration for time, need, coverage, and adaptability are found to be the criteria by which a searcher selects a method, and sometimes both methods are used. There is a tradeoff between batch mode's slower…

Functionalization of polycarbonate with proteins; open-tubular enzymatic microreactors.

PubMed

Ogończyk, D; Jankowski, P; Garstecki, P

2012-08-07

This paper examines a set of techniques for the immobilization of enzymes on the surface of microchannels fabricated in polycarbonate (PC). Our experiments identify the method that uses combined physico-chemical immobilization on a layer of polyethyleneimine (PEI) as a reproducible vista for the robust immobilization of proteins. As an example, we demonstrate the fabrication, throughput and stability of an open-tubular reactor draped with alkaline phosphatase (ALP, EC 3.1.3.1) as a model enzyme. As PC is suitable for industrial applications the method could potentially be used to immobilize proteins in numbered-up implementations.

Contribution of microreactor technology and flow chemistry to the development of green and sustainable synthesis.

PubMed

Fanelli, Flavio; Parisi, Giovanna; Degennaro, Leonardo; Luisi, Renzo

2017-01-01

Microreactor technology and flow chemistry could play an important role in the development of green and sustainable synthetic processes. In this review, some recent relevant examples in the field of flash chemistry, catalysis, hazardous chemistry and continuous flow processing are described. Selected examples highlight the role that flow chemistry could play in the near future for a sustainable development.

Thermomyces lanuginosus lipase-catalyzed synthesis of natural flavor esters in a continuous flow microreactor.

PubMed

Gumel, Ahmad Mohammed; Annuar, M S M

2016-06-01

Enzymatic catalysis is considered to be among the most environmental friendly processes for the synthesis of fine chemicals. In this study, lipase from Thermomyces lanuginosus (Lecitase Ultra™) was used to catalyze the synthesis of flavor esters, i.e., methyl butanoate and methyl benzoate by esterification of the acids with methanol in a microfluidic system. Maximum reaction rates of 195 and 115 mM min -1 corresponding to catalytic efficiencies (k cat /K M ) of 0.30 and 0.24 min -1  mM -1 as well as yield conversion of 54 and 41 % were observed in methyl butanoate and methyl benzoate synthesis, respectively. Catalytic turnover (k cat ) was higher for methyl butanoate synthesis. Rate of synthesis and yield decreased with increasing flow rates. For both esters, increase in microfluidic flow rate resulted in increased advective transport over molecular diffusion and reaction rate, thus lower conversion. In microfluidic synthesis using T. lanuginosus lipase, the following reaction conditions were 40 °C, flow rate 0.1 mL min -1 , and 123 U g -1 enzyme loading found to be the optimum operating limits. The work demonstrated the application of enzyme(s) in a microreactor system for the synthesis of industrially important esters.

Hydrothermal gasification of Cladophora glomerata macroalgae over its hydrochar as a catalyst for hydrogen-rich gas production.

PubMed

Safari, Farid; Norouzi, Omid; Tavasoli, Ahmad

2016-12-01

A tubular batch micro-reactor system was used for hydrothermal gasification (HTG) of Cladophora glomerata (C. glomerata) as green macroalgae found in the southern coast of the Caspian Sea, Iran. Non-catalytic tests were performed to determine the optimum condition for hydrogen production. Hydrochar, as a solid residue of non-catalytic HTG was characterized by BET, FESEM, and ICP-OES methods to determine its physiochemical properties. Surface area and pore volume of C. glomerata increased drastically after HTG. Also, the aqueous products were identified and quantified by GC-MS and GC-FID methods. Hydrochar was loaded to the reactor to determine its catalytic effect on HTG. HTG was promoted by inorganic compounds in the hydrochar and its porosity. The maximum hydrogen yield of 9.63mmol/g was observed in the presence of algal hydrochar with the weight ratio of 0.4 to feedstock. Also, acids production was inhibited while phenol production was promoted in the presence of hydrochar. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Study on HPLC fingerprint of Oldenlandia diffusa].

PubMed

Chen, Yan; Yao, Zhi-Hong; Dai, Yi; Cheng, Hong; Wen, Li-Rong; Zhou, Guang-Xiong; Yao, Xin-Sheng

2012-06-01

To establish the HPLC fingerprint chromatogram of Oldenlandia diffusa coupled with chemometrics means for the quality control of multi-batches of medicinal material. The separation was developed on C18 column(4.6 mm x 250 mm, 5 microm) by gradient elution with acetonitrile-water(both containing 0.1 per thousand (V/V) ocetic acid) as mobile phase at a flow rate of 0.8 mL/min, the detection wavelength at 238 nm and column temperature at 30 degrees C. The HPLC fingerprint chromatogram of Oldenlandia diffusa was set up and the main characteristic peaks were identified by comparing with chemical reference substance. The quality of 22 batches of medicinal material was evaluated by similarity assay as well as principal component analysis (PCA) and cluster analysis. The established HPLC fingerprint chromatogram of Oldenlandia diffusa was specific, precise, reproducible and stable. 11 peaks were chemically identified. The similarity of 17 batches of Oldenlandia diffusa was obviously higher than 5 batches of adulterants. PCA showed that 17 batches of Oldenlandia diffusa were in a domain and 5 batches of adulterants were far apart from the domain. The cluster analysis of the 22 batches of medicinal material showed that 17 batches of Oldenlandia diffusa were in a cluster while 5 batches of adulterants were excluded. Further cluster analysis was carried out for the quality consistency of 17 batches of Oldenlandia diffusa and accordingly they were devided into 4 clusters. With the combination of chemometrics means, the HPLC fingerprint chromatogram provides a method for evaluation of authenticity and quality control of Oldenlandia diffusa, which is favorable to improve overall quality control of Oldenlandia diffusa.

Cementation of colloidal particles on electrodes in a galvanic microreactor.

PubMed

Jan, Linda; Punckt, Christian; Aksay, Ilhan A

2013-07-10

We have studied the processes leading to the cementation of colloidal particles during their autonomous assembly on corroding copper electrodes within a Cu-Au galvanic microreactor. We determined the onset of particle immobilization through particle tracking, monitored the dissolution of copper as well as the deposition of insoluble products of the corrosion reactions in situ, and showed that particle immobilization initiated after reaction products (RPs) began to deposit on the electrode substrate. We further demonstrated that the time and the extent of RP precipitation and thus the strength of the particle-substrate bond could be tuned by varying the amount of copper in the system and the microreactor pH. The ability to cement colloidal particles at locations undergoing corrosion illustrates that the studied colloidal assembly approach holds potential for applications in dynamic material property adaptation.

The nature of chlorine-inhibition of photocatalytic degradation of dichloroacetic acid in a TiO2-based microreactor.

PubMed

Krivec, M; Dillert, R; Bahnemann, D W; Mehle, A; Štrancar, J; Dražić, G

2014-07-28

Photocatalytic degradation of dichloroacetic acid (DCA) was studied in a continuous-flow set-up using a titanium microreactor with an immobilized double-layered TiO2 nanoparticle/nanotube film. Chloride ions, formed during the degradation process, negatively affect the photocatalytic efficiency and at a certain concentration (approximately 0.5 mM) completely stop the reaction in the microreactor. Two proposed mechanisms of inhibition with chloride ions, competitive adsorption and photogenerated-hole scavenging, have been proposed and investigated by adsorption isotherms and electron paramagnetic resonance (EPR) measurements. The results show that chloride ions block the DCA adsorption sites on the titania surface and reduce the amount of adsorbed DCA molecules. The scavenging effect of chloride ions during photocatalysis through the formation of chlorine radicals was not detected.

Bioproduction of food additives hexanal and hexanoic acid in a microreactor.

PubMed

Šalić, Anita; Pindrić, Katarina; Zelić, Bruno

2013-12-01

Hexanal and hexanoic acid have number of applications in food and cosmetic industry because of their organoleptic characteristics. Problems like low yields, formation of unwanted by-products, and large quantities of waste in their traditional production processes are the reasons for developing new production methods. Biotransformation in a microreactor, as an alternative to classical synthesis processes, is being investigated. Because conditions in microreactors can be precisely controlled, the quality of the product and its purity can also be improved. Biocatalytic oxidation of hexanol to hexanal and hexanoic acid using suspended and immobilized permeabilized whole baker's yeast cells and suspended and immobilized purified alcohol dehydrogenase (ADH) was investigated in this study. Three different methods for covalent immobilization of biocatalyst were analyzed, and the best method for biocatalyst attachment on microchannel wall was used in the production of hexanal and hexanoic acid.

Contribution of microreactor technology and flow chemistry to the development of green and sustainable synthesis

PubMed Central

Fanelli, Flavio; Parisi, Giovanna

2017-01-01

Microreactor technology and flow chemistry could play an important role in the development of green and sustainable synthetic processes. In this review, some recent relevant examples in the field of flash chemistry, catalysis, hazardous chemistry and continuous flow processing are described. Selected examples highlight the role that flow chemistry could play in the near future for a sustainable development. PMID:28405232

Pharmacy on Demand Feasibility Assessment

DTIC Science & Technology

2008-07-19

We have successfully carried out the first two steps of the ibuprofen synthesis in our microreactor using homogeneous reactions in a continuous...Average of two trials. c Average of three trials. d Using a 0.25 M stock solution of isobutylbenzene. e Using a 0.5 M stock solution of...the creation of a packed-bed microreactor is the preparation of the solid-supported reagent. We have previously demonstrated that the performance

Novel Catalyst for the Chirality Selective Synthesis of Single Walled Carbon Nanotubes

DTIC Science & Technology

2015-05-12

hierarchical structures comprising nitrogen- doped reduced GO (rGO) and acid- oxidized SWCNTs was produced using a linear hydrothermal microreactor. Fiber...structures comprising nitrogen- doped reduced GO (rGO) and acidoxidized SWCNTs was produced using a linear hydrothermal microreactor. Fiber micro... doped into Co/SiO2 catalysts to change their chirality selectivity. Further, enrichment of (9,8) nanotubes was carried out by extraction using fluorene

A replaceable dual-enzyme capillary microreactor using magnetic beads and its application for simultaneous detection of acetaldehyde and pyruvate.

PubMed

Shi, Jing; Zhao, Wenwen; Chen, Yuanfang; Guo, Liping; Yang, Li

2012-07-01

A novel replaceable dual-enzyme capillary microreactor was developed and evaluated using magnetic fields to immobilize the alcohol dehydrogenase (ADH)- and lactate dehydrogenase (LDH)-coated magnetic beads at desired positions in the capillary. The dual-enzyme assay was achieved by measuring the two consumption peaks of the coenzyme β-nicotinamide adenine dinucleotide (NADH), which were related to the ADH reaction and LDH reaction. The dual-enzyme capillary microreactor was constructed using magnetic beads without any modification of the inner surface of the capillary, and showed great stability and reproducibility. The electrophoretic resolution for different analytes can be easily controlled by altering the relative distance of different enzyme-coated magnetic beads. The apparent K(m) values for acetaldehyde with ADH-catalyzed reaction and for pyruvate with LDH-catalyzed reaction were determined. The detection limits for acetaldehyde and pyruvate determination are 0.01 and 0.016 mM (S/N = 3), respectively. The proposed method was successfully applied to simultaneously determine the acetaldehyde and pyruvate contents in beer samples. The results indicated that combing magnetic beads with CE is of great value to perform replaceable and controllable multienzyme capillary microreactor for investigation of a series of enzyme reactions and determination of multisubstrates. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In situ IR and X-ray high spatial-resolution microspectroscopy measurements of multistep organic transformation in flow microreactor catalyzed by Au nanoclusters.

PubMed

Gross, Elad; Shu, Xing-Zhong; Alayoglu, Selim; Bechtel, Hans A; Martin, Michael C; Toste, F Dean; Somorjai, Gabor A

2014-03-05

Analysis of catalytic organic transformations in flow reactors and detection of short-lived intermediates are essential for optimization of these complex reactions. In this study, spectral mapping of a multistep catalytic reaction in a flow microreactor was performed with a spatial resolution of 15 μm, employing micrometer-sized synchrotron-based IR and X-ray beams. Two nanometer sized Au nanoclusters were supported on mesoporous SiO2, packed in a flow microreactor, and activated toward the cascade reaction of pyran formation. High catalytic conversion and tunable products selectivity were achieved under continuous flow conditions. In situ synchrotron-sourced IR microspectroscopy detected the evolution of the reactant, vinyl ether, into the primary product, allenic aldehyde, which then catalytically transformed into acetal, the secondary product. By tuning the residence time of the reactants in a flow microreactor a detailed analysis of the reaction kinetics was performed. An in situ micrometer X-ray absorption spectroscopy scan along the flow reactor correlated locally enhanced catalytic conversion, as detected by IR microspectroscopy, to areas with high concentration of Au(III), the catalytically active species. These results demonstrate the fundamental understanding of the mechanism of catalytic reactions which can be achieved by the detailed mapping of organic transformations in flow reactors.

Brewery and liquid manure wastewaters as potential feedstocks for microbial fuel cells: a performance study.

PubMed

Angosto, J M; Fernández-López, J A; Godínez, C

2015-01-01

This work aims at the comparison of the electrical and chemical performance of microbial fuel cells (MFCs) fed with several types of brewery and manure industrial wastewaters. Experiments were conducted in a single-cell MFC with the cathode exposed to air operated in batch and fed-batch modes. In fed-batch mode, after 4 days of operation, a standard MFC was refilled with crude wastewater to regenerate the biofilm and recreate initial feeding conditions. Brewery wastewater (CV1) mixed with pig-farm liquid manure (PU sample) gave the highest voltage (199.8 mV) and power density (340 mW/m3) outputs than non-mixed brewery waste water. Also, coulombic efficiency is much larger in the mixture (11%) than in the others (2-3%). However, in terms of chemical oxygen demand removal, the performance showed to be poorer (53%) for the mixed sample than in the pure brewery sample (93%). Fed-batch operation showed to be a good alternate for quasi-continuous operation, with equivalent electrical and chemical yields as compared with normal batchwise operation.

40 CFR Table 2 to Subpart Ffff of... - Emission Limits and Work Practice Standards for Batch Process Vents

Code of Federal Regulations, 2010 CFR

2010-07-01

...: Miscellaneous Organic Chemical Manufacturing Pt. 63, Subpt. FFFF, Table 2 Table 2 to Subpart FFFF of Part 63... vents a. Reduce collective uncontrolled organic HAP emissions from the sum of all batch process vents... applicable. b. Reduce collective uncontrolled organic HAP emissions from the sum of all batch process vents...

40 CFR Table 2 to Subpart Ffff of... - Emission Limits and Work Practice Standards for Batch Process Vents

Code of Federal Regulations, 2011 CFR

2011-07-01

...: Miscellaneous Organic Chemical Manufacturing Pt. 63, Subpt. FFFF, Table 2 Table 2 to Subpart FFFF of Part 63... vents a. Reduce collective uncontrolled organic HAP emissions from the sum of all batch process vents... applicable. b. Reduce collective uncontrolled organic HAP emissions from the sum of all batch process vents...

Pyrolysis of Cyclopentadienone: Mechanistic Insights from a Direct Measurement of Product Branching Ratios

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ormond, Thomas K.; Scheer, Adam M.; Nimlos, Mark R.

2015-07-16

The thermal decomposition of cyclopentadienone (C5H4-O) has been studied in a flash pyrolysis continuous flow microreactor. Passing dilute samples of o-phenylene sulfite (C6H4O2SO) in He through the microreactor at elevated temperatures yields a relatively clean source of C5H4-O. The pyrolysis of C5H4-O was investigated over the temperature range 1000-2000 K.

Versatile hydrogel-based nanocrystal microreactors towards uniform fluorescent photonic crystal supraballs

NASA Astrophysics Data System (ADS)

Zhang, Jing; Tian, Yu; Ling, Lu-Ting; Yin, Su-Na; Wang, Cai-Feng; Chen, Su

2014-12-01

Versatile hydrogel-based nanocrystal (NC) microreactors were designed in this work for the construction of uniform fluorescence colloidal photonic crystal (CPC) supraballs. The hydrogel-based microspheres with sizes ranging from 150 to 300 nm were prepared by seeded copolymerization of acrylic acid and 2-hydroxyethyl methacrylate with micrometer-sized PS seed particles. As an independent NC microreactor, the as-synthesized hydrogel microsphere can effectively capture the guest cadmium ions due to the abundant carboxyl groups inside. Followed by the introduction of chalcogenides, in situ generation of higher-uptake NCs with sizes less than 5 nm was finally realized. Additionally, with the aid of the microfluidic device, the as-obtained NC-latex hybrids can be further self-assembled to bi-functional CPC supraballs bearing brilliant structural colors and uniform fluorescence. This research offers an alternative way to finely bind CPCs with NCs, which will facilitate progress in fields of self-assembled functional colloids and photonic materials.

CE-microreactor-CE-MS/MS for protein analysis

PubMed Central

Schoenherr, Regine M.; Ye, Mingliang; Vannatta, Michael

2008-01-01

We present a proof-of-principle for a fully automated bottom-up approach to protein characterization. Proteins are first separated by capillary electrophoresis. A pepsin microreactor is incorporated into the distal end of this capillary. Peptides formed in the reactor are transferred to a second capillary, where they are separated by capillary electrophoresis and characterized by mass spectrometry. While peptides generated from one digestion are being separated in the second capillary, the next protein fraction undergoes digestion in the microreactor. The migration time in the first dimension capillary is characteristic of the protein while migration time in the second dimension is characteristic of the peptide. Spot capacity for the two-dimensional separation is 590. A MS/MS analysis of a mixture of cytochrome C and myoglobin generated Mascot MOWSE scores of 107 for cytochrome C and 58 for myoglobin. The sequence coverages were 48% and 22%, respectively. PMID:17295444

Continuous flow synthesis of VO2 nanoparticles or nanorods by using a microreactor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Jie; Sun, Yugang; Muehleisen, Ralph T.

The invention provides a method for producing composite nanoparticles, the method using a first compound capable of transitioning from a monoclinic to a tetragonal rutile crystal state upon heating, and having the steps of subjecting the first compound to a hydrothermal synthesis to create anisotropic crystals of the compound; encapsulating the first compound with a second compound to create a core-shell construct; and annealing the construct as needed. Also provided is a device for continuously synthesizing composite nanoparticles, the device having a first precursor supply and a second precursor supply; a mixer to homogeneously combine the first precursor and secondmore » precursor to create a liquor; a first microreactor to subject the liquor to hydrothermic conditions to create an\\isotropic particles in a continuous operation mode; and a second microreactor for coating the particles with a third precursor to create a core-shell construct.« less

Paper microfluidic-based enzyme catalyzed double microreactor.

PubMed

Ferrer, Ivonne M; Valadez, Hector; Estala, Lissette; Gomez, Frank A

2014-08-01

We describe a paper microfluidic-based enzyme catalyzed double microreactor assay using fluorescent detection. Here, solutions of lactate dehydrogenase (LDH) and diaphorase (DI) were directly spotted onto the microfluidic paper-based analytical device (μPAD). Samples containing lactic acid, resazurin, and nicotinamide adenine dinucleotide oxidized form (NAD(+) ), potassium chloride (KCl), and BSA, in MES buffer were separately spotted onto the μPAD and MES buffer flowed through the device. A cascade reaction occurs upon the sample spot overlapping with LDH to form pyruvate and nicotinamide adenine dinucleotide reduced form (NADH). Subsequently, NADH is used in the conversion of resazurin to fluorescent resorufin by DI. The μPAD avoids the need of surface functionalization or enzyme immobilization steps. These microreactor devices are low cost and easy to fabricate and effect reaction based solely on buffer capillary action. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Mineralogical characterization of selected shales in support of nuclear waste repository studies: Progress report, October 1987--September 1988

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, S. Y.; Hyder, L. K.; Baxter, P. M.

1989-07-01

One objective of the Sedimentary Rock Program at the Oak Ridge National Laboratory has been to examine end-member shales to develop a data base that will aid in evaluations if shales are ever considered as a repository host rock. Five end-member shales were selected for comprehensive characterization: the Chattanooga Shale from Fentress County, Tennessee; the Pierre Shale from Gregory County, South Dakota; the Green River Formation from Garfield County, Colorado; and the Nolichucky Shale and Pumpkin Valley Shale from Roane County, Tennessee. Detailed micromorphological and mineralogical characterizations of the shales were completed by Lee et al. (1987) in ORNL/TM-10567. Thismore » report is a supplemental characterization study that was necessary because second batches of the shale samples were needed for additional studies. Selected physical, chemical, and mineralogical properties were determined for the second batches; and their properties were compared with the results from the first batches. Physical characterization indicated that the second-batch and first-batch samples had a noticeable difference in apparent-size distributions but had similar primary-particle-size distributions. There were some differences in chemical composition between the batches, but these differences were not considered important in comparison with the differences among the end-member shales. The results of x-ray diffraction analyses showed that the second batches had mineralogical compositions very similar to the first batches. 9 refs., 9 figs., 4 tabs.« less

The use of selective adsorbents in capillary electrophoresis-mass spectrometry for analyte preconcentration and microreactions: a powerful three-dimensional tool for multiple chemical and biological applications.

PubMed

Guzman, N A; Stubbs, R J

2001-10-01

Much attention has recently been directed to the development and application of online sample preconcentration and microreactions in capillary electrophoresis using selective adsorbents based on chemical or biological specificity. The basic principle involves two interacting chemical or biological systems with high selectivity and affinity for each other. These molecular interactions in nature usually involve noncovalent and reversible chemical processes. Properly bound to a solid support, an "affinity ligand" can selectively adsorb a "target analyte" found in a simple or complex mixture at a wide range of concentrations. As a result, the isolated analyte is enriched and highly purified. When this affinity technique, allowing noncovalent chemical interactions and biochemical reactions to occur, is coupled on-line to high-resolution capillary electrophoresis and mass spectrometry, a powerful tool of chemical and biological information is created. This paper describes the concept of biological recognition and affinity interaction on-line with high-resolution separation, the fabrication of an "analyte concentrator-microreactor", optimization conditions of adsorption and desorption, the coupling to mass spectrometry, and various applications of clinical and pharmaceutical interest.

1,6-Conjugate addition of zinc alkyls to para-quinone methides in a continuous-flow microreactor.

PubMed

Jadhav, Abhijeet S; Anand, Ramasamy Vijaya

2016-12-20

An efficient method for the synthesis of alkyl diarylmethanes through the 1,6-conjugate addition of dialkylzinc reagents to para-quinone methides (p-QMs) has been developed under continuous flow conditions using a microreactor. This protocol allows to access unsymmetrical alkyl diarylmethanes in moderate to excellent yields using a wide range of p-QMs and dialkylzinc reagents. Interestingly, this transformation worked well without the requirement of a catalyst.

PMMA microreactor for chemiluminescence detection of Cu (II) based on 1,10-Phenanthroline-hydrogen peroxide reaction.

PubMed

Chen, Xueye; Shen, Jienan; Li, Tiechuan

2016-01-01

A microreactor for the chemiluminescence detection of copper (II) in water samples, based on the measurement of light emitted from the copper (II) catalysed oxidation of 1,10-phenanthroline by hydrogen peroxide in basic aqueous solution, is presented. Polymethyl methacrylate (PMMA) was chose as material for fabricating the microreactor with mill and hot bonding method. Optimized reagents conditions were found to be 6.3 × 10(-5)mol/L 1,10-phenanthroline, 1.5 × 10(-3)mol/L hydrogen peroxide, 7.0 × 10(-2)mol/L sodium hydroxide and 2.4 × 10(-5)mol/L Hexadecyl trimethyl ammonium Bromide (CTMAB). In the continuous flow injection mode the system can perform fully automated detection with a reagent consumption of only 3.5 μL each time. The linear range of the Cu (II) ions concentration was 1.5 × 10(-8) mol/L to 1.0 × 10(-4) mol/L, and the detection limit was 9.4 × 10(-9)mol/L with the S/N ratio of 4. The relative standard deviation was 3.0 % for 2.0 × 10(-6) mol/L Cu (II) ions (n = 10). The most obvious features of the detection method are simplicity, rapidity and easy fabrication of the microreactor.

Efficient synthesis of highly fluorescent carbon dots by microreactor method and their application in Fe3+ ion detection.

PubMed

Rao, Longshi; Tang, Yong; Li, Zongtao; Ding, Xinrui; Liang, Guanwei; Lu, Hanguang; Yan, Caiman; Tang, Kairui; Yu, Binhai

2017-12-01

Rapidly obtaining strong photoluminescence (PL) of carbon dots with high stability is crucial in all practical applications of carbon dots, such as cell imaging and biological detection. In this study, we proposed a rapid, continuous carbon dots synthesis technique by using a microreactor method. By taking advantage of the microreactor, we were able to rapidly synthesized CDs at a large scale in less than 5min, and a high quantum yield of 60.1% was achieved. This method is faster and more efficient than most of the previously reported methods. To explore the relationship between the microreactor structure and CDs PL properties, Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) were carried out. The results show the surface functional groups and element contents influence the PL emission. Subsequent ion detection experiments indicated that CDs are very suitable for use as nanoprobes for Fe 3+ ion detection, and the lowest detection limit for Fe 3+ is 0.239μM, which is superior to many other research studies. This rapid and simple synthesis method will not only aid the development of the quantum dots industrialization but also provide a powerful and portable tool for the rapid and continuous online synthesis of quantum dots supporting their application in cell imaging and safety detection. Copyright © 2017 Elsevier B.V. All rights reserved.

A ceramic microreactor for the synthesis of water soluble CdS and CdS/ZnS nanocrystals with on-line optical characterization

NASA Astrophysics Data System (ADS)

Pedro, Sara Gómez-De; Puyol, Mar; Izquierdo, David; Salinas, Iñigo; de La Fuente, J. M.; Alonso-Chamarro, Julián

2012-02-01

In this paper, a computer controlled microreactor to synthesize water soluble CdS and CdS/ZnS nanocrystals with in situ monitoring of the reaction progress is developed. It is based on ceramic tapes and the Low-Temperature Co-fired Ceramics technology (LTCC). As well the microsystem set-up, the microreactor fluidic design has also been thoroughly optimized. The final device is based on a hydrodynamic focusing of the reagents followed by a three-dimensional micromixer. This generates monodispersed and stable CdS and core-shell CdS/ZnS nanocrystals of 4.5 and 4.2 nm, respectively, with reproducible optical properties in terms of fluorescence emission wavelengths, bandwidth, and quantum yields, which is a key requirement for their future analytical applications. The synthetic process is also controlled in real time with the integration of an optical detection system for absorbance and fluorescence measurements based on commercial miniaturized optical components. This makes possible the efficient managing of the hydrodynamic variables to obtain the desired colloidal suspension. As a result, a simple, economic, robust and portable microsystem for the well controlled synthesis of CdS and CdS/ZnS nanocrystals is presented. Moreover, the reaction takes place in aqueous medium, thus allowing the direct modular integration of this microreactor in specific analytical microsystems, which require the use of such quantum dots as labels.

Droplet microfluidics with a nanoemulsion continuous phase.

PubMed

Gu, Tonghan; Yeap, Eunice W Q; Somasundar, Ambika; Chen, Ran; Hatton, T Alan; Khan, Saif A

2016-07-05

We present the first study of a novel, generalizable method that uses a water-in-oil nanoemulsion as the continuous phase to generate uniform aqueous micro-droplets in a capillary-based microfluidic system. We first study the droplet generation mechanism in this system and compare it to the more conventional case where a simple oil/solvent (with surfactant) is used as the continuous phase. Next, we present two versatile methods - adding demulsifying chemicals and heat treatment - to allow active online chemical interaction between the continuous and dispersed phases. These methods allow each generated micro-droplet to act as a well-mixed micro-reactor with walls that are 'permeable' to the nanoemulsion droplets and their contents. Finally, we demonstrate an application of this system in the fabrication of uniform hydrogel (alginate) micro-beads with control over particle properties such as size and swelling. Our work expands the toolbox of droplet-based microfluidics, enabling new opportunities and applications involving active colloidal continuous phases carrying chemical payloads, both in advanced materials synthesis and droplet-based screening and diagnostic methods.

Model-Based Design of Biochemical Microreactors

PubMed Central

Elbinger, Tobias; Gahn, Markus; Neuss-Radu, Maria; Hante, Falk M.; Voll, Lars M.; Leugering, Günter; Knabner, Peter

2016-01-01

Mathematical modeling of biochemical pathways is an important resource in Synthetic Biology, as the predictive power of simulating synthetic pathways represents an important step in the design of synthetic metabolons. In this paper, we are concerned with the mathematical modeling, simulation, and optimization of metabolic processes in biochemical microreactors able to carry out enzymatic reactions and to exchange metabolites with their surrounding medium. The results of the reported modeling approach are incorporated in the design of the first microreactor prototypes that are under construction. These microreactors consist of compartments separated by membranes carrying specific transporters for the input of substrates and export of products. Inside the compartments of the reactor multienzyme complexes assembled on nano-beads by peptide adapters are used to carry out metabolic reactions. The spatially resolved mathematical model describing the ongoing processes consists of a system of diffusion equations together with boundary and initial conditions. The boundary conditions model the exchange of metabolites with the neighboring compartments and the reactions at the surface of the nano-beads carrying the multienzyme complexes. Efficient and accurate approaches for numerical simulation of the mathematical model and for optimal design of the microreactor are developed. As a proof-of-concept scenario, a synthetic pathway for the conversion of sucrose to glucose-6-phosphate (G6P) was chosen. In this context, the mathematical model is employed to compute the spatio-temporal distributions of the metabolite concentrations, as well as application relevant quantities like the outflow rate of G6P. These computations are performed for different scenarios, where the number of beads as well as their loading capacity are varied. The computed metabolite distributions show spatial patterns, which differ for different experimental arrangements. Furthermore, the total output of G6P increases for scenarios where microcompartimentation of enzymes occurs. These results show that spatially resolved models are needed in the description of the conversion processes. Finally, the enzyme stoichiometry on the nano-beads is determined, which maximizes the production of glucose-6-phosphate. PMID:26913283

The Study and Development of Metal Oxide Reactive Adsorbents for the Destruction of Toxic Organic Compounds

DTIC Science & Technology

2008-04-15

been achieved, but our microreactor studies showed a slight loss in product flow from the reactor, indicating a loss of decomposition capacity for...examination by infrared spectroscopy. A second sample of the same solid was placed in the microreactor as before and treated in the same fashion... a collection of information if it does not display a currently valid OMB control number. PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ADDRESS. a

Preparation of calcium hydroxyapatite nanoparticles using microreactor and their characteristics of protein adsorption.

PubMed

Kandori, Kazuhiko; Kuroda, Tomohiko; Togashi, Shigenori; Katayama, Erika

2011-02-03

The calcium hydroxyapatite Ca(10)(PO(4))(6)(OH)(2) (Hap) nanoparticles were prepared by using microreactor and employed these Hap nanoparticles to clarify the adsorption behavior of proteins. The size of Hap particles produced by the microreactor reduced in the order of a hardness of the reaction conditions for mixing Ca(OH)(2) and H(3)PO(4) aqueous solutions, such as flow rates of both solutions and temperature. Finally, the size of the smallest Hap nanoparticle became 2 × 15 nm(2), similar to that of BSA molecule (4 × 14 nm(2)). It is noteworthy that the smallest Hap nanoparticles still possesses rodlike shape, suggesting that particles are grown along c-axis even though the reactants mixed very rapidly in narrow channels of the microreactors. The X-ray diffraction patterns of the Hap nanoparticles revealed that the crystallinity of the materials produced by the microreactor is low. The FTIR measurement indicated that the Hap nanoparticles produced by microreactor were carbonate-substituted type B Hap, where the carbonate ions replace the phosphate ions in the crystal lattice. All the adsorption isotherms of acidic bovine serum albumin (BSA), neutral myoglobin (MGB), and basic lysozyme (LSZ) onto Hap nanoparticles from 1 × 10(-4) mol/dm(3) KCl solution were the Langmuirian type. The saturated amounts of adsorbed BSA (n(S)(BSA)) for the Hap nanoparticles produced by microreactor were decreased with decrease in the mean particle length, and finally it reduced to zero for the smallest Hap nanoparticles. Similar results were observed for the adsorption of LSZ; the saturated amounts of adsorbed LSZ (n(S)(LSZ)) also reduced to zero for the smallest Hap nanoparticles. However, in the case of MGB, the saturated mounts of adsorbed MGB (n(S)(MGB)) are also depressed with decreased in their particle size, but about half of MGB molecules still adsorbed onto the smallest Hap nanoparticles. This difference in the protein adsorption behavior was explained by the difference in the size and flexibility of three kinds of proteins. The reduction of n(S)(BSA) is due to the decrease in the fraction of C sites on the side face of each Hap nanoparticle; i.e., there is not enough area left on the nanoparticle surface to adsorb large BSA molecules even though the BSA molecules are soft and their conformations are alterable. The reduction of n(S)(LSZ) was explained by the reduction of P sites. Further, rigidity of the LSZ molecules was given another possibility of the depression of n(S)(LSZ) for the Hap nanoparticles. However, MGB molecules with small and soft structure were adsorbed on the Hap nanoparticle surface by changing their conformation. We could control the amounts of adsorbed proteins by changing the particle size of Hap in the nanometer range and kinds of proteins. These obtained results may be useful for developing biomimetic materials for bone grafts and successful surgical devices in the biochemical field.

Parallel steady state studies on a milliliter scale accelerate fed-batch bioprocess design for recombinant protein production with Escherichia coli.

PubMed

Schmideder, Andreas; Cremer, Johannes H; Weuster-Botz, Dirk

2016-11-01

In general, fed-batch processes are applied for recombinant protein production with Escherichia coli (E. coli). However, state of the art methods for identifying suitable reaction conditions suffer from severe drawbacks, i.e. direct transfer of process information from parallel batch studies is often defective and sequential fed-batch studies are time-consuming and cost-intensive. In this study, continuously operated stirred-tank reactors on a milliliter scale were applied to identify suitable reaction conditions for fed-batch processes. Isopropyl β-d-1-thiogalactopyranoside (IPTG) induction strategies were varied in parallel-operated stirred-tank bioreactors to study the effects on the continuous production of the recombinant protein photoactivatable mCherry (PAmCherry) with E. coli. Best-performing induction strategies were transferred from the continuous processes on a milliliter scale to liter scale fed-batch processes. Inducing recombinant protein expression by dynamically increasing the IPTG concentration to 100 µM led to an increase in the product concentration of 21% (8.4 g L -1 ) compared to an implemented high-performance production process with the most frequently applied induction strategy by a single addition of 1000 µM IPGT. Thus, identifying feasible reaction conditions for fed-batch processes in parallel continuous studies on a milliliter scale was shown to be a powerful, novel method to accelerate bioprocess design in a cost-reducing manner. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:1426-1435, 2016. © 2016 American Institute of Chemical Engineers.

Biodegradation of Jet Fuel-4 (JP-4) in Sequencing Batch Reactors

DTIC Science & Technology

1992-06-01

nalw~eo %CUMENTATION PAGE__ _ _ _ _ _ _ _ _O 74S Ab -A258 020 L AW POi~W6 DATI .~ TYP AIMqm ,-& 0 U. glbs A~ I ma"&LFUN Mu BIODEGRADATION OF JET FUEL...Specific Objectives of This Proposal Are: 1. To assess the ability of C. resinae , P. chrysosporium and selected bacterial consortia to degrade individual...chemical components of JP-4. 2. To develop a sequencing batch reactor that utilizes C. resinae to degrade chemical components of JP-4 in contaminated

Transition Metal Dichalcogenide Growth via Close Proximity Precursor Supply

NASA Astrophysics Data System (ADS)

O'Brien, Maria; McEvoy, Niall; Hallam, Toby; Kim, Hye-Young; Berner, Nina C.; Hanlon, Damien; Lee, Kangho; Coleman, Jonathan N.; Duesberg, Georg S.

2014-12-01

Reliable chemical vapour deposition (CVD) of transition metal dichalcogenides (TMDs) is currently a highly pressing research field, as numerous potential applications rely on the production of high quality films on a macroscopic scale. Here, we show the use of liquid phase exfoliated nanosheets and patterned sputter deposited layers as solid precursors for chemical vapour deposition. TMD monolayers were realized using a close proximity precursor supply in a CVD microreactor setup. A model describing the growth mechanism, which is capable of producing TMD monolayers on arbitrary substrates, is presented. Raman spectroscopy, photoluminescence, X-ray photoelectron spectroscopy, atomic force microscopy, transmission electron microscopy, scanning electron microscopy and electrical transport measurements reveal the high quality of the TMD samples produced. Furthermore, through patterning of the precursor supply, we achieve patterned growth of monolayer TMDs in defined locations, which could be adapted for the facile production of electronic device components.

Green Route for Silver Nanoparticles Synthesis by Raphanus Sativus Extract in a Continuous Flow Tubular Microreactor

NASA Astrophysics Data System (ADS)

Jolhe, P. D.; Bhanvase, B. A.; Patil, V. S.; Sonawane, S. H.

The present work deals with the investigation of the greener route for the production of silver nanoparticles using Raphanus sativus (R. sativus) bioextract in a continuous flow tubular microreactor. The parameters affecting the particle size and distribution were investigated. From the results obtained it can be inferred that the ascorbic acid (reducing agent) present in the R. sativus bioextract is responsible for the reduction of silver ions. At optimum condition, the particle size distribution of nanoparticles is found between 18nm and 39nm. The absorbance value was found to be decreased with an increase in the diameter of the microreactor. It indicates that a number of nuclei are formed in the micrometer sized (diameter) reactor because of the better solute transfer rate leading to the formation of large number of silver nanoparticles. The study of antibacterial activity of green synthesized silver nanoparticles shows effective inhibitory activity against waterborne pathogens, Shegella and Listeria bacteria.

Hydration of acrylonitrile to produce acrylamide using biocatalyst in a membrane dispersion microreactor.

PubMed

Li, Jiahui; Chen, Jie; Wang, Yujun; Luo, Guangsheng; Yu, Huimin

2014-10-01

In this work, a membrane dispersion microreactor was utilized for the hydration of acrylonitrile to produce acrylamide. Through observation using a microscopy, it was found that the acrylonitrile was dispersed into the continuous phase (the aqueous phase contains nitrile hydratase (NHase)) as droplets with a diameter ranged from 25 to 35 μm, hence the mass transfer specific surface area was significantly increased, and the concentration of acrylamide reached 52.5 wt% within 50 min. By contrast, in stirred tanks, the concentration of acrylamide only got 39.5 wt% within 245 min. Moreover, only a few amounts of acrylonitrile were accumulated in this microreactor system. Through optimizing the flow rate, the concentration of acrylamide reached 45.8 wt% within 35 min, the short reaction time greatly weakened the inhibition of acrylonitrile and acrylamide on the enzyme activity, which is suitable for prolonging the life of free cell. Copyright © 2014 Elsevier Ltd. All rights reserved.

RELATIVE LEACHING AND AQUATIC TOXICITY OF PRESSURE-TREATED WOOD PRODUCTS USING BATCH LEACHING TESTS

EPA Science Inventory

Samples of southern yellow pine dimensional lumber, each treated with one of five different waterborne chemical preservatives, were leached using 18-hour batch leaching tests. The wood preservatives included chromated copper arsenate (CCA), alkaline copper quaternary (ACQ), coppe...

Physical and Chemical Microstructural Damage in Pressed CL-20 explosives

NASA Astrophysics Data System (ADS)

Demol, Gauthier; Sandusky, Harold W.

1999-06-01

Based upon its molecular composition, its structure, and its heat of formation, it was expected that CL-20 (hexanitrohexaazaisowurtzitane) would be more energetic and more sensitive than RDX and HMX. Reports of batch-to-batch variations in the sensitivity of neat CL-20 have led to its sensitivity being ranked in the range between the sensitivity of RDX and that of PETN. The ultimate utility of CL-20 as an ingredient in explosive and propellant formulations will depend upon the ability to understand the factors that are responsible for this batch-to-batch variability, and to control the sensitivity in formulations within acceptable limits. This work is a characterization of CL-20 at various stages in its life cycle. The evolution of damage from the initial neat crystals of CL-20 to the ready-to-use pressed pellets will be described. This characterization includes physical documentation using light microscopy and Scanning Electron Microscopy. Spatially resolved chemical analysis is also performed using Fourier-Transform Infrared Spectroscopy.

Sludge Washing and Demonstration of the DWPF Nitric/Formic Flowsheet in the SRNL Shielded Cells for Sludge Batch 9 Qualification

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pareizs, J.; Newell, D.; Martino, C.

Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to qualify the next batch of sludge – Sludge Batch 9 (SB9). Current practice is to prepare sludge batches in Tank 51 by transferring sludge to Tank 51 from other tanks. The sludge is washed and transferred to Tank 40, the current Defense Waste Process Facility (DWPF) feed tank. Prior to sludge transfer from Tank 51 to Tank 40, the Tank 51 sludge must be qualified. SRNL qualifies the sludge in multiple steps. First, a Tank 51 sample is received, then characterized, washed, and again characterized. SRNL thenmore » demonstrates the DWPF Chemical Process Cell (CPC) flowsheet with the sludge. The final step of qualification involves chemical durability measurements of glass fabricated in the DWPF CPC demonstrations. In past sludge batches, SRNL had completed the DWPF demonstration with Tank 51 sludge. For SB9, SRNL has been requested to process a blend of Tank 51 and Tank 40 at a targeted ratio of 44% Tank 51 and 56% Tank 40 on an insoluble solids basis.« less

A ceramic microreactor for the synthesis of water soluble CdS and CdS/ZnS nanocrystals with on-line optical characterization.

PubMed

Gómez-de Pedro, Sara; Puyol, Mar; Izquierdo, David; Salinas, Iñigo; de la Fuente, J M; Alonso-Chamarro, Julián

2012-02-21

In this paper, a computer controlled microreactor to synthesize water soluble CdS and CdS/ZnS nanocrystals with in situ monitoring of the reaction progress is developed. It is based on ceramic tapes and the Low-Temperature Co-fired Ceramics technology (LTCC). As well the microsystem set-up, the microreactor fluidic design has also been thoroughly optimized. The final device is based on a hydrodynamic focusing of the reagents followed by a three-dimensional micromixer. This generates monodispersed and stable CdS and core-shell CdS/ZnS nanocrystals of 4.5 and 4.2 nm, respectively, with reproducible optical properties in terms of fluorescence emission wavelengths, bandwidth, and quantum yields, which is a key requirement for their future analytical applications. The synthetic process is also controlled in real time with the integration of an optical detection system for absorbance and fluorescence measurements based on commercial miniaturized optical components. This makes possible the efficient managing of the hydrodynamic variables to obtain the desired colloidal suspension. As a result, a simple, economic, robust and portable microsystem for the well controlled synthesis of CdS and CdS/ZnS nanocrystals is presented. Moreover, the reaction takes place in aqueous medium, thus allowing the direct modular integration of this microreactor in specific analytical microsystems, which require the use of such quantum dots as labels. This journal is © The Royal Society of Chemistry 2012

Synthesis and investigation of reaction mechanisms of diamondoids produced using plasmas generated inside microcapillaries in supercritical xenon

NASA Astrophysics Data System (ADS)

Oshima, Fumito; Stauss, Sven; Inose, Yoshifumi; Terashima, Kazuo

2014-01-01

We have synthesized diamondoids using dielectric barrier discharge microplasmas generated inside a microcapillary reactor in supercritical xenon. The plasmas were generated near the critical temperature (T_{\\text{crit}} = 389.75\\,\\text{K}) and pressure (p_{\\text{crit}} = 5.84\\,\\text{MPa}) of xenon in the ranges of T/T_{\\text{crit}} = 0.964-0.983 and p/p_{\\text{crit}} = 0.998\\text-1.026 under both batch-type and continuous flow conditions with gas flow rates of 0.01-0.5 mL min-1. Micro-Raman spectra of the synthesized particles showed features characteristic of diamondoids, while gas chromatography-mass spectrometry measurements revealed that diamondoids up to undecamantane were possibly synthesized. Further, the amount of obtained diamantane was greater than those obtained using previously reported diamondoid synthesis processes that involve plasmas in supercritical fluids. This increase is attributed to the higher solubility of the supercritical medium, i.e., xenon, and the higher efficiency of the microreactor. A detailed gas chromatography-mass spectrometry analysis showed that higher diamondoids grow in a stepwise manner via the alternate removal of hydrogen atoms and the addition of methyl groups.

Unusual behavior in the reactivity of 5-substituted-1H-tetrazoles in a resistively heated microreactor

PubMed Central

Gutmann, Bernhard; Glasnov, Toma N; Razzaq, Tahseen; Goessler, Walter; Roberge, Dominique M

2011-01-01

Summary The decomposition of 5-benzhydryl-1H-tetrazole in an N-methyl-2-pyrrolidone/acetic acid/water mixture was investigated under a variety of high-temperature reaction conditions. Employing a sealed Pyrex glass vial and batch microwave conditions at 240 °C, the tetrazole is comparatively stable and complete decomposition to diphenylmethane requires more than 8 h. Similar kinetic data were obtained in conductively heated flow devices with either stainless steel or Hastelloy coils in the same temperature region. In contrast, in a flow instrument that utilizes direct electric resistance heating of the reactor coil, tetrazole decomposition was dramatically accelerated with rate constants increased by two orders of magnitude. When 5-benzhydryl-1H-tetrazole was exposed to 220 °C in this type of flow reactor, decomposition to diphenylmethane was complete within 10 min. The mechanism and kinetic parameters of tetrazole decomposition under a variety of reaction conditions were investigated. A number of possible explanations for these highly unusual rate accelerations are presented. In addition, general aspects of reactor degradation, corrosion and contamination effects of importance to continuous flow chemistry are discussed. PMID:21647324

In situ {sup 13}C MAS NMR study of n-hexane conversion on Pt and Pd supported on basic materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ivanova, I.I.; Pasau-Claerbout, A.; Seivert, M.

n-Hexane conversion was studied in situ on Pt and Pd supported on aluminum-stabilized magnesium oxide and Pt on Zeolite KL catalysts (Pt/Mg(Al)O, Pd/Mg(Al)O and Pt/KL) by means of {sup 13}C MAS NMR spectroscopy. n-Hexane 1-{sup 13}C was used as a labelled reactant. Forty NMR lines corresponding to 14 different products were resolved and identified. The NMR line assignments were confirmed by adsorption of model compounds. The NMR results were further quantified and compared with continuous flow microreactor tests. Four parallel reaction pathways were identified under flow conditions: isomerization, cracking, dehydrocyclization, and dehydrogenation. Aromatization occurs via two reaction routes: (1) n-hexanemore » dehydrogenation towards hexadienes and hexatrienes, followed by dehydrogenation of a cyclic intermediate. The former reaction pathway is prevented under NMR batch conditions. High pressures induced in the NMR cells at high reaction temperatures (573, 653 K) shift the reaction equilibrium towards hydrogenation. NMR experiments showed that on Pt catalysts aromatization occurs via a cyclohexane intermediate, whereas on Pd it takes place via methylcyclopentane ring enlargement. 54 refs., 15 figs., 3 tabs.« less

Predicting critical micelle concentration and micelle molecular weight of polysorbate 80 using compendial methods.

PubMed

Braun, Alexandra C; Ilko, David; Merget, Benjamin; Gieseler, Henning; Germershaus, Oliver; Holzgrabe, Ulrike; Meinel, Lorenz

2015-08-01

This manuscript addresses the capability of compendial methods in controlling polysorbate 80 (PS80) functionality. Based on the analysis of sixteen batches, functionality related characteristics (FRC) including critical micelle concentration (CMC), cloud point, hydrophilic-lipophilic balance (HLB) value and micelle molecular weight were correlated to chemical composition including fatty acids before and after hydrolysis, content of non-esterified polyethylene glycols and sorbitan polyethoxylates, sorbitan- and isosorbide polyethoxylate fatty acid mono- and diesters, polyoxyethylene diesters, and peroxide values. Batches from some suppliers had a high variability in functionality related characteristic (FRC), questioning the ability of the current monograph in controlling these. Interestingly, the combined use of the input parameters oleic acid content and peroxide value - both of which being monographed methods - resulted in a model adequately predicting CMC. Confining the batches to those complying with specifications for peroxide value proved oleic acid content alone as being predictive for CMC. Similarly, a four parameter model based on chemical analyses alone was instrumental in predicting the molecular weight of PS80 micelles. Improved models based on analytical outcome from fingerprint analyses are also presented. A road map controlling PS80 batches with respect to FRC and based on chemical analyses alone is provided for the formulator. Copyright © 2014 Elsevier B.V. All rights reserved.

Biomass-derived Syngas Utilization for Fuels and Chemicals - Final Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dayton, David C

2010-03-24

Executive Summary The growing gap between petroleum production and demand, mounting environmental concerns, and increasing fuel prices have stimulated intense interest in research and development (R&D) of alternative fuels, both synthetic and bio-derived. Currently, the most technically defined thermochemical route for producing alternative fuels from lignocellulosic biomass involves gasification/reforming of biomass to produce syngas (carbon monoxide [CO] + hydrogen [H2]), followed by syngas cleaning, Fischer-Tropsch synthesis (FTS) or mixed alcohol synthesis, and some product upgrading via hydroprocessing or separation. A detailed techno-economic analysis of this type of process has recently been published [1] and it highlights the need for technicalmore » breakthroughs and technology demonstration for gas cleanup and fuel synthesis. The latter two technical barrier areas contribute 40% of the total thermochemical ethanol cost and 70% of the production cost, if feedstock costs are factored out. Developing and validating technologies that reduce the capital and operating costs of these unit operations will greatly reduce the risk for commercializing integrated biomass gasification/fuel synthesis processes for biofuel production. The objective of this project is to develop and demonstrate new catalysts and catalytic processes that can efficiently convert biomass-derived syngas into diesel fuel and C2-C4 alcohols. The goal is to improve the economics of the processes by improving the catalytic activity and product selectivity, which could lead to commercialization. The project was divided into 4 tasks: Task 1: Reactor Systems: Construction of three reactor systems was a project milestone. Construction of a fixed-bed microreactor (FBR), a continuous stirred tank reactor (CSTR), and a slurry bubble column reactor (SBCR) were completed to meet this milestone. Task 2: Iron Fischer-Tropsch (FT) Catalyst: An attrition resistant iron FT catalyst will be developed and tested. Task 3: Chemical Synthesis: Promising process routes will be identified for synthesis of selected chemicals from biomass-derived syngas. A project milestone was to select promising mixed alcohol catalysts and screen productivity and performance in a fixed bed micro-reactor using bottled syngas. This milestone was successfully completed in collaboration withour catalyst development partner. Task 4: Modeling, Engineering Evaluation, and Commercial Assessment: Mass and energy balances of conceptual commercial embodiment for FT and chemical synthesis were completed.« less

40 CFR 63.488 - Methods and procedures for batch front-end process vent group determination.

Code of Federal Regulations, 2010 CFR

2010-07-01

... engineering principles, measurable process parameters, or physical or chemical laws or properties. Examples of... primary condenser recovering monomer, reaction products, by-products, or solvent from a stripper operated in batch mode, and the primary condenser recovering monomer, reaction products, by-products, or...

MODELING HEXAVALENT CHROMIUM REDUCTION IN GROUND- WATER IN FIELD-SCALE TRANSPORT AND LABORATORY BATCH EXPERIMENTS

EPA Science Inventory

A plausible and consistent model is developed to obtain a quantitative description of the gradual disappearance of hexavalent chromium (Cr(VI)) from groundwater in a small-scale field tracer test and in batch kinetic experiments using aquifer sediments under similar chemical cond...

Immobilized enzyme studies in a microscale bioreactor.

PubMed

Jones, Francis; Forrest, Scott; Palmer, Jim; Lu, Zonghuan; Elmore, John; Elmore, Bill B

2004-01-01

Novel microreactors with immobilized enzymes were fabricated using both silicon and polymer-based microfabrication techniques. The effectiveness of these reactors was examined along with their behavior over time. Urease enzyme was successfully incorporated into microchannels of a polymeric matrix of polydimethylsiloxane and through layer-bylayer self-assembly techniques onto silicon. The fabricated microchannels had cross-sectional dimensions ranging from tens to hundreds of micrometers in width and height. The experimental results for continuous-flow microreactors are reported for the conversion of urea to ammonia by urease enzyme. Urea conversions of >90% were observed.

Investigation of vinegar production using a novel shaken repeated batch culture system.

PubMed

Schlepütz, Tino; Büchs, Jochen

2013-01-01

Nowadays, bioprocesses are developed or optimized on small scale. Also, vinegar industry is motivated to reinvestigate the established repeated batch fermentation process. As yet, there is no small-scale culture system for optimizing fermentation conditions for repeated batch bioprocesses. Thus, the aim of this study is to propose a new shaken culture system for parallel repeated batch vinegar fermentation. A new operation mode - the flushing repeated batch - was developed. Parallel repeated batch vinegar production could be established in shaken overflow vessels in a completely automated operation with only one pump per vessel. This flushing repeated batch was first theoretically investigated and then empirically tested. The ethanol concentration was online monitored during repeated batch fermentation by semiconductor gas sensors. It was shown that the switch from one ethanol substrate quality to different ethanol substrate qualities resulted in prolonged lag phases and durations of the first batches. In the subsequent batches the length of the fermentations decreased considerably. This decrease in the respective lag phases indicates an adaptation of the acetic acid bacteria mixed culture to the specific ethanol substrate quality. Consequently, flushing repeated batch fermentations on small scale are valuable for screening fermentation conditions and, thereby, improving industrial-scale bioprocesses such as vinegar production in terms of process robustness, stability, and productivity. Copyright © 2013 American Institute of Chemical Engineers.

Micro-Raman Technology to Interrogate Two-Phase Extraction on a Microfluidic Device.

PubMed

Nelson, Gilbert L; Asmussen, Susan E; Lines, Amanda M; Casella, Amanda J; Bottenus, Danny R; Clark, Sue B; Bryan, Samuel A

2018-05-21

Microfluidic devices provide ideal environments to study solvent extraction. When droplets form and generate plug flow down the microfluidic channel, the device acts as a microreactor in which the kinetics of chemical reactions and interfacial transfer can be examined. Here, we present a methodology that combines chemometric analysis with online micro-Raman spectroscopy to monitor biphasic extractions within a microfluidic device. Among the many benefits of microreactors is the ability to maintain small sample volumes, which is especially important when studying solvent extraction in harsh environments, such as in separations related to the nuclear fuel cycle. In solvent extraction, the efficiency of the process depends on complex formation and rates of transfer in biphasic systems. Thus, it is important to understand the kinetic parameters in an extraction system to maintain a high efficiency and effectivity of the process. This monitoring provided concentration measurements in both organic and aqueous plugs as they were pumped through the microfluidic channel. The biphasic system studied was comprised of HNO 3 as the aqueous phase and 30% (v/v) tributyl phosphate in n-dodecane comprised the organic phase, which simulated the plutonium uranium reduction extraction (PUREX) process. Using pre-equilibrated solutions (post extraction), the validity of the technique and methodology is illustrated. Following this validation, solutions that were not equilibrated were examined and the kinetics of interfacial mass transfer within the biphasic system were established. Kinetic results of extraction were compared to kinetics already determined on a macro scale to prove the efficacy of the technique.

Immobilised enzyme microreactor for screening of multi-step bioconversions: characterisation of a de novo transketolase-ω-transaminase pathway to synthesise chiral amino alcohols.

PubMed

Matosevic, S; Lye, G J; Baganz, F

2011-09-20

Complex molecules are synthesised via a number of multi-step reactions in living cells. In this work, we describe the development of a continuous flow immobilized enzyme microreactor platform for use in evaluation of multi-step bioconversion pathways demonstrating a de novo transketolase/ω-transaminase-linked asymmetric amino alcohol synthesis. The prototype dual microreactor is based on the reversible attachment of His₆-tagged enzymes via Ni-NTA linkage to two surface derivatised capillaries connected in series. Kinetic parameters established for the model transketolase (TK)-catalysed conversion of lithium-hydroxypyruvate (Li-HPA) and glycolaldehyde (GA) to L-erythrulose using a continuous flow system with online monitoring of reaction output was in good agreement with kinetic parameters determined for TK in stop-flow mode. By coupling the transketolase catalysed chiral ketone forming reaction with the biocatalytic addition of an amine to the TK product using a transaminase (ω-TAm) it is possible to generate chiral amino alcohols from achiral starting compounds. We demonstrated this in a two-step configuration, where the TK reaction was followed by the ω-TAm-catalysed amination of L-erythrulose to synthesise 2-amino-1,3,4-butanetriol (ABT). Synthesis of the ABT product via the dual reaction and the on-line monitoring of each component provided a full profile of the de novo two-step bioconversion and demonstrated the utility of this microreactor system to provide in vitro multi-step pathway evaluation. Copyright © 2011 Elsevier B.V. All rights reserved.

A fast and sensitive method for evaluating nuclides migration characteristics in rock medium by using micro-channel reactor concept

NASA Astrophysics Data System (ADS)

Okuyama, Keita; Sasahira, Akira; Noshita, Kenji; Yoshida, Takuma; Kato, Kazuyuki; Nagasaki, Shinya; Ohe, Toshiaki

Experimental effort to evaluate the barrier performance of geologic disposal requires relatively long testing periods and chemically stable conditions. We have developed a new technique, the micro mock-up method, to present a fast and sensitive method to measure both nuclide diffusivity and sorption coefficient within a day to overcome such disadvantage of the conventional method. In this method, a Teflon plate having a micro channel (10-200 μm depth, 2, 4 mm width) is placed just beneath the rock sample plate, radionuclide solution is injected into the channel with constant rate. The breakthrough curve is being measured until a steady state. The outlet flux in the steady state however does not meet the inlet flux because of the matrix diffusion into the rock body. This inlet-outlet difference is simply related to the effective diffusion coefficient ( De) and the distribution coefficient ( Kd) of rock sample. Then, we adopt a fitting procedure to speculate Kd and De values by comparing the observation to the theoretical curve of the two-dimensional diffusion-advection equation. In the present study, we measured De of 3H by using both the micro mock-up method and the conventional through-diffusion method for comparison. The obtained values of De by two different ways for granite sample (Inada area of Japan) were identical: 1.0 × 10 -11 and 9.0 × 10 -12 m 2/s but the testing period was much different: 10 h and 3 days, respectively. We also measured the breakthrough curve of 85Sr and the resulting Kd and De agreed well to the previous study obtained by the batch sorption experiments with crushed samples. The experimental evidence and the above advantages reveal that the micro mock-up method based on the microreactor concept is powerful and much advantageous when compared to the conventional method.

Development of ultrasonically levitated drops as microreactors for study of enzyme kinetics and potential as a universal portable analysis system

NASA Astrophysics Data System (ADS)

Scheeline, A.; Pierre, Z.; Field, C. R.; Ginsberg, M. D.

2009-05-01

Development of microfluidics has focused on carrying out chemical synthesis and analysis in ever-smaller volumes of solution. In most cases, flow systems are made of either quartz, glass, or an easily moldable polymer such as polydimethylsiloxane (Whitesides 2006). As the system shrinks, the ratio of surface area to volume increases. For studies of either free radical chemistry or protein chemistry, this is undesirable. Proteins stick to surfaces, biofilms grow on surfaces, and radicals annihilate on walls (Lewis et al. 2006). Thus, under those circumstances where small amounts of reactants must be employed, typical microfluidic systems are incompatible with the chemistry one wishes to study. We have developed an alternative approach. We use ultrasonically levitated microliter drops as well mixed microreactors. Depending on whether capillaries (to form the drop) and electrochemical sensors are in contact with the drop or whether there are no contacting solids, the ratio of solid surface area to volume is low or zero. The only interface seen by reactants is a liquid/air interface (or, more generally, liquid/gas, as any gas may be used to support the drop). While drop levitation has been reported since at least the 1940's, we are the second group to carry out enzyme reactions in levitated drops, (Weis; Nardozzi 2005) and have fabricated the lowest power levitator in the literature (Field; Scheeline 2007). The low consumption aspects of ordinary microfluidics combine with a contact-free determination cell (the levitated drop) that ensures against cross-contamination, minimizes the likelihood of biofilm formation, and is robust to changes in temperature and humidity (Lide 1992). We report kinetics measurements in levitated drops and explain how outgrowths of these accomplishments will lead to portable chemistry/biology laboratories well suited to detection of a wide range of chemical and biological agents in the asymmetric battlefield environment.

Enhanced lifetime for thin-dielectric microdischarge-arrays operating in DC

NASA Astrophysics Data System (ADS)

Dussart, Remi; Felix, Valentin; Overzet, Lawrence; Aubry, Olivier; Stolz, Arnaud; Lefaucheux, Philippe; Gremi-Univ Orleans-Cnrs Collaboration; University Of Texas At Dallas Collaboration

2016-09-01

Micro-hollow cathode discharge arrays using silicon as the cathode have a very limited lifetime because the silicon bubbles and initiates micro-arcing. To avoid this destructive behavior, the same configuration was kept but, another material was selected for the cathode. Using micro and nanotechnologies ordinarily used in microelectronic and MEMS device fabrication, we made arrays of cathode boundary layer (CBL)-type microreactors consisting of nickel electrodes separated by a 6 µm thick SiO2 layer. Microdischarges were ignited in arrays of 100 µm diameter holes at different pressures (200750 Torr) in different gases. Electrical and optical measurements were made to characterize the arrays. Unlike the microdischarges produced using silicon cathodes, the Ni cathode discharges remain very stable with essentially no micro-arcing. DC currents between 50 and 900 µA flowed through each microreactor with a discharge voltage of typically 200 V. Stable V-I characteristics showing both the normal and abnormal regimes were observed and are consistent with the spread of the plasma over the cathode area. Due to their stability and lifetime, new applications of these DC, CBL-type microreactors can now be envisaged.

Immobilization of peroxidase enzyme onto the porous silicon structure for enhancing its activity and stability

NASA Astrophysics Data System (ADS)

Sahare, Padmavati; Ayala, Marcela; Vazquez-Duhalt, Rafael; Agrawal, Vivechana

2014-08-01

In this work, a commercial peroxidase was immobilized onto porous silicon (PS) support functionalized with 3-aminopropyldiethoxysilane (APDES) and the performance of the obtained catalytic microreactor was studied. The immobilization steps were monitored and the activity of the immobilized enzyme in the PS pores was spectrophotometrically determined. The enzyme immobilization in porous silicon has demonstrated its potential as highly efficient enzymatic reactor. The effect of a polar organic solvent (acetonitrile) and the temperature (up to 50°C) on the activity and stability of the biocatalytic microreactor were studied. After 2-h incubation in organic solvent, the microreactor retained 80% of its initial activity in contrast to the system with free soluble peroxidase that lost 95% of its activity in the same period of time. Peroxidase immobilized into the spaces of the porous silicon support would be perspective for applications in treatments for environmental security such as removal of leached dye in textile industry or in treatment of different industrial effluents. The system can be also applied in the field of biomedicine.

PTFE-based microreactor system for the continuous synthesis of full-visible-spectrum emitting cesium lead halide perovskite nanocrystals.

PubMed

Zhang, Chengxi; Luan, Weiling; Yin, Yuhang; Yang, Fuqian

2017-01-01

Colloidal perovskite nanocrystals comprised of all inorganic cesium lead halide (CsPbX 3 , X = Cl, Br, I or a mixture thereof) have potential as optical gain materials due to their high luminescence efficiency. In this work, cesium lead halide nanocrystals are continuously synthesized via a microreactor system consisting of poly(tetrafluoroethylene) (PTFE) capillaries. The synthesized nanocrystals possess excellent optical properties, including a full width at half maximum of 19-35 nm, high fluorescence quantum yield of 47.8-90.55%, and photoluminescence emission in the range of 450-700 nm. For the same precursor concentrations, the photoluminescence emission peak generally increases with increasing reaction temperature, revealing a controllable temperature effect on the photoluminescence characteristics of the synthesized nanocrystals. For quantum dots synthesized with a Br/I ratio of 1:3, a slight blue shift was observed for reaction temperatures greater than 100 °C. This PTFE-based microreactor system provides the unique capability of continuously synthesizing high-quality perovskite nanocrystals that emit over the full visible spectrum with applications ranging from displays and optoelectronic devices.

PTFE-based microreactor system for the continuous synthesis of full-visible-spectrum emitting cesium lead halide perovskite nanocrystals

PubMed Central

Zhang, Chengxi; Yin, Yuhang

2017-01-01

Colloidal perovskite nanocrystals comprised of all inorganic cesium lead halide (CsPbX3, X = Cl, Br, I or a mixture thereof) have potential as optical gain materials due to their high luminescence efficiency. In this work, cesium lead halide nanocrystals are continuously synthesized via a microreactor system consisting of poly(tetrafluoroethylene) (PTFE) capillaries. The synthesized nanocrystals possess excellent optical properties, including a full width at half maximum of 19–35 nm, high fluorescence quantum yield of 47.8–90.55%, and photoluminescence emission in the range of 450–700 nm. For the same precursor concentrations, the photoluminescence emission peak generally increases with increasing reaction temperature, revealing a controllable temperature effect on the photoluminescence characteristics of the synthesized nanocrystals. For quantum dots synthesized with a Br/I ratio of 1:3, a slight blue shift was observed for reaction temperatures greater than 100 °C. This PTFE-based microreactor system provides the unique capability of continuously synthesizing high-quality perovskite nanocrystals that emit over the full visible spectrum with applications ranging from displays and optoelectronic devices. PMID:29259867

LOSS OF ORGANIC CHEMICALS IN SOIL: PURE COMPOUND TREATABILITY STUDIES

EPA Science Inventory

Comprehensive screening data on the treatability of 32 organic chemicals in soil were developed. Of the evaluated chemicals, 22 were phenolic compounds. Aerobic batch laboratory microcosm experiments were conducted using two soils: an acidic clay soil with <1% organic matter and ...

Organic Chemical Attribution Signatures for the Sourcing of a Mustard Agent and Its Starting Materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fraga, Carlos G.; Bronk, Krys; Dockendorff, Brian P.

Chemical attribution signatures (CAS) are being investigated for the sourcing of chemical warfare (CW) agents and their starting materials that may be implicated in chemical attacks or CW proliferation. The work reported here demonstrates for the first time trace impurities produced during the synthesis of tris(2-chloroethyl)amine (HN3) that point to specific reagent stocks used in the synthesis of this CW agent. Thirty batches of HN3 were synthesized using different combinations of commercial stocks of triethanolamine (TEA), thionyl chloride, chloroform, and acetone. The HN3 batches and reagent stocks were then analyzed for impurities by gas chromatography/mass spectrometry. Reaction-produced impurities indicative ofmore » specific TEA and chloroform stocks were exclusively discovered in HN3 batches made with those reagent stocks. In addition, some reagent impurities were found in the HN3 batches that were presumably not altered during synthesis and believed to be indicative of reagent type regardless of stock. Supervised classification using partial least squares discriminant analysis (PLSDA) on the impurity profiles of chloroform samples from seven stocks resulted in an average classification error by cross-validation of 2.4%. A classification error of zero was obtained using the seven-stock PLSDA model on a validation set of samples from an arbitrarily selected chloroform stock. In a separate analysis, all samples from two of seven chloroform stocks that were purposely not modeled had their samples matched to a chloroform stock rather than assigned a “no class” classification.« less

In situ characterization of catalysts and membranes in a microchannel under high-temperature water gas shift reaction conditions

NASA Astrophysics Data System (ADS)

Cavusoglu, G.; Dallmann, F.; Lichtenberg, H.; Goldbach, A.; Dittmeyer, R.; Grunwaldt, J.-D.

2016-05-01

Microreactor technology with high heat transfer in combination with stable catalysts is a very attractive approach for reactions involving major heat effects such as methane steam reforming and to some extent, also the high temperature water gas shift (WGS) reaction. For this study Rh/ceria catalysts and an ultrathin hydrogen selective membrane were characterized in situ in a microreactor specially designed for x-ray absorption spectroscopic measurements under WGS conditions. The results of these experiments can serve as a basis for further development of the catalysts and membranes.

GCKP84-general chemical kinetics code for gas-phase flow and batch processes including heat transfer effects

NASA Technical Reports Server (NTRS)

Bittker, D. A.; Scullin, V. J.

1984-01-01

A general chemical kinetics code is described for complex, homogeneous ideal gas reactions in any chemical system. The main features of the GCKP84 code are flexibility, convenience, and speed of computation for many different reaction conditions. The code, which replaces the GCKP code published previously, solves numerically the differential equations for complex reaction in a batch system or one dimensional inviscid flow. It also solves numerically the nonlinear algebraic equations describing the well stirred reactor. A new state of the art numerical integration method is used for greatly increased speed in handling systems of stiff differential equations. The theory and the computer program, including details of input preparation and a guide to using the code are given.

A KINETIC MODEL FOR H2O2/UV PROCESS IN A COMPLETELY MIXED BATCH REACTOR. (R825370C076)

EPA Science Inventory

A dynamic kinetic model for the advanced oxidation process (AOP) using hydrogen peroxide and ultraviolet irradiation (H₂O₂/UV) in a completely mixed batch reactor (CMBR) is developed. The model includes the known elementary chemical and photochemical reac...

40 CFR Table 2 to Subpart Ffff of... - Emission Limits and Work Practice Standards for Batch Process Vents

Code of Federal Regulations, 2012 CFR

2012-07-01

... Pollutants: Miscellaneous Organic Chemical Manufacturing Pt. 63, Subpt. FFFF, Table 2 Table 2 to Subpart FFFF... Group 1 batch process vents a. Reduce collective uncontrolled organic HAP emissions from the sum of all... a flare); or Not applicable. b. Reduce collective uncontrolled organic HAP emissions from the sum of...

Manufacturing methods and applications of membranes in microfluidics.

PubMed

Chen, Xueye; Shen, Jienan; Hu, Zengliang; Huo, Xuyao

2016-12-01

Applications of membranes in microfluidics solved many thorny problems for analytical chemistry and bioscience, so that the use of membranes in microfluidics has been a topic of growing interest. Many different examples have been reported, demonstrating the versatile use of membranes. This work reviews a lot of applications of membranes in microfluidics. Membranes in microfluidics for applications including chemical reagents detection, gas detection, drug screening, cell, protein, microreactor, electrokinetical fluid, pump and valve and fluid transport control and so on, have been analyzed and discussed. In addition, the definition and basic concepts of membranes are summed up. And the methods of manufacturing membranes in microfluidics are discussed. This paper will provide a helpful reference to researchers who want to study applications of membranes in microfluidics.

Development of a chemically defined platform fed-batch culture media for monoclonal antibody-producing CHO cell lines with optimized choline content.

PubMed

Kuwae, Shinobu; Miyakawa, Ichiko; Doi, Tomohiro

2018-01-11

A chemically defined platform basal medium and feed media were developed using a single Chinese hamster ovary (CHO) cell line that produces a monoclonal antibody (mAb). Cell line A, which showed a peak viable cell density of 5.9 × 10 6  cells/mL and a final mAb titer of 0.5 g/L in batch culture, was selected for the platform media development. Stoichiometrically balanced feed media were developed using glucose as an indicator of cell metabolism to determine the feed rates of all other nutrients. A fed-batch culture of cell line A using the platform fed-batch medium yielded a 6.4 g/L mAb titer, which was 12-fold higher than that of the batch culture. To examine the applicability of the platform basal medium and feed media, three other cell lines (A16, B, and C) that produce mAbs were cultured using the platform fed-batch medium, and they yielded mAb titers of 8.4, 3.3, and 6.2 g/L, respectively. The peak viable cell densities of the three cell lines ranged from 1.3 × 10 7 to 1.8 × 10 7  cells/mL. These results show that the nutritionally balanced fed-batch medium and feeds worked well for other cell lines. During the medium development, we found that choline limitation caused a lower cell viability, a lower mAb titer, a higher mAb aggregate content, and a higher mannose-5 content. The optimal choline chloride to glucose ratio for the CHO cell fed-batch culture was determined. Our platform basal medium and feed media will shorten the medium-development time for mAb-producing cell lines.

[Identification of the authentic quality of Longdanxiegan pill by systematic quantified fingerprint method based on three wavelength fusion chromatogram].

PubMed

Sun, Guoxiang; Zhang, Jingxian

2009-05-01

The three wavelength fusion high performance liquid chromatographic fingerprin (TWFFP) of Longdanxiegan pill (LDXGP) was established to identify the quality of LDXGP by the systematic quantified fingerprint method. The chromatographic fingerprints (CFPs) of the 12 batches of LDXGP were determined by reversed-phase high performance liquid chromatography. The technique of multi-wavelength fusion fingerprint was applied during processing the fingerprints. The TWFFPs containing 63 co-possessing peaks were obtained when choosing baicalin peak as the referential peak. The 12 batches of LDXGP were identified with hierarchical clustering analysis by using macro qualitative similarity (S(m)) as the variable. According to the results of classification, the referential fingerprint (RFP) was synthesized from 10 batches of LDXGP. Taking the RFP for the qualified model, all the 12 batches of LDXGP were evaluated by the systematic quantified fingerprint method. Among the 12 batches of LDXGP, 9 batches were completely qualified, the contents of 1 batch were obviously higher while the chemical constituents quantity and distributed proportion in 2 batches were not qualified. The systematic quantified fingerprint method based on the technique of multi-wavelength fusion fingerprint ca effectively identify the authentic quality of traditional Chinese medicine.

Pyrolysis of the Simplest Carbohydrate, Glycolaldehyde (CHO-CH2OH), and Glyoxal in a Heated Microreactor.

PubMed

Porterfield, Jessica P; Baraban, Joshua H; Troy, Tyler P; Ahmed, Musahid; McCarthy, Michael C; Morgan, Kathleen M; Daily, John W; Nguyen, Thanh Lam; Stanton, John F; Ellison, G Barney

2016-04-14

Both glycolaldehyde and glyoxal were pyrolyzed in a set of flash-pyrolysis microreactors. The pyrolysis products resulting from CHO-CH2OH and HCO-CHO were detected and identified by vacuum ultraviolet (VUV) photoionization mass spectrometry. Complementary product identification was provided by argon matrix infrared absorption spectroscopy. Pyrolysis pressures in the microreactor were about 100 Torr, and contact times with the microreactors were roughly 100 μs. At 1200 K, the products of glycolaldehyde pyrolysis are H atoms, CO, CH2═O, CH2═C═O, and HCO-CHO. Thermal decomposition of HCO-CHO was studied with pulsed 118.2 nm photoionization mass spectrometry and matrix infrared absorption. Under these conditions, glyoxal undergoes pyrolysis to H atoms and CO. Tunable VUV photoionization mass spectrometry provides a lower bound for the ionization energy (IE)(CHO-CH2OH) ≥ 9.95 ± 0.05 eV. The gas-phase heat of formation of glycolaldehyde was established by a sequence of calorimetric experiments. The experimental result is ΔfH298(CHO-CH2OH) = -75.8 ± 1.3 kcal mol(-1). Fully ab initio, coupled cluster calculations predict ΔfH0(CHO-CH2OH) of -73.1 ± 0.5 kcal mol(-1) and ΔfH298(CHO-CH2OH) of -76.1 ± 0.5 kcal mol(-1). The coupled-cluster singles doubles and noniterative triples correction calculations also lead to a revision of the geometry of CHO-CH2OH. We find that the O-H bond length differs substantially from earlier experimental estimates, due to unusual zero-point contributions to the moments of inertia.

A multi-enzyme microreactor-based online electrochemical system for selective and continuous monitoring of acetylcholine.

PubMed

Lin, Yuqing; Yu, Ping; Mao, Lanqun

2015-06-07

This study demonstrates an online electrochemical system (OECS) for selective and continuous measurements of acetylcholine (ACh) through efficiently integrating in vivo microdialysis, a multi-enzyme microreactor and an electrochemical detector. A multi-enzyme microreactor was prepared first by co-immobilizing two kinds of enzymes, i.e. choline oxidase (ChOx) and catalase (Cat), onto magnetite nanoparticles and then confining the as-formed nanoparticles into a fused-silica capillary with the assistance of an external magnet. The multi-enzyme microreactor was settled between an in vivo microdialysis sampling system and an electrochemical detector to suppress the interference from choline toward ACh detection. Selective detection of ACh was accomplished using the electrochemical detector with ACh esterase (AChE) and ChOx as the recognition units for ACh and Prussian blue (PB) as the electrocatalyst for the reduction of hydrogen peroxide (H2O2). The current recorded with the OECS was linear with the concentration of ACh (I/nA = -3.90CACh/μM + 1.21, γ = 0.998) within a concentration range of 5 μM to 100 μM. The detection limit, based on a signal-to-noise ratio of 3, was calculated to be 1 μM. Interference investigation demonstrates that the OECS did not produce an observable current response toward physiological levels of common electroactive species, such as ascorbic acid (AA), dopamine (DA), 3,4-dihydroxyphenylacetic acid (DOPAC), and uric acid (UA). The high selectivity and the good linearity in combination with the high stability may enable the OECS developed here as a potential system for continuous monitoring of cerebral ACh release in some physiological and pathological processes.

Rapid characterization of chemical markers for discrimination of Moutan Cortex and its processed products by direct injection-based mass spectrometry profiling and metabolomic method.

PubMed

Li, Chao-Ran; Li, Meng-Ning; Yang, Hua; Li, Ping; Gao, Wen

2018-06-01

Processing of herbal medicines is a characteristic pharmaceutical technique in Traditional Chinese Medicine, which can reduce toxicity and side effect, improve the flavor and efficacy, and even change the pharmacological action entirely. It is significant and crucial to perform a method to find chemical markers for differentiating herbal medicines in different processed degrees. The aim of this study was to perform a rapid and reasonable method to discriminate Moutan Cortex and its processed products, and to reveal the characteristics of chemical components depend on chemical markers. Thirty batches of Moutan Cortex and its processed products, including 11 batches of Raw Moutan Cortex (RMC), 9 batches of Moutan Cortex Tostus (MCT) and 10 batches of Moutan Cortex Carbonisatus (MCC), were directly injected in electrospray ionization quadrupole time-of-flight mass spectrometry (ESI-QTOF MS) for rapid analysis in positive and negative mode. Without chromatographic separation, each run was completed within 3 min. The raw MS data were automatically extracted by background deduction and molecular feature (MF) extraction algorithm. In negative mode, a total of 452 MFs were obtained and then pretreated by data filtration and differential analysis. After that, the filtered 85 MFs were treated by principal component analysis (PCA) to reduce the dimensions. Subsequently, a partial least squares discrimination analysis (PLS-DA) model was constructed for differentiation and chemical markers detection of Moutan Cortex in different processed degrees. The positive mode data were treated as same as those in negative mode. RMC, MCT and MCC were successfully classified. Moreover, 14 and 3 chemical markers from negative and positive mode respectively, were screened by the combination of their relative peak areas and the parameter variable importance in the projection (VIP) values in PLS-DA model. The content changes of these chemical markers were employed in order to illustrate chemical changes of Moutan Cortex after processed. These results showed that the proposed method which combined non-targeted metabolomics analysis with multivariate statistics analysis is reasonable and effective. It could not only be applied to discriminate herbal medicines and their processing products, but also to reveal the characteristics of chemical components during processing. Copyright © 2018. Published by Elsevier GmbH.

Discrete-Event Simulation in Chemical Engineering.

ERIC Educational Resources Information Center

Schultheisz, Daniel; Sommerfeld, Jude T.

1988-01-01

Gives examples, descriptions, and uses for various types of simulation systems, including the Flowtran, Process, Aspen Plus, Design II, GPSS, Simula, and Simscript. Explains similarities in simulators, terminology, and a batch chemical process. Tables and diagrams are included. (RT)

Development of batch producible hot embossing 3D nanostructured surface-enhanced Raman scattering chip technology

NASA Astrophysics Data System (ADS)

Huang, Chu-Yu; Tsai, Ming-Shiuan

2017-09-01

The main purpose of this study is to develop a batch producible hot embossing 3D nanostructured surface-enhanced Raman chip technology for high sensitivity label-free plasticizer detection. This study utilizing the AAO self-assembled uniform nano-hemispherical array barrier layer as a template to create a durable nanostructured nickel mold. With the hot embossing technique and the durable nanostructured nickel mold, we are able to batch produce the 3D Nanostructured Surface-enhanced Raman Scattering Chip with consistent quality. In addition, because of our SERS chip can be fabricated by batch processing, the fabrication cost is low. Therefore, the developed method is very promising to be widespread and extensively used in rapid chemical and biomolecular detection applications.

Continuous synthesis of drug-loaded nanoparticles using microchannel emulsification and numerical modeling: effect of passive mixing

PubMed Central

Ortiz de Solorzano, Isabel; Uson, Laura; Larrea, Ane; Miana, Mario; Sebastian, Victor; Arruebo, Manuel

2016-01-01

By using interdigital microfluidic reactors, monodisperse poly(d,l lactic-co-glycolic acid) nanoparticles (NPs) can be produced in a continuous manner and at a large scale (~10 g/h). An optimized synthesis protocol was obtained by selecting the appropriated passive mixer and fluid flow conditions to produce monodisperse NPs. A reduced NP polydispersity was obtained when using the microfluidic platform compared with the one obtained with NPs produced in a conventional discontinuous batch reactor. Cyclosporin, an immunosuppressant drug, was used as a model to validate the efficiency of the microfluidic platform to produce drug-loaded monodisperse poly(d,l lactic-co-glycolic acid) NPs. The influence of the mixer geometries and temperatures were analyzed, and the experimental results were corroborated by using computational fluid dynamic three-dimensional simulations. Flow patterns, mixing times, and mixing efficiencies were calculated, and the model supported with experimental results. The progress of mixing in the interdigital mixer was quantified by using the volume fractions of the organic and aqueous phases used during the emulsification–evaporation process. The developed model and methods were applied to determine the required time for achieving a complete mixing in each microreactor at different fluid flow conditions, temperatures, and mixing rates. PMID:27524896

Continuous synthesis of drug-loaded nanoparticles using microchannel emulsification and numerical modeling: effect of passive mixing.

PubMed

Ortiz de Solorzano, Isabel; Uson, Laura; Larrea, Ane; Miana, Mario; Sebastian, Victor; Arruebo, Manuel

2016-01-01

By using interdigital microfluidic reactors, monodisperse poly(d,l lactic-co-glycolic acid) nanoparticles (NPs) can be produced in a continuous manner and at a large scale (~10 g/h). An optimized synthesis protocol was obtained by selecting the appropriated passive mixer and fluid flow conditions to produce monodisperse NPs. A reduced NP polydispersity was obtained when using the microfluidic platform compared with the one obtained with NPs produced in a conventional discontinuous batch reactor. Cyclosporin, an immunosuppressant drug, was used as a model to validate the efficiency of the microfluidic platform to produce drug-loaded monodisperse poly(d,l lactic-co-glycolic acid) NPs. The influence of the mixer geometries and temperatures were analyzed, and the experimental results were corroborated by using computational fluid dynamic three-dimensional simulations. Flow patterns, mixing times, and mixing efficiencies were calculated, and the model supported with experimental results. The progress of mixing in the interdigital mixer was quantified by using the volume fractions of the organic and aqueous phases used during the emulsification-evaporation process. The developed model and methods were applied to determine the required time for achieving a complete mixing in each microreactor at different fluid flow conditions, temperatures, and mixing rates.

Controlled and tunable polymer particles' production using a single microfluidic device

NASA Astrophysics Data System (ADS)

Amoyav, Benzion; Benny, Ofra

2018-04-01

Microfluidics technology offers a new platform to control liquids under flow in small volumes. The advantage of using small-scale reactions for droplet generation along with the capacity to control the preparation parameters, making microfluidic chips an attractive technology for optimizing encapsulation formulations. However, one of the drawback in this methodology is the ability to obtain a wide range of droplet sizes, from sub-micron to microns using a single chip design. In fact, typically, droplet chips are used for micron-dimension particles, while nanoparticles' synthesis requires complex chips design (i.e., microreactors and staggered herringbone micromixer). Here, we introduce the development of a highly tunable and controlled encapsulation technique, using two polymer compositions, for generating particles ranging from microns to nano-size using the same simple single microfluidic chip design. Poly(lactic-co-glycolic acid) (PLGA 50:50) or PLGA/polyethylene glycol polymeric particles were prepared with focused-flow chip, yielding monodisperse particle batches. We show that by varying flow rate, solvent, surfactant and polymer composition, we were able to optimize particles' size and decrease polydispersity index, using simple chip designs with no further related adjustments or costs. Utilizing this platform, which offers tight tuning of particle properties, could offer an important tool for formulation development and can potentially pave the way towards a better precision nanomedicine.

New Electronic Materials and CO2 Reduction.

DTIC Science & Technology

1988-02-02

REPORT DOCUMENTATION PAGE ! a ;t, C ’ SE -R .r N ’ D RE--R’tThVE "j f ’ .NUS UNCLASSIFIED APPROVED FOR PUBLIC RELEASE AD-A240 192 Lit R 11 II6 NOOO 14...by H12 have been carried out at 290C in a microreactor with a H2 /CO ration of 9/1. The catalysts studied were iron(III) oxide, iron(1I) diiron(1II...Methanation studies have been carried out at 290’C in a microreactor with a H 2 /CO ratio of 9/1. The catalysts studied were iron(III) oxide, iron(IT

Hydrogen production through aqueous-phase reforming of ethylene glycol in a washcoated microchannel.

PubMed

D'Angelo, M Fernanda Neira; Ordomsky, Vitaly; Paunovic, Violeta; van der Schaaf, John; Schouten, Jaap C; Nijhuis, T Alexander

2013-09-01

Aqueous-phase reforming (APR) of biocarbohydrates is conducted in a catalytically stable washcoated microreactor where multiphase hydrogen removal enhances hydrogen efficiency. Single microchannel experiments are conducted following a simplified model based on the microreactor concept. A coating method to deposit a Pt-based catalyst on the microchannel walls is selected and optimized. APR reactivity tests are performed by using ethylene glycol as the model compound. Optimum results are achieved with a static washcoating technique; a highly uniform and well adhered 5 μm layer is deposited on the walls of a 320 μm internal diameter (ID) microchannel in one single step. During APR of ethylene glycol, the catalyst layer exhibits high stability over 10 days after limited initial deactivation. The microchannel presents higher conversion and selectivity to hydrogen than a fixed-bed reactor. The benefits of using a microreactor for APR can be further enhanced by utilizing increased Pt loadings, higher reaction temperatures, and larger carbohydrates (e.g., glucose). The use of microtechnology for aqueous-phase reforming will allow for a great reduction in the reformer size, thus rendering it promising for distributed hydrogen production. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Advances in microreaction technology for portable fuel cell applications: Wall coating of thin catalytic films in microreactors

NASA Astrophysics Data System (ADS)

Bravo Bersano, Jaime Cristian

This research has focused on the need to coat microreactor systems composed of channels in the micron size range of 100 to 1000 mum. The experimental procedures and learning are outlined in terms of slurry and surface preparation requirements which are detailed in the experimental section. This system is motivated and applied to micro methanol steam reformers. Thus, a detailed discussion on the driving motivation is given in the introduction. The low temperatures required for steam-reforming of methanol ˜ 493°K (220°C) make it possible to utilize the reformate as a feed to the fuel cell anode. The group of catalysts that shows the highest activity for methanol steam reforming (SR) at low temperature has composition of CuO/ZnO/Al 2O3, which is also the catalyst used for methanol synthesis. Steam reforming of methanol is a highly endothermic process. Conventional reactor configurations, such as a packed bed reactor, operate in a heat transfer limited mode for this reaction. Using catalyst in packed bed form for portable devices is also not convenient due to high pressure drop and possible channeling of gases in addition to poor heat transfer. A wall-coated catalyst represents a superior geometry since it provides lower pressure drop and ease of manufacturing. Due to their small size, microreactors are especially suited for endothermic reactions whose reactivity depends on the rate of heat input. A brief review on microreaction technology is given with a comprehensive survey for catalyst integration into microreactors for catalytic heterogeneous gas phase reactions. The strength of this research is the model that was developed to coat the interior of micron sized capillaries with coats of CuO/ZnO/Al2O 3 slurries as thick as 25 mum in the dry state. The details of the model are given in terms Taylor's theory and Rayleigh's theory. A model is presented that can predict the coat thickness based on experimental conditions The model combines Taylor's experimental work with Lord Rayleigh's instability theory for annular coatings. The model presented serves as a design tool for microreactor design. The model can also estimate the maximum coat thickness possible for a given system. The results are presented in graphical format in the Microchannel Coating Model chapter.

Oxidation and adduct formation of xenobiotics in a microfluidic electrochemical cell with boron doped diamond electrodes and an integrated passive gradient rotation mixer.

PubMed

van den Brink, Floris T G; Wigger, Tina; Ma, Liwei; Odijk, Mathieu; Olthuis, Wouter; Karst, Uwe; van den Berg, Albert

2016-10-05

Reactive xenobiotic metabolites and their adduct formation with biomolecules such as proteins are important to study as they can be detrimental to human health. Here, we present a microfluidic electrochemical cell with integrated micromixer to study phase I and phase II metabolism as well as protein adduct formation of xenobiotics in a purely instrumental approach. The newly developed microfluidic device enables both the generation of reactive metabolites through electrochemical oxidation and subsequent adduct formation with biomolecules in a chemical microreactor. This allows us to study the detoxification of reactive species with glutathione and to predict potential toxicity of xenobiotics as a result of protein modification. Efficient mixing in microfluidic systems is a slow process due to the typically laminar flow conditions in shallow channels. Therefore, a passive gradient rotation micromixer has been designed that is capable of mixing liquids efficiently in a 790 pL volume within tens of milliseconds. The mixing principle relies on turning the concentration gradient that is initially established by bringing together two streams of liquid, to take advantage of the short diffusion distances in the shallow microchannels of thin-layer flow cells. The mixer is located immediately downstream of the working electrode of an electrochemical cell with integrated boron doped diamond electrodes. In conjunction with mass spectrometry, the two microreactors integrated in a single device provide a powerful tool to study the metabolism and toxicity of xenobiotics, which was demonstrated by the investigation of the model compound 1-hydroxypyrene.

Enhanced d-lactic acid production by recombinant Saccharomyces cerevisiae following optimization of the global metabolic pathway.

PubMed

Yamada, Ryosuke; Wakita, Kazuki; Mitsui, Ryosuke; Ogino, Hiroyasu

2017-09-01

Utilization of renewable feedstocks for the production of bio-based chemicals such as d-lactic acid by engineering metabolic pathways in the yeast Saccharomyces cerevisiae has recently become an attractive option. In this study, to realize efficient d-lactic acid production by S. cerevisiae, the expression of 12 glycolysis-related genes and the Leuconostoc mesenteroides d-LDH gene was optimized using a previously developed global metabolic engineering strategy, and repeated batch fermentation was carried out using the resultant strain YPH499/dPdA3-34/DLDH/1-18. Stable d-lactic acid production through 10 repeated batch fermentations was achieved using YPH499/dPdA3-34/DLDH/1-18. The average d-lactic acid production, productivity, and yield with 10 repeated batch fermentations were 60.3 g/L, 2.80 g/L/h, and 0.646, respectively. The present study is the first report of the application of a global metabolic engineering strategy for bio-based chemical production, and it shows the potential for efficient production of such chemicals by global metabolic engineering of the yeast S. cerevisiae. Biotechnol. Bioeng. 2017;114: 2075-2084. © 2017 Wiley Periodicals, Inc. © 2017 Wiley Periodicals, Inc.

A preliminary evaluation of a reusable digital sterilization indicator prototype.

PubMed

Puttaiah, R; Griggs, J; D'Onofrio, M

2014-09-01

Sterilization of critical and semicritical instruments used in patient care must undergo a terminal process of sterilization. Use of chemical and physical indicators are important in providing information on the sterilizer's performance during each cycle. Regular and periodic monitoring of sterilizers using biological indicators is necessary in periodically validating performance of sterilizers. Data loggers or independent digital parametric indicators are innovative devices that provide more information than various classes chemical indicators. In this study we evaluated a prototype of an independent digital parametric indicator's use in autoclaves. The purpose of this study was to evaluate the performance of an independent digital indicator/data logger prototype (DS1922F) that could be used for multiple cycles within an autoclave.MG Materials and methods: Three batches of the DS1922F (150 samples) were used in this study that was conducted in a series. The first batch was challenged with 300 sterilization cycles within an autoclave and the data loggers evaluated to study failures and the reason for failure, make corrections and improve the prototype design. After changes made based on studying the first batch, the second batch of the prototype (150 samples) were challenged once again with 300 sterilization cycles within an autoclave and failure studied again in further improvement of the prototype. The final batch (3rd batch) of the prototype (150 samples) was challenged again but with 600 cycles to see how long they would last. Kaplan-Meier survival analysis analyses of all three batches was conducted (α = 0.05) and failed samples qualitatively studied in understanding the variables involved in the failure of the prototype, and in improving quality. Each tested batch provided crucial information on device failure and helped in improvement of the prototype. Mean lifetime survival of the final batch (Batch 3) of prototype was 498 (480, 516) sterilization cycles in an autoclave. In this study, the final batch of the DS1922F prototype data logger was found to be robust in withstanding the challenge of 600 autoclave cycles, with a mean lifetime of more than 450 cycles, multiple times more than prescribed number of cycles. Instrument reprocessing is among the important aspects of infection control. While stringent procedures are followed in instrument reprocessing within the clinic in assuring patient safety, regular use of sterilization process indicators and periodic biological validation of the sterilizer's performance is necessary. Chemical indicators for use in Autoclaves provide information on whether the particular cycle's parameters were achieved but do not provide at what specific point in time or temperature the failure occurred. Data loggers and associated reader software as the tested prototype in this evaluation (DS1922F), are designed to provide continuous information on time and temperature of the prescribed cycle. Data loggers provide immediate information on the process as opposed to Biological Indicators that take from days to a week in obtaining a confirmatory result. Further, many countries do not have the sterilization monitoring service infrastructure to meet the demands of the end users. In the absence of sterilization monitoring services, use of digital data loggers for each sterilization cycle is more pragmatic.

An approach to optimize the batch mixing process for improving the quality consistency of the products made from traditional Chinese medicines*

PubMed Central

Yan, Bin-jun; Qu, Hai-bin

2013-01-01

The efficacy of traditional Chinese medicine (TCM) is based on the combined effects of its constituents. Variation in chemical composition between batches of TCM has always been the deterring factor in achieving consistency in efficacy. The batch mixing process can significantly reduce the batch-to-batch quality variation in TCM extracts by mixing them in a well-designed proportion. However, reducing the quality variation without sacrificing too much of the production efficiency is one of the challenges. Accordingly, an innovative and practical batch mixing method aimed at providing acceptable efficiency for industrial production of TCM products is proposed in this work, which uses a minimum number of batches of extracts to meet the content limits. The important factors affecting the utilization ratio of the extracts (URE) were studied by simulations. The results have shown that URE was affected by the correlation between the contents of constituents, and URE decreased with the increase in the number of targets and the relative standard deviations of the contents. URE could be increased by increasing the number of storage tanks. The results have provided a reference for designing the batch mixing process. The proposed method has possible application value in reducing the quality variation in TCM and providing acceptable production efficiency simultaneously. PMID:24190450

An approach to optimize the batch mixing process for improving the quality consistency of the products made from traditional Chinese medicines.

PubMed

Yan, Bin-jun; Qu, Hai-bin

2013-11-01

The efficacy of traditional Chinese medicine (TCM) is based on the combined effects of its constituents. Variation in chemical composition between batches of TCM has always been the deterring factor in achieving consistency in efficacy. The batch mixing process can significantly reduce the batch-to-batch quality variation in TCM extracts by mixing them in a well-designed proportion. However, reducing the quality variation without sacrificing too much of the production efficiency is one of the challenges. Accordingly, an innovative and practical batch mixing method aimed at providing acceptable efficiency for industrial production of TCM products is proposed in this work, which uses a minimum number of batches of extracts to meet the content limits. The important factors affecting the utilization ratio of the extracts (URE) were studied by simulations. The results have shown that URE was affected by the correlation between the contents of constituents, and URE decreased with the increase in the number of targets and the relative standard deviations of the contents. URE could be increased by increasing the number of storage tanks. The results have provided a reference for designing the batch mixing process. The proposed method has possible application value in reducing the quality variation in TCM and providing acceptable production efficiency simultaneously.

40 CFR 52.777 - Control strategy: photochemical oxidants (hydrocarbons).

Code of Federal Regulations, 2013 CFR

2013-07-01

... lithography operations, business plastics, automotive plastics, and synthetic organic chemical manufacturing..., automotive plastics, and synthetic organic chemical manufacturing industries (SOCMI) batch processes... Michigan area, and an agreed order between U.S. Steel (currently USX Corporation) and the IDEM signed by...

40 CFR 52.777 - Control strategy: photochemical oxidants (hydrocarbons).

Code of Federal Regulations, 2012 CFR

2012-07-01

... lithography operations, business plastics, automotive plastics, and synthetic organic chemical manufacturing..., automotive plastics, and synthetic organic chemical manufacturing industries (SOCMI) batch processes... Michigan area, and an agreed order between U.S. Steel (currently USX Corporation) and the IDEM signed by...

Deoxygenation of waste cooking oil and non-edible oil for the production of liquid hydrocarbon biofuels.

PubMed

Romero, M J A; Pizzi, A; Toscano, G; Busca, G; Bosio, B; Arato, E

2016-01-01

Deoxygenation of waste cooking vegetable oil and Jatropha curcas oil under nitrogen atmosphere was performed in batch and semi-batch experiments using CaO and treated hydrotalcite (MG70) as catalysts at 400 °C. In batch conditions a single liquid fraction (with yields greater than 80 wt.%) was produced containing a high proportion of hydrocarbons (83%). In semi-batch conditions two liquid fractions (separated by a distillation step) were obtained: a light fraction and an intermediate fraction containing amounts of hydrocarbons between 72-80% and 85-88% respectively. In order to assess the possible use of the liquid products as alternative fuels a complete chemical characterization and measurement of their properties were carried out. Copyright © 2015 Elsevier Ltd. All rights reserved.

High Solid Fed-batch Butanol Fermentation with Simultaneous Product Recovery: Part II - Process Integration.

PubMed

Qureshi, Nasib; Klasson, K Thomas; Saha, Badal C; Liu, Siqing

2018-04-25

In these studies liquid hot water (LHW) pretreated and enzymatically hydrolyzed Sweet Sorghum Bagasse (SSB) hydrolyzates were fermented in a fed-batch reactor. As reported in the preceding paper, the culture was not able to ferment the hydrolyzate I in a batch process due to presence of high level of toxic chemicals, in particular acetic acid released from SSB during the hydrolytic process. To be able to ferment the hydrolyzate I obtained from 250 gL -1 SSB hydrolysis, a fed-batch reactor with in-situ butanol recovery was devised. The process was started with the hydrolyzate II and when good cell growth and vigorous fermentation were observed, the hydrolyzate I was slowly fed to the reactor. In this manner the culture was able to ferment all the sugars present in both the hydrolyzates to acetone butanol ethanol (ABE). In a control batch reactor in which ABE was produced from glucose, ABE productivity and yield of 0.42 gL -1 h -1 and 0.36 were obtained, respectively. In the fed-batch reactor fed with SSB hydrolyzates these productivity and yield values were 0.44 gL -1 h -1 and 0.45, respectively. ABE yield in the integrated system was high due to utilization of acetic acid to convert to ABE. In summary we were able to utilize both the hydrolyzates obtained from LHW pretreated and enzymatically hydrolyzed SSB (250 gL -1 ) and convert them to ABE. Complete fermentation was possible due to simultaneous recovery of ABE by vacuum. This article is protected by copyright. All rights reserved. © 2018 American Institute of Chemical Engineers.

Characterization of the SRNL-Washed tank 51 sludge batch 9 qualification sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pareizs, J. M.

2016-01-01

Savannah River National Laboratory (SRNL) personnel have been requested to qualify the next sludge batch (Sludge Batch 9 – SB9) for processing at the Defense Waste Processing Facility (DWPF). To accomplish this task, Savannah River Remediation (SRR) sent SRNL a 3-L sample of Tank 51H slurry to be characterized, washed, and then used in a lab-scale demonstration of the DWPF flowsheet (after combining with Tank 40H sludge). SRNL has washed the Tank 51H sample per the Tank Farm washing strategy as of October 20, 2015. A part of the qualification process is extensive radionuclide and chemical characterization of the SRNL-washedmore » Tank 51H slurry. This report documents the chemical characterization of the washed slurry; radiological characterization is in progress and will be documented in a separate report. The analytical results of this characterization are comparable to the Tank Farm projections. Therefore, it is recommended that SRNL use this washed slurry for the ongoing SB9 qualification activities.« less

[Correlation of HPLC Characteristic Spectra of Vinegar Corydalis Rhizoma Decoction Pieces, Water Decoction and Formula Granules].

PubMed

Wei, Mei; Du, Lan-zhe; Li, Hui; Zhang, Guang-da; Chen, Xiang-dong

2015-05-01

To study the correlation of characteristic spectra of Vinegar Corydalis Rhizoma decoction pieces, water decoction and formula granules by HPLC, and to investigate the transfer of the main chemical constituents between three different forms. The analysis was carried out by a Phenomenex Gemini C18 column (250 mm x 4.6 mm,5 μm) with acetonitrile-1% acetic acid and ammonium acetate buffer solution (pH 6.0) as the mobile phase in a gradient elution mode. The detection wavelength was 280 nm with a flow rate of 0.8 mL /min. The column temperature was 30 degrees C. The characteristic spectra from 11 batches of Vinegar Corydalis Rhizoma decoction pieces, 11 batches of water decoction and 11 batches of formula granules were established respectively. Ten peaks in the HPLC characteristic spectra from 11 batches of formula granules could be tracked in the water decoction, nine peaks in the HPLC characteristic spectra could be tracked in the decoction pieces. In the ten common peaks, four components such as protopine, palnatine chloride, berberine hydrochloride and tetrahydropalmatine were verified. The main chemical components of Vinegar Corydalis Rhizoma decoction pieces, water decoction and formula granules are basically the same, the common component contents have similar proportion.

Noninvasive detection of lung cancer using exhaled breath

PubMed Central

Fu, Xiao-An; Li, Mingxiao; Knipp, Ralph J; Nantz, Michael H; Bousamra, Michael

2014-01-01

Early detection of lung cancer is a key factor for increasing the survival rates of lung cancer patients. The analysis of exhaled breath is promising as a noninvasive diagnostic tool for diagnosis of lung cancer. We demonstrate the quantitative analysis of carbonyl volatile organic compounds (VOCs) and identification of lung cancer VOC markers in exhaled breath using unique silicon microreactor technology. The microreactor consists of thousands of micropillars coated with an ammonium aminooxy salt for capture of carbonyl VOCs in exhaled breath by means of oximation reactions. Captured aminooxy-VOC adducts are analyzed by nanoelectrospray Fourier transform-ion cyclotron resonance (FT-ICR) mass spectrometry (MS). The concentrations of 2-butanone, 2-hydroxyacetaldehyde, 3-hydroxy-2-butanone, and 4-hydroxyhexenal (4-HHE) in the exhaled breath of lung cancer patients (n = 97) were significantly higher than in the exhaled breath of healthy smoker and nonsmoker controls (n = 88) and patients with benign pulmonary nodules (n = 32). The concentration of 2-butanone in exhaled breath of patients (n = 51) with stages II though IV non–small cell lung cancer (NSCLC) was significantly higher than in exhaled breath of patients with stage I (n = 34). The carbonyl VOC profile in exhaled breath determined using this new silicon microreactor technology provides for the noninvasive detection of lung cancer. PMID:24402867

Highly efficient TiO2-based microreactor for photocatalytic applications.

PubMed

Krivec, Matic; Žagar, Kristina; Suhadolnik, Luka; Čeh, Miran; Dražić, Goran

2013-09-25

A photocatalytic, TiO2-based microreactor is designed and fabricated on a metal-titanium foil. The microchannel is mechanically engraved in the substrate foil, and a double-layered TiO2 anatase film is immobilized on its inner walls with a two-step synthesis, which included anodization and a hydrothermal treatment. X-ray diffraction (XRD) and scanning electron microscopy (SEM) confirm the presence of an approximately 10-μm-thick layer of titania nanotubes and anatase nanoparticles. The SEM and transmission electron microscopy (TEM) of the cross sections show a dense interface between the titanium substrate and the TiO2 nanotubes. An additional layer of TiO2-anatase nanoparticles on the top of the film provides a large, photocatalytic surface area. The metal-titanium substrate with a functionalized serpentine channel is sealed with UV-transparent Plexiglas, and four 0.8-mW UV LEDs combined with a power controller on a small printed-circuit board are fixed over the substrate. The photocatalytic activity and the kinetic properties for the degradation of caffeine are provided, and the longer-term stability of the TiO2 film is evaluated. The results show that after 6 months of use and 3600 working cycles the microreactor still exhibits 60% of its initial efficiency.

Microfluidic reactors for visible-light photocatalytic water purification assisted with thermolysis

PubMed Central

Wang, Ning; Tan, Furui; Wan, Li; Wu, Mengchun

2014-01-01

Photocatalytic water purification using visible light is under intense research in the hope to use sunlight efficiently, but the conventional bulk reactors are slow and complicated. This paper presents an integrated microfluidic planar reactor for visible-light photocatalysis with the merits of fine flow control, short reaction time, small sample volume, and long photocatalyst durability. One additional feature is that it enables one to use both the light and the heat energy of the light source simultaneously. The reactor consists of a BiVO4-coated glass as the substrate, a blank glass slide as the cover, and a UV-curable adhesive layer as the spacer and sealant. A blue light emitting diode panel (footprint 10 mm × 10 mm) is mounted on the microreactor to provide uniform irradiation over the whole reactor chamber, ensuring optimal utilization of the photons and easy adjustments of the light intensity and the reaction temperature. This microreactor may provide a versatile platform for studying the photocatalysis under combined conditions such as different temperatures, different light intensities, and different flow rates. Moreover, the microreactor demonstrates significant photodegradation with a reaction time of about 10 s, much shorter than typically a few hours using the bulk reactors, showing its potential as a rapid kit for characterization of photocatalyst performance. PMID:25584117

Preparation of a dual-enzyme co-immobilized capillary microreactor and simultaneous screening of multiple enzyme inhibitors by capillary electrophoresis.

PubMed

Lin, Pingtan; Zhao, Shulin; Lu, Xin; Ye, Fanggui; Wang, Hengshan

2013-08-01

A CE method based on a dual-enzyme co-immobilized capillary microreactor was developed for the simultaneous screening of multiple enzyme inhibitors. The capillary microreactor was prepared by co-immobilizing adenosine deaminase and xanthine oxidase on the inner wall at the inlet end of the separation capillary. The enzymes were first immobilized on gold nanoparticles, and the functionalized gold nanoparticles were then assembled on the inner wall at the inlet end of the separation capillary treated with polyethyleneimine. With the developed CE method, the substrates and products were baseline separated within 3 min. The activity of the immobilized enzyme can be directly detected by measuring the peak height of the products. A statistical parameter Z' factor was recommended for evaluation of the accuracy of a drug screening system. In the present study, it was calculated to be larger than 0.5, implying a good accuracy. Finally, screening a small compound library containing two known enzyme inhibitors and 20 natural extracts by the proposed method was demonstrated. The known inhibitors were identified, and some natural extracts were found to be positive for two-enzyme inhibition by the present method. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Nearly 1000 Protein Identifications from 50 ng of Xenopus laevis Zygote Homogenate Using Online Sample Preparation on a Strong Cation Exchange Monolith Based Microreactor Coupled with Capillary Zone Electrophoresis.

PubMed

Zhang, Zhenbin; Sun, Liangliang; Zhu, Guijie; Cox, Olivia F; Huber, Paul W; Dovichi, Norman J

2016-01-05

A sulfonate-silica hybrid strong cation exchange monolith microreactor was synthesized and coupled to a linear polyacrylamide coated capillary for online sample preparation and capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) bottom-up proteomic analysis. The protein sample was loaded onto the microreactor in an acidic buffer. After online reduction, alkylation, and digestion with trypsin, the digests were eluted with 200 mM ammonium bicarbonate at pH 8.2 for CZE-MS/MS analysis using 1 M acetic acid as the background electrolyte. This combination of basic elution and acidic background electrolytes results in both sample stacking and formation of a dynamic pH junction. 369 protein groups and 1274 peptides were identified from 50 ng of Xenopus laevis zygote homogenate, which is comparable with an offline sample preparation method, but the time required for sample preparation was decreased from over 24 h to less than 40 min. Dramatically improved performance was produced by coupling the reactor to a longer separation capillary (∼100 cm) and a Q Exactive HF mass spectrometer. 975 protein groups and 3749 peptides were identified from 50 ng of Xenopus protein using the online sample preparation method.

A biofilm microreactor system for simultaneous electrochemical and nuclear magnetic resonance techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Renslow, Ryan S.; Babauta, Jerome T.; Majors, Paul D.

2014-03-01

In order to fully understand electrochemically active biofilms and the limitations to their scale-up in industrial biofilm reactors, a complete picture of the microenvironments inside the biofilm is needed. Nuclear magnetic resonance (NMR) techniques are ideally suited for the study of biofilms and for probing their microenvironments because these techniques allow for non-invasive interrogation and in situ monitoring with high resolution. By combining NMR with simultaneous electrochemical techniques, it is possible to sustain and study live electrochemically active biofilms. Here, we introduce a novel biofilm microreactor system that allows for simultaneous electrochemical and NMR techniques (EC-NMR) at the microscale. Microreactorsmore » were designed with custom radiofrequency resonator coils, which allowed for NMR measurements of biofilms growing on polarized gold electrodes. For an example application of this system, we grew Geobacter sulfurreducens biofilms. NMR was used to investigate growth media flow velocities, which were compared to simulated laminar flow, and electron donor concentrations inside the biofilms. We use Monte Carlo error analysis to estimate standard deviations of the electron donor concentration measurements within the biofilm. The EC-NMR biofilm microreactor system can ultimately be used to correlate extracellular electron transfer rates with metabolic reactions and explore extracellular electron transfer mechanisms.« less

Micro-reactors for characterization of nanostructure-based sensors.

PubMed

Savu, R; Silveira, J V; Flacker, A; Vaz, A R; Joanni, E; Pinto, A C; Gobbi, A L; Santos, T E A; Rotondaro, A L P; Moshkalev, S A

2012-05-01

Fabrication and testing of micro-reactors for the characterization of nanosensors is presented in this work. The reactors have a small volume (100 μl) and are equipped with gas input/output channels. They were machined from a single piece of kovar in order to avoid leaks in the system due to additional welding. The contact pins were electrically insulated from the body of the reactor using a borosilicate sealing glass and the reactor was hermetically sealed using a lid and an elastomeric o-ring. One of the advantages of the reactor lies in its simple assembly and ease of use with any vacuum/gas system, allowing the connection of more than one device. Moreover, the lid can be modified in order to fit a window for in situ optical characterization. In order to prove its versatility, carbon nanotube-based sensors were tested using this micro-reactor. The devices were fabricated by depositing carbon nanotubes over 1 μm thick gold electrodes patterned onto Si/SiO(2) substrates. The sensors were tested using oxygen and nitrogen atmospheres, in the pressure range between 10(-5) and 10(-1) mbar. The small chamber volume allowed the measurement of fast sensor characteristic times, with the sensors showing good sensitivity towards gas and pressure as well as high reproducibility.

Micro-reactors for characterization of nanostructure-based sensors

NASA Astrophysics Data System (ADS)

Savu, R.; Silveira, J. V.; Flacker, A.; Vaz, A. R.; Joanni, E.; Pinto, A. C.; Gobbi, A. L.; Santos, T. E. A.; Rotondaro, A. L. P.; Moshkalev, S. A.

2012-05-01

Fabrication and testing of micro-reactors for the characterization of nanosensors is presented in this work. The reactors have a small volume (100 μl) and are equipped with gas input/output channels. They were machined from a single piece of kovar in order to avoid leaks in the system due to additional welding. The contact pins were electrically insulated from the body of the reactor using a borosilicate sealing glass and the reactor was hermetically sealed using a lid and an elastomeric o-ring. One of the advantages of the reactor lies in its simple assembly and ease of use with any vacuum/gas system, allowing the connection of more than one device. Moreover, the lid can be modified in order to fit a window for in situ optical characterization. In order to prove its versatility, carbon nanotube-based sensors were tested using this micro-reactor. The devices were fabricated by depositing carbon nanotubes over 1 μm thick gold electrodes patterned onto Si/SiO2 substrates. The sensors were tested using oxygen and nitrogen atmospheres, in the pressure range between 10-5 and 10-1 mbar. The small chamber volume allowed the measurement of fast sensor characteristic times, with the sensors showing good sensitivity towards gas and pressure as well as high reproducibility.

Stimuli-Responsive Reagent System for Enabling Microfluidic Immunoassays with Biomarker Purification and Enrichment

PubMed Central

2015-01-01

Immunoassays have been translated into microfluidic device formats, but significant challenges relating to upstream sample processing still limit their applications. Here, stimuli-responsive polymer–antibody conjugates are utilized in a microfluidic immunoassay to enable rapid biomarker purification and enrichment as well as sensitive detection. The conjugates were constructed by covalently grafting poly(N-isopropylacrylamide) (PNIPAAm), a thermally responsive polymer, to the lysine residues of anti-prostate specific antigen (PSA) Immunoglobulin G (IgG) using carbodiimide chemistry via the polymer end-carboxylate. The antibody-PNIPAAm (capture) conjugates and antibody-alkaline phosphatase (detection) conjugates formed sandwich immunocomplexes via PSA binding in 50% human plasma. The complexes were loaded into a recirculating poly(dimethylsiloxane) microreactor, equipped with micropumps and transverse flow features, for subsequent separation, enrichment, and quantification. The immunocomplexes were captured by heating the solution to 39 °C, mixed over the transverse features for 2 min, and washed with warm buffer. In one approach, the assay utilized immunocomplex solution that was contained in an 80 nL microreactor, which was loaded with solution at room temperature and subsequently heated to 39 °C. The assay took 25 min and resulted in 37 pM PSA limit of detection (LOD), which is comparable to a plate ELISA employing the same antibody pair. In another approach, the microreactor was preheated to 39 °C, and immunocomplex solution was flowed through the reactor, mixed, and washed. When the specimen volume was increased to 7.5 μL by repeating the capture process three times, the higher specimen volume led to immunocomplex enrichment within the microreactor. The resulting assay LOD was 0.5 pM, which is 2 orders of magnitude lower than the plate ELISA. Both approaches generate antigen specific signal over a clinically significant range. The sample processing capabilities and subsequent utility in a biomarker assay demonstrate the opportunity for stimuli-responsive polymer–protein conjugates in novel diagnostic technologies. PMID:25405605

Synthesis and Manipulation of Semiconductor Nanocrystals inMicrofluidic Reactors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chan, Emory Ming-Yue

2006-01-01

Microfluidic reactors are investigated as a mechanism tocontrol the growth of semiconductor nanocrystals and characterize thestructural evolution of colloidal quantum dots. Due to their shortdiffusion lengths, low thermal masses, and predictable fluid dynamics,microfluidic devices can be used to quickly and reproducibly alterreaction conditions such as concentration, temperature, and reactiontime, while allowing for rapid reagent mixing and productcharacterization. These features are particularly useful for colloidalnanocrystal reactions, which scale poorly and are difficult to controland characterize in bulk fluids. To demonstrate the capabilities ofnanoparticle microreactors, a size series of spherical CdSe nanocrystalswas synthesized at high temperature in a continuous-flow, microfabricatedglass reactor. Nanocrystalmore » diameters are reproducibly controlled bysystematically altering reaction parameters such as the temperature,concentration, and reaction time. Microreactors with finer control overtemperature and reagent mixing were designed to synthesize nanoparticlesof different shapes, such as rods, tetrapods, and hollow shells. The twomajor challenges observed with continuous flow reactors are thedeposition of particles on channel walls and the broad distribution ofresidence times that result from laminar flow. To alleviate theseproblems, I designed and fabricated liquid-liquid segmented flowmicroreactors in which the reaction precursors are encapsulated inflowing droplets suspended in an immiscible carrier fluid. The synthesisof CdSe nanocrystals in such microreactors exhibited reduced depositionand residence time distributions while enabling the rapid screening aseries of samples isolated in nL droplets. Microfluidic reactors werealso designed to modify the composition of existing nanocrystals andcharacterize the kinetics of such reactions. The millisecond kinetics ofthe CdSe-to-Ag 2Se nanocrystal cation exchange reaction are measured insitu with micro-X-ray Absorption Spectroscopy in silicon microreactorsspecifically designed for rapid mixing and time-resolved X-rayspectroscopy. These results demonstrate that microreactors are valuablefor controlling and characterizing a wide range of reactions in nLvolumes even when nanoscale particles, high temperatures, causticreagents, and rapid time scales are involved. These experiments providethe foundation for future microfluidic investigations into the mechanismsof nanocrystal growth, crystal phase evolution, and heterostructureassembly.« less

Cyrano "Nose" The Smell of Success

NASA Technical Reports Server (NTRS)

2001-01-01

Cyrano Sciences, Inc. has commercialized a simple, accurate, non- invasive tool that enables "machines to smell". The Cyranose 320 is used for quality control purposes in the food and chemical industries. Using a sensor array and onboard pattern recognition algorithms, the lightweight, portable device works by exposing an array of polymer composite sensors to the chemical components in a vapor. When the sensors come in contact with the vapor, the polymer expands like a sponge, changing the resistance of the composites. The change in resistance is measured, and from that measurement, the presence of a pre-trained substance is determined with a quick and accurate diagnosis. This real-time, portable device enables food companies to spot test raw materials for batch-to-batch consistency, spoilage, or contamination. The Cyranose 320 is also used by chemical and petrochemical companies for quick assessment of the chemical status associated with various industrial processes. Profiling a chemical environment in a hazardous materials situation allows emergency crews to accurately select fire retardants, containment strategies, and protective gear. Future applications for the Cyranose 320 are fast growing and other uses of this technology are on the horizon.

Consumption and diffusion of dissolved oxygen in sedimentary rocks.

PubMed

Manaka, M; Takeda, M

2016-10-01

Fe(II)-bearing minerals (e.g., biotite, chlorite, and pyrite) are a promising reducing agent for the consumption of atmospheric oxygen in repositories for the geological disposal of high-level radioactive waste. To estimate effective diffusion coefficients (D e , in m 2 s -1 ) for dissolved oxygen (DO) and the reaction rates for the oxidation of Fe(II)-bearing minerals in a repository environment, we conducted diffusion-chemical reaction experiments using intact rock samples of Mizunami sedimentary rock. In addition, we conducted batch experiments on the oxidation of crushed sedimentary rock by DO in a closed system. From the results of the diffusion-chemical reaction experiments, we estimated the values of D e for DO to lie within the range 2.69×10 -11

Colorimetric sensor array for determination and identification of toxic industrial chemicals.

PubMed

Feng, Liang; Musto, Christopher J; Kemling, Jonathan W; Lim, Sung H; Zhong, Wenxuan; Suslick, Kenneth S

2010-11-15

A low-cost yet highly sensitive colorimetric sensor array for the detection and identification of toxic industrial chemicals (TICs) has been developed. The sensor consists of a disposable array of cross-responsive nanoporous pigments whose colors are changed by diverse chemical interactions with analytes. Clear differentiation among 20 different TICs has been easily achieved at both their IDLH (immediately dangerous to life or health) concentration within 2 min of exposure and PEL (permissible exposure limit) concentration within 5 min of exposure with no errors or misclassifications. Detection limits are generally well below the PEL (in most cases below 5% of PEL) and are typically in the low ppb range. The colorimetric sensor array is not responsive to changes in humidity or temperature over a substantial range. The printed arrays show excellent batch to batch reproducibility and long shelf life (greater than 3 months).

Ferrous Iron Oxidation by Thiobacillus ferrooxidans: Inhibition with Benzoic Acid, Sorbic Acid, and Sodium Lauryl Sulfate

PubMed Central

Onysko, Steven J.; Kleinmann, Robert L. P.; Erickson, Patricia M.

1984-01-01

Benzoic acid, sorbic acid, and sodium lauryl sulfate at low concentrations (5 to 10 mg/liter) each effectively inhibited bacterial oxidation of ferrous iron in batch cultures of Thiobacillus ferrooxidans. The rate of chemical oxidation of ferrous iron in low-pH, sterile batch reactors was not substantially affected at the tested concentrations (5 to 50 mg/liter) of any of the compounds. PMID:16346592

Highly sensitive silicon microreactor for catalyst testing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Henriksen, Toke R.; Hansen, Ole; Department of Physics, Danish National Research Foundation's Center for Individual Nanoparticle Functionality

2009-12-15

A novel microfabricated chemical reactor for highly sensitive measurements of catalytic activity and surface kinetics is presented. The reactor is fabricated in a silicon chip and is intended for gas-phase reactions at pressures ranging from 0.1 to 5.0 bar. A high sensitivity is obtained by directing the entire gas flow through the catalyst bed to a mass spectrometer, thus ensuring that nearly all reaction products are present in the analyzed gas flow. Although the device can be employed for testing a wide range of catalysts, the primary aim of the design is to allow characterization of model catalysts which canmore » only be obtained in small quantities. Such measurements are of significant fundamental interest but are challenging because of the low surface areas involved. The relationship between the reaction zone gas flow and the pressure in the reaction zone is investigated experimentally. A corresponding theoretical model is presented, and the gas flow through an on-chip flow-limiting capillary is predicted to be in the intermediate regime. The experimental data for the gas flow are found to be in good agreement with the theoretical model. At typical experimental conditions, the total gas flow through the reaction zone is around 3x10{sup 14} molecules s{sup -1}, corresponding to a gas residence time in the reaction zone of about 11 s. To demonstrate the operation of the microreactor, CO oxidation on low-area platinum thin film circles is employed as a test reaction. Using temperature ramping, it is found that platinum catalysts with areas as small as 15 {mu}m{sup 2} are conveniently characterized with the device.« less

Stabilization of Hydrogen Production via Methanol Steam Reforming in Microreactor by Al2O3 Nano-Film Enhanced Catalyst Adhesion.

PubMed

Jeong, Heondo; Na, Jeong-Geol; Jang, Min Su; Ko, Chang Hyun

2016-05-01

In hydrogen production by methanol steam reforming reaction with microchannel reactor, Al2O3 thin film formed by atomic layer deposition (ALD) was introduced on the surface of microchannel reactor prior to the coating of catalyst particles. Methanol conversion rate and hydrogen production rate, increased in the presence of Al2O3 thin film. Over-view and cross-sectional scanning electron microscopy study showed that the adhesion between catalyst particles and the surface of microchannel reactor enhanced due to the presence of Al2O3 thin film. The improvement of hydrogen production rate inside the channels of microreactor mainly came from the stable fixation of catalyst particles on the surface of microchannels.

Gas bubble formation and its pressure signature in T-junction of a microreactor

NASA Astrophysics Data System (ADS)

Pouya, Shahram; Koochesfahani, Manoochehr

2013-11-01

The segmented gas-liquid flow is of particular interest in microreactors used for high throughput material synthesis with enhanced mixing and more efficient reaction. A typical geometry to introduce gas plugs into the reactor is a T-junction where the dispersed liquid is squeezed and pinched by the continuous fluid in the main branch of the junction. We present experimental data of time resolved pressure along with synchronous imaging of the drop formation at the junction to show the transient behavior of the process. The stability of the slug regime and the regularity of the slug/plug pattern are investigated in this study. This work was supported by the CRC Program of the National Science Foundation, Grant Number CHE-0714028.

The influence of pH adjustment on kinetics parameters in tapioca wastewater treatment using aerobic sequencing batch reactor system

NASA Astrophysics Data System (ADS)

Mulyani, Happy; Budianto, Gregorius Prima Indra; Margono, Kaavessina, Mujtahid

2018-02-01

The present investigation deals with the aerobic sequencing batch reactor system of tapioca wastewater treatment with varying pH influent conditions. This project was carried out to evaluate the effect of pH on kinetics parameters of system. It was done by operating aerobic sequencing batch reactor system during 8 hours in many tapioca wastewater conditions (pH 4.91, pH 7, pH 8). The Chemical Oxygen Demand (COD) and Mixed Liquor Volatile Suspended Solids (MLVSS) of the aerobic sequencing batch reactor system effluent at steady state condition were determined at interval time of two hours to generate data for substrate inhibition kinetics parameters. Values of the kinetics constants were determined using Monod and Andrews models. There was no inhibition constant (Ki) detected in all process variation of aerobic sequencing batch reactor system for tapioca wastewater treatment in this study. Furthermore, pH 8 was selected as the preferred aerobic sequencing batch reactor system condition in those ranging pH investigated due to its achievement of values of kinetics parameters such µmax = 0.010457/hour and Ks = 255.0664 mg/L COD.

Nisin production of Lactococcus lactis N8 with hemin-stimulated cell respiration in fed-batch fermentation system.

PubMed

Kördikanlıoğlu, Burcu; Şimşek, Ömer; Saris, Per E J

2015-01-01

In this study, nisin production of Lactococcus lactis N8 was optimized by independent variables of glucose, hemin and oxygen concentrations in fed-batch fermentation in which respiration of cells was stimulated with hemin. Response surface model was able to explain the changes of the nisin production of L. lactis N8 in fed-batch fermentation system with high fidelity (R(2) 98%) and insignificant lack of fit. Accordingly, the equation developed indicated the optimum parameters for glucose, hemin, and dissolved oxygen were 8 g L(-1) h(-1) , 3 μg mL(-1) and 40%, respectively. While 1711 IU mL(-1) nisin was produced by L. lactis N8 in control fed-batch fermentation, 5410 IU mL(-1) nisin production was achieved within the relevant optimum parameters where the respiration of cell was stimulated with hemin. Accordingly, nisin production was enhanced 3.1 fold in fed-batch fermentation using hemin. In conclusion the nisin production of L. lactis N8 was enhanced extensively as a result of increasing the biomass by stimulating the cell respiration with adding the hemin in the fed-batch fermentation. © 2015 American Institute of Chemical Engineers.

Highly attrition-resistant zinc oxide-based sorbents for H{sub 2}S removal by spray-drying technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, J.B.; Baek, J.I.; Ryu, C.K.

2008-07-15

A ZnO-based sorbent, ZAC 32N, applicable to transport reactors was successfully prepared by the spray-drying technique. Another sorbent, ZAC 32SU, was prepared by scale-up preparation of ZAC 32N sorbent. The physical properties of the sorbents such as attrition resistance, specific surface area, pore volume, and particle size were extensively characterized and exhibited a good potential for use in transport applications. The chemical reactivity tested in the thermogravimetric analyzer and microreactor exhibited desirable characteristics for effective desulfurization of syngas streams in the range of 450-550{sup o}C. Bench-scale tests for the sorbent ZAC 32SU were performed for a continuous 160 h withmore » a steady solid circulation of 54.6 kg/h. The results showed 99.5%+ desulfurization at 500-550{sup o}C and reasonable regenerability at 550-620{sup o}C. Test results on the physical properties and chemical reactivity indicated that the performance of developed sorbents proved to be outstanding.« less

Microscale Interface Synthesis of Ni-B Amorphous Nanoparticles from NiSO4 by Sodium Borohydride Reduction in Microreactor

NASA Astrophysics Data System (ADS)

Xu, Lei; Peng, Jinhui; Meng, Binfang; Li, Wei; Liu, Bingguo; Luo, Huilong

2016-09-01

Amorphous nanoparticles have attracted a large amount of interest due to their superior catalytic activity and unique selectivity. The Ni-B amorphous nanoparticles were synthesized from aqueous reduction of NiSO4 by sodium borohydride in microscale interface at room temperature. The size, morphology, elemental compositions, and the chemical composition on the surface of Ni-B amorphous nanoparticles were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). All the results showed that the synthesized particles are Ni-B amorphous nanoparticles with uniform in size distribution and having good dispersion. The mean particle diameter of Ni-B amorphous nanoparticles was around 9 nm. The present work provides an alternative synthesis route for the Ni-B amorphous nanoparticles.

Rate and yield relationships in the production of xanthan gum by batch fermentations using complex and chemically defined growth media

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pinches, A.; Pallent, L.J.

1986-10-01

Rate and yield information relating to biomass and product formation and to nitrogen, glucose and oxygen consumption are described for xanthan gum batch fermentations in which both chemically defined (glutamate nitrogen) and complex (peptone nitrogen) media are employed. Simple growth and product models are used for data interpretation. For both nitrogen sources, rate and yield parameter estimates are shown to be independent of initial nitrogen concentrations. For stationary phases, specific rates of gum production are shown to be independent of nitrogen source but dependent on initial nitrogen concentration. The latter is modeled empirically and suggests caution in applying simple productmore » models to xanthan gum fermentations. 13 references.« less

[Determination of short chain chlorinated paraffins in polyvinyl chloride plastics by gas chromatography-negative chemical ion/mass spectrometry].

PubMed

Xing, Yuanna; Lin, Zhihui; Feng, Anhong; Wang, Xin; Gong, Yemeng; Chen, Zeyong

2015-02-01

A novel method was established to determine short chain chlorinated paraffins (SC-CPs) in polyvinyl chloride (PVC) plastics by gas chromatography-negative chemical ion/mass spectrometry (GC-NCI/MS). Ultrasonic extraction was used to extract SCCPs from PVC plastics. The optimal extraction time was 1.5 h, and concentrated sulfuric acid was adopted to purify the extracted solution. Finally, SCCPs in a sample were detected by GC-NCI/MS at 160 C and with methane reagent gas at 1. 5 mL/min. This method was not influenced by medium chain chlorinated paraffins (MCCPs) in the sample, and accurate quantitation was made for SCCPs. Twelve batches of samples were analyzed and SCCPs were detected in each batch with the contents from 0. 3 x 10(2)mg/kg to 3. 5 x 10(4)mg/kg. With respect to European limitation of SC-CPs (1%), four batches of samples did not comply with the European regulation, and they accounted for 33. 3%. Obviously, high SCCPs risk was presented in PVC plastics.

Acceptance Test Data for BWXT Coated Particle Batches 93172B and 93173B—Defective IPyC and Pyrocarbon Anisotropy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hunn, John D.; Helmreich, Grant W.; Dyer, John A.

Coated particle batches J52O-16-93172B and J52O-16-93173B were produced by Babcock and Wilcox Technologies (BWXT) as part of the production campaign for the Advanced Gas Reactor Fuel Development and Qualification (AGR) Program’s AGR-5/6/7 irradiation test in the Idaho National Laboratory (INL) Advanced Test Reactor (ATR), but were not used in the final fuel composite. However, these batches may be used as demonstration production-scale coated particle fuel for other experiments. Each batch was coated in a 150-mm-diameter production-scale fluidized-bed chemical vapor deposition (CVD) furnace. Tristructural isotropic (TRISO) coatings were deposited on 425-μm-nominal-diameter spherical kernels from BWXT lot J52R-16-69317 containing a mixture ofmore » 15.5%-enriched uranium carbide and uranium oxide (UCO). The TRISO coatings consisted of four consecutive CVD layers: a ~50% dense carbon buffer layer with 100-μm-nominal thickness, a dense inner pyrolytic carbon (IPyC) layer with 40-μm-nominal thickness, a silicon carbide (SiC) layer with 35-μm-nominal thickness, and a dense outer pyrolytic carbon (OPyC) layer with 40-μm-nominal thickness. The TRISO-coated particle batches were sieved to upgrade the particles by removing over-sized and under-sized material, and the upgraded batches were designated by appending the letter A to the end of the batch number (e.g., 93172A). Secondary upgrading by sieving was performed on the A-designated batches to remove particles with missing or very-thin buffer layers that were identified during previous analysis of the individual batches for defective IPyC, as reported in the acceptance test data report for the AGR-5/6/7 production batches [Hunn et al. 2017b]. The additionally-upgraded batches were designated by appending the letter B to the end of the batch number (e.g., 93172B).« less

Tailoring surface and photocatalytic properties of ZnO and nitrogen-doped ZnO nanostructures using microwave-assisted facile hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Rangel, R.; Cedeño, V.; Ramos-Corona, A.; Gutiérrez, R.; Alvarado-Gil, J. J.; Ares, O.; Bartolo-Pérez, P.; Quintana, P.

2017-08-01

Microwave hydrothermal synthesis, using an experimental 23 factorial design, was used to produce tunable ZnO nano- and microstructures, and their potential as photocatalysts was explored. Photocatalytic reactions were conducted in a microreactor batch system under UV and visible light irradiation, while monitoring methylene blue degradation, as a model system. The variables considered in the microwave reactor to produce ZnO nano- or microstructures, were time, NaOH concentration and synthesis temperature. It was found that, specific surface area and volume/surface area ratio were affected as a consequence of the synthesis conditions. In the second stage, the samples were plasma treated in a nitrogen atmosphere, with the purpose of introducing nitrogen into the ZnO crystalline structure. The central idea is to induce changes in the material structure as well as in its optical absorption, to make the plasma-treated material useful as photocatalyst in the visible region of the electromagnetic spectrum. Pristine ZnO and nitrogen-doped ZnO compounds were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), specific surface area (BET), XPS, and UV-Vis diffuse reflectance spectroscopy. The results show that the methodology presented in this work is effective in tailoring the specific surface area of the ZnO compounds and incorporation of nitrogen into their structure, factors which in turn, affect its photocatalytic behavior.

Review of electric discharge microplasmas generated in highly fluctuating fluids: Characteristics and application to nanomaterials synthesis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stauss, Sven, E-mail: sven.stauss@plasma.k.u-tokyo.ac.jp; Terashima, Kazuo, E-mail: kazuo@plasma.k.u-tokyo.ac.jp; Muneoka, Hitoshi

2015-05-15

Plasma-based fabrication of novel nanomaterials and nanostructures is indispensible for the development of next-generation electronic devices and for green energy applications. In particular, controlling the interactions between plasmas and materials interfaces, and the plasma fluctuations, is crucial for further development of plasma-based processes and bottom-up growth of nanomaterials. Electric discharge microplasmas generated in supercritical fluids represent a special class of high-pressure plasmas, where fluctuations on the molecular scale influence the discharge properties and the possible bottom-up growth of nanomaterials. This review discusses an anomaly observed for direct current microplasmas generated near the critical point, a local decrease in the breakdownmore » voltage. This anomalous behavior is suggested to be caused by the concomitant decrease of the ionization potential due to the formation of clusters near the critical point, and the formation of extended electron mean free paths caused by the high-density fluctuation near the critical point. It is also shown that in the case of dielectric barrier microdischarges generated close to the critical point, the high-density fluctuation of the supercritical fluid persists. The final part of the review discusses the application of discharges generated in supercritical fluids to synthesis of nanomaterials, in particular, molecular diamond—so-called diamondoids—by microplasmas generated inside conventional batch-type and continuous flow microreactors.« less

Continuous/Batch Mg/MgH2/H2O-Based Hydrogen Generator

NASA Technical Reports Server (NTRS)

Kindler, Andrew; Huang, Yuhong

2010-01-01

A proposed apparatus for generating hydrogen by means of chemical reactions of magnesium and magnesium hydride with steam would exploit the same basic principles as those discussed in the immediately preceding article, but would be designed to implement a hybrid continuous/batch mode of operation. The design concept would simplify the problem of optimizing thermal management and would help to minimize the size and weight necessary for generating a given amount of hydrogen.

Acceptance Test Data for Candidate AGR-5/6/7 TRISO Particle Batches BWXT Coater Batches 93165 93172 Defective IPyC Fraction and Pyrocarbon Anisotropy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Helmreich, Grant W.; Hunn, John D.; Skitt, Darren J.

2017-03-01

Coated particle fuel batches J52O-16-93165, 93166, 93168, 93169, 93170, and 93172 were produced by Babcock and Wilcox Technologies (BWXT) for possible selection as fuel for the Advanced Gas Reactor Fuel Development and Qualification (AGR) Program’s AGR-5/6/7 irradiation test in the Idaho National Laboratory (INL) Advanced Test Reactor (ATR). Some of these batches may alternately be used as demonstration coated particle fuel for other experiments. Each batch was coated in a 150-mm-diameter production-scale fluidized-bed chemical vapor deposition (CVD) furnace. Tristructural isotropic (TRISO) coatings were deposited on 425-μm-nominal-diameter spherical kernels from BWXT lot J52R-16-69317 containing a mixture of 15.5%-enriched uranium carbide andmore » uranium oxide (UCO). The TRISO coatings consisted of four consecutive CVD layers: a ~50% dense carbon buffer layer with 100-μm-nominal thickness, a dense inner pyrolytic carbon (IPyC) layer with 40-μm-nominal thickness, a silicon carbide (SiC) layer with 35-μm-nominal thickness, and a dense outer pyrolytic carbon (OPyC) layer with 40-μmnominal thickness. The TRISO-coated particle batches were sieved to upgrade the particles by removing over-sized and under-sized material, and the upgraded batches were designated by appending the letter A to the end of the batch number (e.g., 93165A).« less

Single-step enantioselective amino acid flux analysis by capillary electrophoresis using on-line sample preconcentration with chemical derivatization.

PubMed

Ptolemy, Adam S; Tran, Lara; Britz-McKibbin, Philip

2006-07-15

Capillary electrophoresis (CE) represents a versatile platform for integrating sample pretreatment with chemical analysis because of its ability to tune analyte electromigration and band dispersion properties in discontinuous electrolyte systems. In this article, a single-step method that combines on-line sample preconcentration with in-capillary chemical derivatization is developed for rapid, sensitive, and enantioselective analysis of micromolar levels of amino acids that lack intrinsic chromophores by CE with UV detection. Time-resolved electrophoretic studies revealed two distinct stages of amino acid band narrowing within the original long sample injection plug occurring both prior to and after in-capillary labeling via zone passing by ortho-phthalaldehyde/N-acetyl l-cysteine (OPA/NAC). This technique enabled direct analysis of d-amino acids in a 95% enantiomeric excess mixture with sub-micromolar detection limits and minimal sample handling, where the capillary functions as a preconcentrator, microreactor, and chiral selector. On-line sample preconcentration with chemical derivatization CE (SPCD-CE) was applied to study the enantioselective amino acid flux in Escherichia coli bacteria cultures, which demonstrated a unique l-Ala efflux into the extracellular medium. New strategies for high-throughput analyses of low-abundance metabolites are important for understanding fundamental physiological processes in bacteria required for screening the efficacy of new classes of antibiotics as well as altered metabolism in genetically modified mutant strains.

Nested potassium hydroxide etching and protective coatings for silicon-based microreactors

NASA Astrophysics Data System (ADS)

de Mas, Nuria; Schmidt, Martin A.; Jensen, Klavs F.

2014-03-01

We have developed a multilayer, multichannel silicon-based microreactor that uses elemental fluorine as a reagent and generates hydrogen fluoride as a byproduct. Nested potassium hydroxide etching (using silicon nitride and silicon oxide as masking materials) was developed to create a large number of channels (60 reaction channels connected to individual gas and liquid distributors) of significantly different depths (50-650 µm) with sloped walls (54.7° with respect to the (1 0 0) wafer surface) and precise control over their geometry. The wetted areas were coated with thermally grown silicon oxide and electron-beam evaporated nickel films to protect them from the corrosive fluorination environment. Up to four Pyrex layers were anodically bonded to three silicon layers in a total of six bonding steps to cap the microchannels and stack the reaction layers. The average pinhole density in as-evaporated films was 3 holes cm-2. Heating during anodic bonding (up to 350 °C for 4 min) did not significantly alter the film composition. Upon fluorine exposure, nickel films (160 nm thick) deposited on an adhesion layer of Cr (10 nm) over an oxidized silicon substrate (up to 500 nm thick SiO2) led to the formation of a nickel fluoride passivation layer. This microreactor was used to investigate direct fluorinations at room temperature over several hours without visible signs of film erosion.

A confined "microreactor" synthesis strategy to three dimensional nitrogen-doped graphene for high-performance sodium ion battery anodes

NASA Astrophysics Data System (ADS)

Li, Jiajie; Zhang, Yumin; Gao, Tangling; Han, Jiecai; Wang, Xianjie; Hultman, Benjamin; Xu, Ping; Zhang, Zhihua; Wu, Gang; Song, Bo

2018-02-01

In virtue of abundant sodium resources, sodium ion batteries (SIBs) have been regarded as one of the most promising alternatives for large-scale energy storage applications. However, the absence of a suitable anode material makes it difficult to realize these applications. Here, we demonstrate an effective synthesis strategy of using a "microreactor" consisting of melamine fiber (inside) and graphene oxide (GO, outside) to fabricate three dimensional (3D) nitrogen doped (N-doped) graphene as high-performance anode materials for sodium ion batteries. Through a controlled pyrolysis, the inside melamine fiber and the outside GO layer has been converted into N-doped graphene and reduced graphene oxide (r-GO) respectively, and thus the "microreactor" is transformed into interconnected 3D N-doped graphene structures. Such highly desired 3D graphene structures show reversible sodium storage capacities up to ∼305 mA h g-1 after 500 cycles at a current density of 0.2 A g-1 and promising long cycling stability with a stable capacity of ∼198 mA h g-1 at 5 A g-1 after 5000 cycles. The high capacity and superior durability in combination with the facile synthesis procedure of the 3D graphene structure make it a promising anode material for SIBs and other energy storage applications.

Modeling hexavalent chromium reduction in groundwater in field-scale transport and laboratory batch experiments

USGS Publications Warehouse

Friedly, J.C.; Davis, J.A.; Kent, D.B.

1995-01-01

A plausible and consistent model is developed to obtain a quantitative description of the gradual disappearance of hexavalent chromium (Cr(VI)) from groundwater in a small-scale field tracer test and in batch kinetic experiments using aquifer sediments under similar chemical conditions. The data exhibit three distinct timescales. Fast reduction occurs in well-stirred batch reactors in times much less than 1 hour and is followed by slow reduction over a timescale of the order of 2 days. In the field, reduction occurs on a timescale of the order of 8 days. The model is based on the following hypotheses. The chemical reduction reaction occurs very fast, and the longer timescales are caused by diffusion resistance. Diffusion into the secondary porosity of grains causes the apparent slow reduction rate in batch experiments. In the model of the field experiments, the reducing agent, heavy Fe(II)-bearing minerals, is heterogeneously distributed in thin strata located between larger nonreducing sand lenses that comprise the bulk of the aquifer solids. It is found that reducing strata of the order of centimeters thick are sufficient to contribute enough diffusion resistance to cause the observed longest timescale in the field. A one-dimensional advection/dispersion model is formulated that describes the major experimental trends. Diffusion rates are estimated in terms of an elementary physical picture of flow through a stratified medium containing identically sized spherical grains. Both reduction and sorption reactions are included. Batch simulation results are sensitive to the fraction of reductant located at or near the surface of grains, which controls the amount of rapid reduction, and the secondary porosity, which controls the rate of slow reduction observed in batch experiments. Results of Cr(VI) transport simulations are sensitive to the thickness and relative size of the reducing stratum. Transport simulation results suggest that nearly all of the reductant must be located in the reducing stratum. Within this context and as long as there is adequate reductive capacity present, the transport simulation results are insensitive to the parameters important for the batch simulations. The results illustrate how a combination of field measurements and batch laboratory studies can be used to improve predictive modeling of contaminant transport.

Flow chemistry using milli- and microstructured reactors-from conventional to novel process windows.

PubMed

Illg, Tobias; Löb, Patrick; Hessel, Volker

2010-06-01

The terminology Novel Process Window unites different methods to improve existing processes by applying unconventional and harsh process conditions like: process routes at much elevated pressure, much elevated temperature, or processing in a thermal runaway regime to achieve a significant impact on process performance. This paper is a review of parts of IMM's works in particular the applicability of above mentioned Novel Process Windows on selected chemical reactions. First, general characteristics of microreactors are discussed like excellent mass and heat transfer and improved mixing quality. Different types of reactions are presented in which the use of microstructured devices led to an increased process performance by applying Novel Process Windows. These examples were chosen to demonstrate how chemical reactions can benefit from the use of milli- and microstructured devices and how existing protocols can be changed toward process conditions hitherto not applicable in standard laboratory equipment. The used milli- and microstructured reactors can also offer advantages in other areas, for example, high-throughput screening of catalysts and better control of size distribution in a particle synthesis process by improved mixing, etc. The chemical industry is under continuous improvement. So, a lot of research is being done to synthesize high value chemicals, to optimize existing processes in view of process safety and energy consumption and to search for new routes to produce such chemicals. Leitmotifs of such undertakings are often sustainable development(1) and Green Chemistry(2).

Twin-Screw Extruders in Ceramic Extrusion

NASA Astrophysics Data System (ADS)

Wiedmann, Werner; Hölzel, Maria

The machines mainly used for compounding plastics, chemicals and food are co-rotating, closely intermeshing twin-screw extruders. Some 30 000 such extruders are in use worldwide, about 1/3 are ZSKs from Coperion Werner & Pfleiderer, Stuttgart. In the chemical industry more and more batch mixers are being replaced by continuous twin-screw kneaders.

Chemical profiling and quantitation of bioactive compounds in Platycladi Cacumen by UPLC-Q-TOF-MS/MS and UPLC-DAD.

PubMed

Zhuang, Bo; Bi, Zhi-Ming; Wang, Zi-Yuan; Duan, Li; Lai, Chang-Jiang-Sheng; Liu, E-Hu

2018-05-30

Platycladi Cacumen (PC) is a traditional Chinese medicine used for the treatment of hemorrhages, cough, asthma and hair loss. To get a better understanding of the chemical constituents in PC, ultra-high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS) and diagnostic ion filtering strategy were firstly employed for chemical profiling of PC. A total of 43 compounds including organic acids and derivatives, flavonoids as well as phenylpropanolds were unambiguously or reasonably identified. Coumarin and lignan were reported for the first time in PC. Chemical variation of 39 batches of PC from different geographical origins and 10 batches of processed product of PC was subsequently investigated by quantitation of nine major flavonoids. The results determined by UPLC coupled with diode array detection (UPLC-DAD) and hierarchical cluster analysis (HCA) indicated that the contents of flavonoids in PC samples differ greatly. This work provides an efficient approach to comprehensively evaluate the quality of PC. Copyright © 2018 Elsevier B.V. All rights reserved.

Size-controlled synthesis of ZnO quantum dots in microreactors

NASA Astrophysics Data System (ADS)

Schejn, Aleksandra; Frégnaux, Mathieu; Commenge, Jean-Marc; Balan, Lavinia; Falk, Laurent; Schneider, Raphaël

2014-04-01

In this paper, we report on a continuous-flow microreactor process to prepare ZnO quantum dots (QDs) with widely tunable particle size and photoluminescence emission wavelengths. X-ray diffraction, electron diffraction, UV-vis, photoluminescence and transmission electron microscopy measurements were used to characterize the synthesized ZnO QDs. By varying operating conditions (temperature, flow rate) or the capping ligand, ZnO QDs with diameters ranging from 3.6 to 5.2 nm and fluorescence maxima from 500 to 560 nm were prepared. Results obtained show that low reaction temperatures (20 or 35 °C), high flow rates and the use of propionic acid as a stabilizing agent are favorable for the production of ZnO QDs with high photoluminescence quantum yields (up to 30%).

Another expert system rule inference based on DNA molecule logic gates

NASA Astrophysics Data System (ADS)

WÄ siewicz, Piotr

2013-10-01

With the help of silicon industry microfluidic processors were invented utilizing nano membrane valves, pumps and microreactors. These so called lab-on-a-chips combined together with molecular computing create molecular-systems-ona- chips. This work presents a new approach to implementation of molecular inference systems. It requires the unique representation of signals by DNA molecules. The main part of this work includes the concept of logic gates based on typical genetic engineering reactions. The presented method allows for constructing logic gates with many inputs and for executing them at the same quantity of elementary operations, regardless of a number of input signals. Every microreactor of the lab-on-a-chip performs one unique operation on input molecules and can be connected by dataflow output-input connections to other ones.

Production of 2,3-butanediol by a low-acid producing Klebsiella oxytoca NBRF4.

PubMed

Han, Sung-Hyuk; Lee, Jung-Eun; Park, Kyungmoon; Park, Yong-Cheol

2013-01-25

2,3-Butanediol (2,3-BDO) is a value-added chemical with great potential for the industrial production of synthetic rubber, plastic and solvent. For microbial production of 2,3-BDO, in this study, Klebsiella oxytoca NBRF4 was constructed by chemical mutation and screening against NaBr, NaBrO(3) and fluoroacetate. Among metabolic enzymes involved in the production of lactate, acetate and 2,3-BDO, K. oxytoca NBRF4 possessed 1.2 times lower specific activities of lactate dehydrogenase and phosphotransacetylase, and 22% higher specific acetoin reductase activity than the K. oxytoca ATCC43863 control strain. A series of batch fermentations in a defined medium and application of a statistical tool of response surface method led to the determination of optimal culture conditions: 10% dissolved oxygen level, pH 4.3 and 38°C. The actual results of batch fermentation at the optimal conditions using 44 g/L glucose were coincident with the predetermined values: 14.4 g/L 2,3-BDO concentration, 0.32 g/g yield. To increase 2,3-BDO titer, fed-batch fermentation of K. oxytoca NBRF4 was performed by an intermittent feeding of 800 g/L glucose to control its concentration around 5-20 g/L in the culture broth. Finally, 34.2g/L 2,3-BDO concentration and 0.35 g/g yield were obtained without organic acid production in 70 hours of the fed-batch culture, which were 2.4 and 1.2 times higher than those of the batch fermentation using 44 g/L glucose. Copyright © 2012 Elsevier B.V. All rights reserved.

Continuous flow chemistry: a discovery tool for new chemical reactivity patterns.

PubMed

Hartwig, Jan; Metternich, Jan B; Nikbin, Nikzad; Kirschning, Andreas; Ley, Steven V

2014-06-14

Continuous flow chemistry as a process intensification tool is well known. However, its ability to enable chemists to perform reactions which are not possible in batch is less well studied or understood. Here we present an example, where a new reactivity pattern and extended reaction scope has been achieved by transferring a reaction from batch mode to flow. This new reactivity can be explained by suppressing back mixing and precise control of temperature in a flow reactor set up.

Isolation of friedelin from black condensate of cork.

PubMed

Pires, Ricardo A; Aroso, Ivo; Silva, Susana P; Mano, João F; Reis, Rui L

2011-11-01

Black condensates (BC) are wastes of the insulation corkboard industry that contain several valuable chemicals, including friedelin, a terpene exhibiting biological activity. Herein, we report a straightforward procedure to extract friedelin from BC. Using this procedure, we were able to extract friedelin with yields between 0.4% and 2.9% and to further purify it obtaining purities from 77.0% to 99.3% (HPLC). The initial BC (2 batches), extracted raw product and purified friedelin were analyzed using FTIR. The extraction yields and purities were found to be directly related to the intensity of the carbonyl vibration at 1713 cm(-1) in the FTIR spectrum of the used BC batch. Therefore, these spectra can be used to screen and select BC batches suitable for friedelin extraction.

Comparison of batch and column tests for the elution of artificial turf system components.

PubMed

Krüger, O; Kalbe, U; Berger, W; Nordhauβ, K; Christoph, G; Walzel, H-P

2012-12-18

Synthetic athletic tracks and turf areas for outdoor sporting grounds may release contaminants due to the chemical composition of some components. A primary example is that of zinc from reused scrap tires (main constituent, styrene butadiene rubber, SBR), which might be harmful to the environment. Thus, methods for the risk assessment of those materials are required. Laboratory leaching methods like batch and column tests are widely used to examine the soil-groundwater pathway. We tested several components for artificial sporting grounds with batch tests at a liquid to solid (LS) ratio of 2 L/kg and column tests with an LS up to 26.5 L/kg. We found a higher zinc release in the batch test eluates for all granules, ranging from 15% higher to 687% higher versus data from column tests for SBR granules. Accompanying parameters, especially the very high turbidity of one ethylene propylene diene monomer rubber (EPDM) or thermoplastic elastomer (TPE) eluates, reflect the stronger mechanical stress of batch testing. This indicates that batch test procedures might not be suitable for the risk assessment of synthetic sporting ground components. Column tests, on the other hand, represent field conditions more closely and allow for determination of time-dependent contaminants release.

Asymmetric reactions in continuous flow

PubMed Central

Mak, Xiao Yin; Laurino, Paola

2009-01-01

Summary An overview of asymmetric synthesis in continuous flow and microreactors is presented in this review. Applications of homogeneous and heterogeneous asymmetric catalysis as well as biocatalysis in flow are discussed. PMID:19478913

Design of two-column batch-to-batch recirculation to enhance performance in ion-exchange chromatography.

PubMed

Persson, Oliver; Andersson, Niklas; Nilsson, Bernt

2018-01-05

Preparative liquid chromatography is a separation technique widely used in the manufacturing of fine chemicals and pharmaceuticals. A major drawback of traditional single-column batch chromatography step is the trade-off between product purity and process performance. Recirculation of impure product can be utilized to make the trade-off more favorable. The aim of the present study was to investigate the usage of a two-column batch-to-batch recirculation process step to increase the performance compared to single-column batch chromatography at a high purity requirement. The separation of a ternary protein mixture on ion-exchange chromatography columns was used to evaluate the proposed process. The investigation used modelling and simulation of the process step, experimental validation and optimization of the simulated process. In the presented case the yield increases from 45.4% to 93.6% and the productivity increases 3.4 times compared to the performance of a batch run for a nominal case. A rapid concentration build-up product can be seen during the first cycles, before the process reaches a cyclic steady-state with reoccurring concentration profiles. The optimization of the simulation model predicts that the recirculated salt can be used as a flying start of the elution, which would enhance the process performance. The proposed process is more complex than a batch process, but may improve the separation performance, especially while operating at cyclic steady-state. The recirculation of impure fractions reduces the product losses and ensures separation of product to a high degree of purity. Copyright © 2017 Elsevier B.V. All rights reserved.

Architecture, Assembly, and Emerging Applications of Branched Functional Polyelectrolytes and Poly(ionic liquid)s.

PubMed

Xu, Weinan; Ledin, Petr A; Shevchenko, Valery V; Tsukruk, Vladimir V

2015-06-17

Branched polyelectrolytes with cylindrical brush, dendritic, hyperbranched, grafted, and star architectures bearing ionizable functional groups possess complex and unique assembly behavior in solution at surfaces and interfaces as compared to their linear counterparts. This review summarizes the recent developments in the introduction of various architectures and understanding of the assembly behavior of branched polyelectrolytes with a focus on functional polyelectrolytes and poly(ionic liquid)s with responsive properties. The branched polyelectrolytes and poly(ionic liquid)s interact electrostatically with small molecules, linear polyelectrolytes, or other branched polyelectrolytes to form assemblies of hybrid nanoparticles, multilayer thin films, responsive microcapsules, and ion-conductive membranes. The branched structures lead to unconventional assemblies and complex hierarchical structures with responsive properties as summarized in this review. Finally, we discuss prospectives for emerging applications of branched polyelectrolytes and poly(ionic liquid)s for energy harvesting and storage, controlled delivery, chemical microreactors, adaptive surfaces, and ion-exchange membranes.

Effect of water activity on rates of serpentinization of olivine.

PubMed

Lamadrid, Hector M; Rimstidt, J Donald; Schwarzenbach, Esther M; Klein, Frieder; Ulrich, Sarah; Dolocan, Andrei; Bodnar, Robert J

2017-07-14

The hydrothermal alteration of mantle rocks (referred to as serpentinization) occurs in submarine environments extending from mid-ocean ridges to subduction zones. Serpentinization affects the physical and chemical properties of oceanic lithosphere, represents one of the major mechanisms driving mass exchange between the mantle and the Earth's surface, and is central to current origin of life hypotheses as well as the search for microbial life on the icy moons of Jupiter and Saturn. In spite of increasing interest in the serpentinization process by researchers in diverse fields, the rates of serpentinization and the controlling factors are poorly understood. Here we use a novel in situ experimental method involving olivine micro-reactors and show that the rate of serpentinization is strongly controlled by the salinity (water activity) of the reacting fluid and demonstrate that the rate of serpentinization of olivine slows down as salinity increases and H 2 O activity decreases.

Effect of water activity on rates of serpentinization of olivine

NASA Astrophysics Data System (ADS)

Lamadrid, Hector M.; Rimstidt, J. Donald; Schwarzenbach, Esther M.; Klein, Frieder; Ulrich, Sarah; Dolocan, Andrei; Bodnar, Robert J.

2017-07-01

The hydrothermal alteration of mantle rocks (referred to as serpentinization) occurs in submarine environments extending from mid-ocean ridges to subduction zones. Serpentinization affects the physical and chemical properties of oceanic lithosphere, represents one of the major mechanisms driving mass exchange between the mantle and the Earth's surface, and is central to current origin of life hypotheses as well as the search for microbial life on the icy moons of Jupiter and Saturn. In spite of increasing interest in the serpentinization process by researchers in diverse fields, the rates of serpentinization and the controlling factors are poorly understood. Here we use a novel in situ experimental method involving olivine micro-reactors and show that the rate of serpentinization is strongly controlled by the salinity (water activity) of the reacting fluid and demonstrate that the rate of serpentinization of olivine slows down as salinity increases and H2O activity decreases.

Micro-view-cell for phase behaviour and in situ Raman analysis of heterogeneously catalysed CO2 hydrogenation

NASA Astrophysics Data System (ADS)

Reymond, Helena; Rudolf von Rohr, Philipp

2017-11-01

The operando study of CO2 hydrogenation is fundamental for a more rational optimisation of heterogeneous catalyst and reactor designs. To further complement the established efficiency of microreactors in reaction screening and bridge the operating and optical gaps, a micro-view-cell is presented for Raman microscopy at extreme conditions with minimum flow interference for genuine reaction analysis. Based on a flat sapphire window unit sealed in a plug flow-type enclosure holding the sample, the cell features unique 14 mm working distance and 0.36 numerical aperture and resists 400 °C and 500 bars. The use of the cell as an in situ tool for fast process monitoring and surface catalyst characterisation is demonstrated with phase behaviour and chemical analysis of the methanol synthesis over a commercial Cu/ZnO/Al2O3 catalyst.

The investigation of degradation reaction of various saccharides in high temperature and high pressure water

NASA Astrophysics Data System (ADS)

Saito, T.; Noguchi, S.; Matsumoto, T.; Sasaki, M.; Goto, M.

2008-07-01

Recently, conversions of polysaccharides included in biomass resources have been studied in order to recover valuable chemicals. Degradation of polysaccharides has been attracted by many researchers, whereas by-products from secondary reactions of the materials have not been studied very well. For the purpose of understanding reaction behavior of various monosaccharides in high-temperature and high-pressure water regions, we investigated reaction pathway and kinetics through reaction experiments of degradation of saccharides in subcritical water. The experiment was conducted by using continuous flow-type micro-reactors. Glucose was used as the starting material. From the experimental results, the conversion of glucose increased with increasing the residence time. The yields of fructose and 1, 6-anhydro-β-D-glucose decreased with increasing the residence time. The yields of organic acids and some aldehydes increased with increasing the residence time.

Abiotic ligation of DNA oligomers templated by their liquid crystal ordering

NASA Astrophysics Data System (ADS)

Fraccia, Tommaso P.; Smith, Gregory P.; Zanchetta, Giuliano; Paraboschi, Elvezia; Yi, Yougwooo; Walba, David M.; Dieci, Giorgio; Clark, Noel A.; Bellini, Tommaso

2015-03-01

It has been observed that concentrated solutions of short DNA oligomers develop liquid crystal ordering as the result of a hierarchically structured supramolecular self-assembly. In mixtures of oligomers with various degree of complementarity, liquid crystal microdomains are formed via the selective aggregation of those oligomers that have a sufficient degree of duplexing and propensity for physical polymerization. Here we show that such domains act as fluid and permeable microreactors in which the order-stabilized molecular contacts between duplex terminals serve as physical templates for their chemical ligation. In the presence of abiotic condensing agents, liquid crystal ordering markedly enhances ligation efficacy, thereby enhancing its own phase stability. The coupling between order-templated ligation and selectivity provided by supramolecular ordering enables an autocatalytic cycle favouring the growth of DNA chains, up to biologically relevant lengths, from few-base long oligomers. This finding suggests a novel scenario for the abiotic origin of nucleic acids.

Effect of water activity on rates of serpentinization of olivine

PubMed Central

Lamadrid, Hector M.; Rimstidt, J. Donald; Schwarzenbach, Esther M.; Klein, Frieder; Ulrich, Sarah; Dolocan, Andrei; Bodnar, Robert J.

2017-01-01

The hydrothermal alteration of mantle rocks (referred to as serpentinization) occurs in submarine environments extending from mid-ocean ridges to subduction zones. Serpentinization affects the physical and chemical properties of oceanic lithosphere, represents one of the major mechanisms driving mass exchange between the mantle and the Earth’s surface, and is central to current origin of life hypotheses as well as the search for microbial life on the icy moons of Jupiter and Saturn. In spite of increasing interest in the serpentinization process by researchers in diverse fields, the rates of serpentinization and the controlling factors are poorly understood. Here we use a novel in situ experimental method involving olivine micro-reactors and show that the rate of serpentinization is strongly controlled by the salinity (water activity) of the reacting fluid and demonstrate that the rate of serpentinization of olivine slows down as salinity increases and H2O activity decreases. PMID:28706268

40 CFR 1065.546 - Validation of minimum dilution ratio for PM batch sampling.

Code of Federal Regulations, 2012 CFR

2012-07-01

... chemical balance terms as given in § 1065.655(e). You may determine the raw exhaust flow rate based on the measured intake air and dilute exhaust molar flow rates and the dilute exhaust chemical balance terms as... air, fuel rate measurements, and fuel properties, consistent with good engineering judgment. (b...

40 CFR 1065.546 - Validation of minimum dilution ratio for PM batch sampling.

Code of Federal Regulations, 2013 CFR

2013-07-01

... chemical balance terms as given in § 1065.655(e). You may determine the raw exhaust flow rate based on the measured intake air and dilute exhaust molar flow rates and the dilute exhaust chemical balance terms as... air, fuel rate measurements, and fuel properties, consistent with good engineering judgment. (b...

40 CFR 1065.546 - Verification of minimum dilution ratio for PM batch sampling.

Code of Federal Regulations, 2014 CFR

2014-07-01

... chemical balance terms as given in § 1065.655(e). You may determine the raw exhaust flow rate based on the measured intake air and dilute exhaust molar flow rates and the dilute exhaust chemical balance terms as... air, fuel rate measurements, and fuel properties, consistent with good engineering judgment. (b...

Effects of storage in ozonised slurry ice on the sensory and microbial quality of sardine (Sardina pilchardus).

PubMed

Campos, Carmen A; Rodríguez, Oscar; Losada, Vanesa; Aubourg, Santiago P; Barros-Velázquez, Jorge

2005-08-25

The use of slurry ice, both alone and in combination with ozone, as compared with traditional flake ice was investigated as a new refrigeration system for the storage of sardine (Sardina pilchardus). Microbiological, chemical and sensory analyses were carried out throughout a storage period of 22 days. According to sensory analyses, sardine specimens stored in ozonised slurry ice had a shelf life of 19 days, while counterpart batches stored in slurry ice or flake ice had shelf lives of 15 and 8 days, respectively. Storage in ozonised slurry ice led to significantly lower counts of aerobic mesophiles, psychrotrophic bacteria, anaerobes, coliforms, and both lipolytic and proteolytic microorganisms in sardine muscle, and of surface counts of mesophiles and psychrotrophic bacteria in sardine skin as compared with the slurry ice and the flake ice batches. In all cases, the slurry ice batch also exhibited significantly lower microbial counts, both in muscle and skin, than the flake ice batch. Chemical parameters revealed that the use of slurry ice slowed down the formation of TVB-N and TMA-N to a significant extent in comparison with storage in flake ice. A combination of slurry ice with ozone also allowed a better control of pH and TMA-N formation as compared with slurry ice alone. This work demonstrates that the combined use of slurry ice and ozone for the storage of sardine can be recommended to improve the quality and extend the shelf life of this fish species.

Cocoa residues as viable biomass for renewable energy production through anaerobic digestion.

PubMed

Acosta, Nayaret; De Vrieze, Jo; Sandoval, Verónica; Sinche, Danny; Wierinck, Isabella; Rabaey, Korneel

2018-05-31

The aim of this work was to evaluate the bioenergy potential of cocoa residue via anaerobic digestion. Batch and fed-batch lab-scale reactors were operated under low and high solids conditions. In the batch tests, 59 ± 4% of Chemical Oxygen Demand (COD) was recovered as methane. This corresponded with an average methane yield of 174 (wet) and 193 (dry) L kg -1 volatile solids fed, whereas a series of fed-batch reactors produced 70 ± 24 (wet) and 107 ± 39 (dry) L CH 4  kg -1 volatile solids fed during stable conditions. A case study was developed for canton Balao (Ecuador) based on our experimental data, operational estimates and available cocoa waste in the area. Annually, 8341 MWh could be produced, meeting 88% of the current electricity demand in Balao. This case study proves the potential for cocoa waste as a source of renewable energy in rural areas. Copyright © 2018 Elsevier Ltd. All rights reserved.

Electrochemical treatment of tannery effluent using a battery integrated DC-DC converter and solar PV power supply--an approach towards environment and energy management.

PubMed

Iyappan, K; Basha, C Ahmed; Saravanathamizhan, R; Vedaraman, N; Tahiyah Nou Shene, C A; Begum, S Nathira

2014-01-01

Electrochemical oxidation of tannery effluent was carried out in batch, batch recirculation and continuous reactor configurations under different conditions using a battery-integrated DC-DC converter and solar PV power supply. The effect of current density, electrolysis time and fluid flow rate on chemical oxygen demand (COD) removal and energy consumption has been evaluated. The results of batch reactor show that a COD reduction of 80.85% to 96.67% could be obtained. The results showed that after 7 h of operation at a current density of 2.5 A dm(-2) and flow rate of 100 L h(-1) in batch recirculation reactor, the removal of COD is 82.14% and the specific energy consumption was found to be 5.871 kWh (kg COD)(-1) for tannery effluent. In addition, the performance of single pass flow reactors (single and multiple reactors) system of various configurations are analyzed.

Development of a Batch Fabrication Process for Chemical Nanosensors: Recent Advancements at NASA Glenn Research Center

NASA Technical Reports Server (NTRS)

Biaggi-Labiosa, Azlin M.

2014-01-01

A major objective in aerospace sensor development is to produce sensors that are small in size, easy to batch fabricate and low in cost, and have low power consumption. Chemical sensors involving nanostructured materials can provide these characteristics as well as the potential for the development of sensor systems with unique properties and improved performance. However, the fabrication and processing of nanostructures for sensor applications currently is limited by the ability to control their location on the sensor platform, which in turn hinders the progress for batch fabrication. This presentation will discuss the following: the development of a novel room temperature methane (CH4) sensor fabricated using porous tin oxide (SnO2) nanorods as the sensing material, the advantages of using nanomaterials in sensor designs, the challenges encountered with the integration of nanostructures into microsensordevices, and the different methods that have been attempted to address these challenges. An approach for the mass production of sensors with nanostructures using a method developed by our group at the NASA Glenn Research Center to control the alignment of nanostructures onto a sensor platform will also be described.

Ready-to-eat vegetables production with low-level water chlorination. An evaluation of water quality, and of its impact on end products.

PubMed

D'Acunzo, Francesca; Del Cimmuto, Angela; Marinelli, Lucia; Aurigemma, Caterina; De Giusti, Maria

2012-01-01

We evaluated the microbiological impact of low-level chlorination (1 ppm free chlorine) on the production of ready-to-eat (RTE) vegetables by monitoring the microbiological quality of irrigation and processing water in two production plants over a 4-season period, as well as the microbiological quality of unprocessed vegetables and RTE product. Water samples were also characterized in terms of some chemical and physico-chemical parameters of relevance in chlorination management. Both producers use water with maximum 1 ppm free chlorine for vegetables rinsing, while the two processes differ by the number of washing cycles. Salmonella spp and Campylobacter spp were detected once in two different irrigation water samples out of nine from one producer. No pathogens were found in the vegetable samples. As expected, the procedure encompassing more washing cycles performed slightly better in terms of total mesophilic count (TMC) when comparing unprocessed and RTE vegetables of the same batch. However, data suggest that low-level chlorination may be insufficient in preventing microbial build-up in the washing equipment and/or batch-to batch cross-contamination.

Deletion of lactate dehydrogenase in Enterobacter aerogenes to enhance 2,3-butanediol production.

PubMed

Jung, Moo-Young; Ng, Chiam Yu; Song, Hyohak; Lee, Jinwon; Oh, Min-Kyu

2012-07-01

2,3-Butanediol is an important bio-based chemical product, because it can be converted into several C4 industrial chemicals. In this study, a lactate dehydrogenase-deleted mutant was constructed to improve 2,3-butanediol productivity in Enterobacter aerogenes. To delete the gene encoding lactate dehydrogenase, λ Red recombination method was successfully adapted for E. aerogenes. The resulting strain produced a very small amount of lactate and 16.7% more 2,3-butanediol than that of the wild-type strain in batch fermentation. The mutant and its parental strain were then cultured with six different carbon sources, and the mutant showed higher carbon source consumption and microbial growth rates in all media. The 2,3-butanediol titer reached 69.5 g/l in 54 h during fed-batch fermentation with the mutant,which was 27.4% higher than that with the parental strain.With further optimization of the medium and aeration conditions,118.05 g/l 2,3-butanediol was produced in 54 h during fed-batch fermentation with the mutant. This is by far the highest titer of 2,3-butanediol with E. aerogenes achieved by metabolic pathway engineering.

Chromatographic separation and continuously referenced, on-line monitoring of creatine kinase isoenzymes by use of an immobilized-enzyme microreactor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Denton, M.S.; Bostick, W.D.; Dinsmore, S.R.

1978-08-01

We describe a new concept in continuously referenced monitoring of the isoenzyme activities of creatine kinase (EC 2.7.3.2) after liquid-chromatographic separation. After separation on a diethylaminoethyl-Sephacel column, the three isoenzymes of creatine kinase undergo a series of coupled enzyme reactions, ultimately resulting in the formation of ultraviolet-detectable NADPH. A major advantage of this detection system is the immobilized-enzyme microreactor (2 x 17 mm), which may be removed and stored refrigerated when not in use. A split-stream configuration allows self-blanking of endogenous ultraviolet-absorbing constituents in authentic sera samples, which would otherwise make definitive diagnosis and quantitation difficult or impossible. This detectionmore » system is applicable to the automated analysis of creatine kinase isoenzymes in the clinical laboratory.« less

Hysteretic Tricolor Electrochromic Systems Based on the Dynamic Redox Properties of Unsymmetrically Substituted Dihydrophenanthrenes and Biphenyl-2,2'-Diyl Dications: Efficient Precursor Synthesis by a Flow Microreactor Method

PubMed Central

Ishigaki, Yusuke; Suzuki, Takanori; Nishida, Jun-ichi; Nagaki, Aiichiro; Takabayashi, Naofumi; Kawai, Hidetoshi; Fujiwara, Kenshu; Yoshida, Jun-ichi

2011-01-01

A series of biphenyl-2,2'-diylbis(diarylmethanol)s 3, which have two kinds of aryl groups at the bay region, were efficiently obtained by integrated flow microreactor synthesis. The diols 3NO/NX are the precursors of unsymmetric biphenylic dications 2NO/NX2+, which are transformed into the corresponding dihydrophenanthrenes 1NO/NX via 2NO/NX+• upon reduction, when they exhibit two-stage color changes. On the other hand, the steady-state concentration of the intermediate 2NO/NX+• is negligible during the oxidation of 1NO/NX to 2NO/NX2+, which reflects unique tricolor electrochromicity with a hysteretic pattern of color change [color 1→color 2→color 3→color 1]. PMID:28824114

Closure for milliliter scale bioreactor

DOEpatents

Klein, David L.; Laidlaw, Robert D.; Andronaco, Gregory; Boyer, Stephen G.

2010-12-14

A closure for a microreactor includes a cap that is configured to be inserted into a well of the microreactor. The cap, or at least a portion of the cap, is compliant so as to form a seal with the well when the cap is inserted. The cap includes an aperture that provides an airway between the inside of the well to the external environment when the cap is inserted into the well. A porous plug is inserted in the aperture, e.g., either directly or in tube that extends through the aperture. The porous plug permits gas within the well to pass through the aperture while preventing liquids from passing through to reduce evaporation and preventing microbes from passing through to provide a sterile environment. A one-way valve may also be used to help control the environment in the well.

The in situ generation and reactive quench of diazonium compounds in the synthesis of azo compounds in microreactors.

PubMed

Akwi, Faith M; Watts, Paul

2016-01-01

In this paper, a micro-fluidic optimized process for the continuous flow synthesis of azo compounds is presented. The continuous flow synthesis of Sudan II azo dye was used as a model reaction for the study. At found optimal azo coupling reaction temperature and pH an investigation of the optimum flow rates of the reactants for the diazotization and azo coupling reactions in Little Things Factory-MS microreactors was performed. A conversion of 98% was achieved in approximately 2.4 minutes and a small library of azo compounds was thus generated under these reaction conditions from couplers with aminated or hydroxylated aromatic systems. The scaled up synthesis of these compounds in PTFE tubing (i.d. 1.5 mm) was also investigated, where good reaction conversions ranging between 66-91% were attained.

Determination of the inhibitory effect of green tea extract on glucose-6-phosphate dehydrogenase based on multilayer capillary enzyme microreactor.

PubMed

Camara, Mohamed Amara; Tian, Miaomiao; Liu, Xiaoxia; Liu, Xin; Wang, Yujia; Yang, Jiqing; Yang, Li

2016-08-01

Natural herbal medicines are an important source of enzyme inhibitors for the discovery of new drugs. A number of natural extracts such as green tea have been used in prevention and treatment of diseases due to their low-cost, low toxicity and good performance. The present study reports an online assay of the activity and inhibition of the green tea extract of the Glucose 6-phosphate dehydrogenase (G6PDH) enzyme using multilayer capillary electrophoresis based immobilized enzyme microreactors (CE-IMERs). The multilayer CE-IMERs were produced with layer-by-layer electrostatic assembly, which can easily enhance the enzyme loading capacity of the microreactor. The activity of the G6PDH enzyme was determined and the enzyme inhibition by the inhibitors from green tea extract was investigated using online assay of the multilayer CE-IMERs. The Michaelis constant (Km ) of the enzyme, the IC50 and Ki values of the inhibitors were achieved and found to agree with those obtained using offline assays. The results show a competitive inhibition of green tea extract on the G6PDH enzyme. The present study provides an efficient and easy-to-operate approach for determining G6PDH enzyme reaction and the inhibition of green tea extract, which may be beneficial in research and the development of natural herbal medicines. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Thermal Decomposition of Methyl Acetate (CH_3COOCH_3) in a Flash-Pyrolysis Micro-Reactor

NASA Astrophysics Data System (ADS)

Porterfield, Jessica P.; Bross, David H.; Ruscic, Branko; Thorpe, James H.; Nguyen, Thanh Lam; Baraban, Joshua H.; Stanton, John F.; Daily, John W.; Ellison, Barney

2017-06-01

The thermal decomposition of methyl acetate (CH_3COOCH_3) has been studied in a set of flash pyrolysis micro-reactors. Samples were diluted to (0.06 - 0.13%) in carrier gases (He, Ar) and subjected to temperatures of 300 - 1600 K at roughly 20 Torr. After residence times of approximately 25 - 150 μseconds, the unimolecular pyrolysis products were detected by vacuum ultraviolet photoionization mass spectrometry at 10.487 eV (118.2 nm). Complementary product identification was provided by matrix isolation infrared spectroscopy. Decomposition began at 1000 K with the observation of (CH_2=C=O, CH_3OH), products of a four centered rearrangement with a Δ_{rxn}H_{298} = 39.1 ± 0.2 kcal mol^{-1}. As the micro-reactor was heated to 1300 K, a mixture of (CH_2=C=O, CH_3OH, CH_3, CH_2=O, H, CO, CO_2) appeared. A new novel pathway is calculated in which both methyl groups leave behind CO_2 simultaneously, Δ_{rxn}H_{298} = 74.5 ± 0.4 kcal mol^{-1}. This pathway is in contrast to step-wise loss of methyl radical, which can go in two ways: Δ_{rxn}H_{298} (CH_3COOCH_3 → CH_3 + COOCH_3) = 95.4 ± 0.4 kcal mol^{-1}, Δ_{rxn}H_{298} (CH_3COOCH_3 → CH_3COO + CH_3) = 88.0 ± 0.3 kcal mol^{-1}.

Fast Batch Production of High-Quality Graphene Films in a Sealed Thermal Molecular Movement System.

PubMed

Xu, Jianbao; Hu, Junxiong; Li, Qi; Wang, Rubing; Li, Weiwei; Guo, Yufen; Zhu, Yongbo; Liu, Fengkui; Ullah, Zaka; Dong, Guocai; Zeng, Zhongming; Liu, Liwei

2017-07-01

Chemical vapor deposition (CVD) growth of high-quality graphene has emerged as the most promising technique in terms of its integrated manufacturing. However, there lacks a controllable growth method for producing high-quality and a large-quantity graphene films, simultaneously, at a fast growth rate, regardless of roll-to-roll (R2R) or batch-to-batch (B2B) methods. Here, a stationary-atmospheric-pressure CVD (SAPCVD) system based on thermal molecular movement, which enables fast B2B growth of continuous and uniform graphene films on tens of stacked Cu(111) foils, with a growth rate of 1.5 µm s -1 , is demonstrated. The monolayer graphene of batch production is found to nucleate from arrays of well-aligned domains, and the films possess few defects and exhibit high carrier mobility up to 6944 cm 2 V -1 s -1 at room temperature. The results indicate that the SAPCVD system combined with single-domain Cu(111) substrates makes it possible to realize fast batch-growth of high-quality graphene films, which opens up enormous opportunities to use this unique 2D material for industrial device applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A high-throughput media design approach for high performance mammalian fed-batch cultures

PubMed Central

Rouiller, Yolande; Périlleux, Arnaud; Collet, Natacha; Jordan, Martin; Stettler, Matthieu; Broly, Hervé

2013-01-01

An innovative high-throughput medium development method based on media blending was successfully used to improve the performance of a Chinese hamster ovary fed-batch medium in shaking 96-deepwell plates. Starting from a proprietary chemically-defined medium, 16 formulations testing 43 of 47 components at 3 different levels were designed. Media blending was performed following a custom-made mixture design of experiments considering binary blends, resulting in 376 different blends that were tested during both cell expansion and fed-batch production phases in one single experiment. Three approaches were chosen to provide the best output of the large amount of data obtained. A simple ranking of conditions was first used as a quick approach to select new formulations with promising features. Then, prediction of the best mixes was done to maximize both growth and titer using the Design Expert software. Finally, a multivariate analysis enabled identification of individual potential critical components for further optimization. Applying this high-throughput method on a fed-batch, rather than on a simple batch, process opens new perspectives for medium and feed development that enables identification of an optimized process in a short time frame. PMID:23563583

Chemical oxygen demand removal efficiency and limited factors study of aminosilicone polymers in a water emulsion by iron-carbon micro-electrolysis.

PubMed

Yang, Shangyuan; Liang, Zhiwei; Yu, Huadong; Wang, Yunlong; Chen, Yingxu

2014-02-01

Micro-electrolysis was applied in the present study to investigate the effect of pH, iron-carbon mass ratio, contact time, and treatment batch on the removal efficiency of chemical oxygen demand (COD) within an aminosilicone emulsion. The results exhibited that the removal efficiency of COD decreased linearly with the batch increase, and this tendency was consistent under the various conditions. The adsorption of activated carbons contributes a large portion to the elimination of COD within the aminosilicone emulsion. The oxidation action of iron-carbon micro-electrolysis was proven and the aminosilicone emulsion's COD removal contribution was approximately 16%. Aminosilicone polymers were adsorbed on the surface of activated carbons and iron chips, which contributes to the decline of COD removal efficiency and limits the contribution of oxidation action.

GICHD Mine Dog Testing Project - Soil Sample Results No.3

DOE Office of Scientific and Technical Information (OSTI.GOV)

PHELAN, JAMES M.; BARNETT, JAMES L.; BENDER, SUSAN FAE ANN

2003-03-01

A mine dog evaluation project initiated by the Geneva International Center for Humanitarian Demining is evaluating the capability and reliability of mine detection dogs. The performance of field-operational mine detection dogs will be measured in test minefields in Afghanistan and Bosnia containing actual, but unfused landmines. Repeated performance testing over two years through various seasonal weather conditions will provide data simulating near real world conditions. Soil samples will be obtained adjacent to the buried targets repeatedly over the course of the test. Chemical analysis results from these soil samples will be used to evaluate correlations between mine dog detection performancemore » and seasonal weather conditions. This report documents the analytical chemical methods and results from the third batch of soils received. This batch contained samples from Kharga, Afghanistan collected in October 2002.« less

GICHD mine dog testing project : soil sample results #5.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Barnett, James L.; Phelan, James M.; Archuleta, Luisa M.

2004-01-01

A mine dog evaluation project initiated by the Geneva International Center for Humanitarian Demining is evaluating the capability and reliability of mine detection dogs. The performance of field-operational mine detection dogs will be measured in test minefields in Afghanistan containing actual, but unfused landmines. Repeated performance testing over two years through various seasonal weather conditions will provide data simulating near real world conditions. Soil samples will be obtained adjacent to the buried targets repeatedly over the course of the test. Chemical analysis results from these soil samples will be used to evaluate correlations between mine dog detection performance and seasonalmore » weather conditions. This report documents the analytical chemical methods and results from the fifth batch of soils received. This batch contained samples from Kharga, Afghanistan collected in June 2003.« less

Luminescent chemical waves in the Cu(II)-catalyzed oscillatory oxidation of SCN- ions with hydrogen peroxide.

PubMed

Pekala, Katarzyna; Jurczakowski, Rafał; Lewera, Adam; Orlik, Marek

2007-05-10

The oscillatory oxidation of thiocyanate ions with hydrogen peroxide, catalyzed by Cu2+ ions in alkaline media, was so far observed as occurring simultaneously in the entire space of the batch or flow reactor. We performed this reaction for the first time in the thin-layer reactor and observed the spatiotemporal course of the above process, in the presence of luminol as the chemiluminescent indicator. A series of luminescent patterns periodically starting from the random reaction center and spreading throughout the entire solution layer was reported. For a batch-stirred system, the bursts of luminescence were found to correlate with the steep decreases of the oscillating Pt electrode potential. These novel results open possibilities for further experimental and theoretical investigations of those spatiotemporal patterns, including studies of the mechanism of this chemically complex process.

Bio-based extraction and stabilization of anthocyanins.

PubMed

Roy, Anirban; Mukherjee, Rudra Palash; Howard, Luke; Beitle, Robert

2016-05-01

This work reports a novel method of recovering anthocyanin compounds from highly-pigmented grapes via a fermentation based approach. It was hypothesized that batch growth of Zymomonas mobilis on simple medium would produce both ethanol and enzymes/biomass-acting materials, the combination of which will provide a superior extraction when compared to simple alcohol extraction. To examine this hypothesis, Z. mobilis was fermented in a batch consisting of mashed Vitis vinifera and glucose, and the recovered anthocyanin pool was compared to that recovered via extraction with ethanol. Data indicated higher amounts of anthocyanins were recovered when compared to simple solvent addition. Additionally, the percent polymeric form of the anthocyanins could be manipulated by the level of aeration maintained in the fermentation. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:601-605, 2016. © 2016 American Institute of Chemical Engineers.

Flow chemistry: intelligent processing of gas-liquid transformations using a tube-in-tube reactor.

PubMed

Brzozowski, Martin; O'Brien, Matthew; Ley, Steven V; Polyzos, Anastasios

2015-02-17

CONSPECTUS: The previous decade has witnessed the expeditious uptake of flow chemistry techniques in modern synthesis laboratories, and flow-based chemistry is poised to significantly impact our approach to chemical preparation. The advantages of moving from classical batch synthesis to flow mode, in order to address the limitations of traditional approaches, particularly within the context of organic synthesis are now well established. Flow chemistry methodology has led to measurable improvements in safety and reduced energy consumption and has enabled the expansion of available reaction conditions. Contributions from our own laboratories have focused on the establishment of flow chemistry methods to address challenges associated with the assembly of complex targets through the development of multistep methods employing supported reagents and in-line monitoring of reaction intermediates to ensure the delivery of high quality target compounds. Recently, flow chemistry approaches have addressed the challenges associated with reactions utilizing reactive gases in classical batch synthesis. The small volumes of microreactors ameliorate the hazards of high-pressure gas reactions and enable improved mixing with the liquid phase. Established strategies for gas-liquid reactions in flow have relied on plug-flow (or segmented flow) regimes in which the gas plugs are introduced to a liquid stream and dissolution of gas relies on interfacial contact of the gas bubble with the liquid phase. This approach confers limited control over gas concentration within the liquid phase and is unsuitable for multistep methods requiring heterogeneous catalysis or solid supported reagents. We have identified the use of a gas-permeable fluoropolymer, Teflon AF-2400, as a simple method of achieving efficient gas-liquid contact to afford homogeneous solutions of reactive gases in flow. The membrane permits the transport of a wide range of gases with significant control of the stoichiometry of reactive gas in a given reaction mixture. We have developed a tube-in-tube reactor device consisting of a pair of concentric capillaries in which pressurized gas permeates through an inner Teflon AF-2400 tube and reacts with dissolved substrate within a liquid phase that flows within a second gas impermeable tube. This Account examines our efforts toward the development of a simple, unified methodology for the processing of gaseous reagents in flow by way of development of a tube-in-tube reactor device and applications to key C-C, C-N, and C-O bond forming and hydrogenation reactions. We further describe the application to multistep reactions using solid-supported reagents and extend the technology to processes utilizing multiple gas reagents. A key feature of our work is the development of computer-aided imaging techniques to allow automated in-line monitoring of gas concentration and stoichiometry in real time. We anticipate that this Account will illustrate the convenience and benefits of membrane tube-in-tube reactor technology to improve and concomitantly broaden the scope of gas/liquid/solid reactions in organic synthesis.

Batch bioethanol production via the biological and chemical saccharification of some Egyptian marine macroalgae.

PubMed

Soliman, Ramadan M; Younis, Sherif A; El-Gendy, Nour Sh; Mostafa, Soha S M; El-Temtamy, Seham A; Hashim, Ahmed I

2018-04-19

Marine seaweeds (macroalgae) cause eutrophication problem and affects the touristic activities. The success of the production of the third generation bioethanol from marine macroalgae depends mainly on the development of an ecofriendly and eco-feasible pretreatment (i.e. hydrolysis) technique, a highly effective saccharification step and finally an efficient bioethanol fermentation step. Therefore, this study aimed to investigate the potentiality of different marine macroalgal strains, collected from Egyptian coasts, for bioethanol production via different saccharification processes. Different marine macroalgal strains; red Jania rubens, green Ulva lactuca. and brown Sargassum latifolium, have been collected from Egyptian Mediterranean and Red Sea shores. Different hydrolysis processes were evaluated to maximize the extraction of fermentable sugars; thermo-chemical hydrolysis with diluted acids (HCl and H 2 SO 4 ) and base (NaOH), hydrothermal hydrolysis followed by saccharification with different fungal strains and finally, thermo-chemical hydrolysis with diluted HCl, followed by fungal saccharification. The hydrothermal hydrolysis of Sargassum latifolium followed by biological saccharification using Trichoderma asperellum RM1 produced maximum total sugars of 510 mg g -1 macroalgal biomass. The integration of the hydrothermal and fungal hydrolyses of the macroalgal biomass with a separate batch fermentation of the produced sugars using two Saccharomyces cerevisiae strains, produced approximately 0.29 g bioethanol g -1 total reducing sugars. A simulated regression modeling for the batch bioethanol fermentation was also performed. This study, supported the possibility of using seaweeds as a renewable source of bioethanol, throughout a suggested integration of macroalgal biomass hydrothermal- and fungal- hydrolysis with a separate batch bioethanol fermentation process of the produced sugars. The usage of marine macroalgae (i.e. seaweeds) as feedstock for bioethanol; an alternative and/or complimentary to petro-fuel, would act as triple fact solution; bioremediation process for ecosystem, renewable energy source and economy savings. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Effect of xylan and lignin removal by batch and flowthrough pretreatment on the enzymatic digestibility of corn stover cellulose.

PubMed

Yang, Bin; Wyman, Charles E

2004-04-05

Compared with batch systems, flowthrough and countercurrent reactors have important potential advantages for pretreating cellulosic biomass, including higher hemicellulose sugar yields, enhanced cellulose digestibility, and reduced chemical additions. Unfortunately, they suffer from high water and energy use. To better understand these trade-offs, comparative data are reported on xylan and lignin removal and enzymatic digestibility of cellulose for corn stover pretreated in batch and flowthrough reactors over a range of flow rates between 160 degrees and 220 degrees C, with water only and also with 0.1 wt% sulfuric acid. Increasing flow with just water enhanced the xylan dissolution rate, more than doubled total lignin removal, and increased cellulose digestibility. Furthermore, adding dilute sulfuric acid increased the rate of xylan removal for both batch and flowthrough systems. Interestingly, adding acid also increased the lignin removal rate with flow, but less lignin was left in solution when acid was added in batch. Although the enzymatic hydrolysis of pretreated cellulose was related to xylan removal, as others have shown, the digestibility was much better for flowthrough compared with batch systems, for the same degree of xylan removal. Cellulose digestibility for flowthrough reactors was related to lignin removal as well. These results suggest that altering lignin also affects the enzymatic digestibility of corn stover. Copyright 2004 Wiley Periodicals, Inc.

Sample preconcentration with chemical derivatization in capillary electrophoresis. Capillary as preconcentrator, microreactor and chiral selector for high-throughput metabolite screening.

PubMed

Ptolemy, Adam S; Britz-McKibbin, Philip

2006-02-17

New strategies for integrating sample pretreatment with chemical analyses under a single format is required for rapid, sensitive and enantioselective analyses of low abundance metabolites in complex biological samples. Capillary electrophoresis (CE) offers a unique environment for controlling analyte/reagent band dispersion and electromigration properties using discontinuous electrolyte systems. Recent work in our laboratory towards developing a high-throughput CE platform for low abundance metabolites via on-line sample preconcentration with chemical derivatization (SPCD) is primarily examined in this review, as there have been surprisingly only a few strategies reported in the literature to date. In-capillary sample preconcentration serves to enhance concentration sensitivity via electrokinetic focusing of long sample injection volumes for lower detection limits, whereas chemical derivatization by zone passing is used to expand detectability and selectivity, notably for enantiomeric resolution of metabolites lacking intrinsic chromophores using nanolitre volumes of reagent. Together, on-line SPCD-CE can provide over a 100-fold improvement in concentration sensitivity, shorter total analysis times, reduced sample handling and improved reliability for a variety of amino acid and amino sugar metabolites, which is also amenable to automated high-throughput screening. This review will highlight basic method development and optimization parameters relevant to SPCD-CE, including applications to bacterial metabolite flux and biomarker analyses. Insight into the mechanism of analyte focusing and labeling by SPCD-CE is also discussed, as well as future directions for continued research.

Selective self-assembly of adenine-silver nanoparticles forms rings resembling the size of cells

NASA Astrophysics Data System (ADS)

Choi, Sungmoon; Park, Soonyoung; Yang, Seon-Ah; Jeong, Yujin; Yu, Junhua

2015-12-01

Self-assembly has played critical roles in the construction of functional nanomaterials. However, the structure of the macroscale multicomponent materials built by the self-assembly of nanoscale building blocks is hard to predict due to multiple intermolecular interactions of great complexity. Evaporation of solvents is usually an important approach to induce kinetically stable assemblies of building blocks with a large-scale specific arrangement. During such a deweting process, we tried to monitor the possible interactions between silver nanoparticles and nucleobases at a larger scale by epifluorescence microscopy, thanks to the doping of silver nanoparticles with luminescent silver nanodots. ssDNA oligomer-stabilized silver nanoparticles and adenine self-assemble to form ring-like compartments similar to the size of modern cells. However, the silver ions only dismantle the self-assembly of adenine. The rings are thermodynamically stable as the drying process only enrich the nanoparticles-nucleobase mixture to a concentration that activates the self-assembly. The permeable membrane-like edge of the ring is composed of adenine filaments glued together by silver nanoparticles. Interestingly, chemicals are partially confined and accumulated inside the ring, suggesting that this might be used as a microreactor to speed up chemical reactions during a dewetting process.

Aerosol Synthesis of N and N-S Doped and Crumpled Graphene Nanostructures.

PubMed

Carraro, Francesco; Cattelan, Mattia; Favaro, Marco; Calvillo, Laura

2018-06-06

Chemically modified graphene⁻based materials (CMG) are currently attracting a vast interest in their application in different fields. In particular, heteroatom-doped graphenes have revealed great potentialities in the field of electrocatalysis as substitutes of fuel cell noble metal⁻based catalysts. In this work, we investigate an innovative process for doping graphene nanostructures. We optimize a novel synthetic route based on aerosol preparation, which allows the simultaneous doping, crumpling, and reduction of graphene oxide (GO). Starting from aqueous solutions containing GO and the dopant precursors, we synthesize N- and N,S-dual-doped 3D graphene nanostructures (N-cGO and N,S-cGO). In the aerosol process, every aerosol droplet can be considered as a microreactor where dopant precursors undergo thermal decomposition and react with the GO flakes. Simultaneously, thanks to the relatively high temperature, GO undergoes crumpling and partial reduction. Using a combination of spectroscopic and microscopic characterization techniques, we investigate the morphology of the obtained materials and the chemical nature of the dopants within the crumpled graphene sheets. This study highlights the versatility of the aerosol process for the design of new CMG materials with tailored electrocatalytic properties.

Merging microfluidics and sonochemistry: towards greener and more efficient micro-sono-reactors.

PubMed

Fernandez Rivas, David; Cintas, Pedro; Gardeniers, Han J G E

2012-11-18

Microfluidics enable the manipulation of chemical reactions using very small amounts of fluid, in channels with dimensions of tens to hundreds of micrometers; so-called microstructured devices, from which the iconic image of chips emerges. The immediate attraction of microfluidics lies in its greenness: use of small quantities of reagents and solvents, and hence less waste, a precise control of reaction conditions, integration of functionality for process intensification, safer and often faster protocols, reliable scale-up, and possibility of performing multiphase reactions. Among the limitations found in microfluidics the facile formation of precipitating products should be highlighted, and in this context, the search for efficient mass and energy transfers is a must. Such limitations have been partially overcome with the aid of ultrasound in conventional flow systems, and can now be successfully used in microreactors, which provide new capabilities. Novel applications and a better understanding of the physical and chemical aspects of sonochemistry can certainly be achieved by combining microfluidics and ultrasound. We will review this nascent area of research, paying attention to the latest developments and showing future directions, which benefit both from the existing microfluidic technology and sonochemistry itself.

Primitive Photosynthetic Architectures Based on Self-Organization and Chemical Evolution of Amino Acids and Metal Ions.

PubMed

Liu, Kai; Ren, Xiaokang; Sun, Jianxuan; Zou, Qianli; Yan, Xuehai

2018-06-01

The emergence of light-energy-utilizing metabolism is likely to be a critical milestone in prebiotic chemistry and the origin of life. However, how the primitive pigment is spontaneously generated still remains unknown. Herein, a primitive pigment model based on adaptive self-organization of amino acids (Cystine, Cys) and metal ions (zinc ion, Zn 2+ ) followed by chemical evolution under hydrothermal conditions is developed. The resulting hybrid microspheres are composed of radially aligned cystine/zinc (Cys/Zn) assembly decorated with carbonate-doped zinc sulfide (C-ZnS) nanocrystals. The part of C-ZnS can work as a light-harvesting antenna to capture ultraviolet and visible light, and use it in various photochemical reactions, including hydrogen (H 2 ) evolution, carbon dioxide (CO 2 ) photoreduction, and reduction of nicotinamide adenine dinucleotide (NAD + ) to nicotinamide adenine dinucleotide hydride (NADH). Additionally, guest molecules (e.g., glutamate dehydrogenase, GDH) can be encapsulated within the hierarchical Cys/Zn framework, which facilitates sustainable photoenzymatic synthesis of glutamate. This study helps deepen insight into the emergent functionality (conversion of light energy) and complexity (hierarchical architecture) from interaction and reaction of prebiotic molecules. The primitive pigment model is also promising to work as an artificial photosynthetic microreactor.

Bacteriophage PRD1 batch experiments to study attachment, detachment and inactivation processes

NASA Astrophysics Data System (ADS)

Sadeghi, Gholamreza; Schijven, Jack F.; Behrends, Thilo; Hassanizadeh, S. Majid; van Genuchten, Martinus Th.

2013-09-01

Knowledge of virus removal in subsurface environments is pivotal for assessing the risk of viral contamination of water resources and developing appropriate protection measures. Columns packed with sand are frequently used to quantify attachment, detachment and inactivation rates of viruses. Since column transport experiments are very laborious, a common alternative is to perform batch experiments where usually one or two measurements are done assuming equilibrium is reached. It is also possible to perform kinetic batch experiments. In that case, however, it is necessary to monitor changes in the concentration with time. This means that kinetic batch experiments will be almost as laborious as column experiments. Moreover, attachment and detachment rate coefficients derived from batch experiments may differ from those determined using column experiments. The aim of this study was to determine the utility of kinetic batch experiments and investigate the effects of different designs of the batch experiments on estimated attachment, detachment and inactivation rate coefficients. The experiments involved various combinations of container size, sand-water ratio, and mixing method (i.e., rolling or tumbling by pivoting the tubes around their horizontal or vertical axes, respectively). Batch experiments were conducted with clean quartz sand, water at pH 7 and ionic strength of 20 mM, and using the bacteriophage PRD1 as a model virus. Values of attachment, detachment and inactivation rate coefficients were found by fitting an analytical solution of the kinetic model equations to the data. Attachment rate coefficients were found to be systematically higher under tumbling than under rolling conditions because of better mixing and more efficient contact of phages with the surfaces of the sand grains. In both mixing methods, more sand in the container yielded higher attachment rate coefficients. A linear increase in the detachment rate coefficient was observed with increased solid-water ratio using tumbling method. Given the differences in the attachment rate coefficients, and assuming the same sticking efficiencies since chemical conditions of the batch and column experiments were the same, our results show that collision efficiencies of batch experiments are not the same as those of column experiments. Upscaling of the attachment rate from batch to column experiments hence requires proper understanding of the mixing conditions. Because batch experiments, in which the kinetics are monitored, are as laborious as column experiments, there seems to be no major advantage in performing batch instead of column experiments.

Acceptance Test Data for the AGR-5/6/7 Irradiation Test Fuel Composite Defective IPyC Fraction and Pyrocarbon Anisotropy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Helmreich, Grant W.; Hunn, John D.; Skitt, Darren J.

Coated particle composite J52R-16-98005 was produced by Babcock and Wilcox Technologies (BWXT) as fuel for the Advanced Gas Reactor Fuel Development and Qualification (AGR) Program’s AGR-5/6/7 irradiation test in the Idaho National Laboratory (INL) Advanced Test Reactor (ATR). This composite was comprised of four coated particle fuel batches J52O-16-93165B (26%), 93168B (26%), 93169B (24%), and 93170B (24%), chosen based on the Quality Control (QC) data acquired for each individual candidate AGR-5/6/7 batch. Each batch was coated in a 150-mm-diameter production-scale fluidized-bed chemical vapor deposition (CVD) furnace. Tristructural isotropic (TRISO) coatings were deposited on 425-μm-nominal-diameter spherical kernels from BWXT Lot J52R-16-69317more » containing a mixture of 15.5%-enriched uranium carbide and uranium oxide (UCO). The TRISO coatings consisted of four consecutive CVD layers: a ~50% dense carbon buffer layer with 100-μm-nominal thickness, a dense inner pyrolytic carbon (IPyC) layer with 40-μm-nominal thickness, a silicon carbide (SiC) layer with 35-μm-nominal thickness, and a dense outer pyrolytic carbon (OPyC) layer with 40-μm-nominal thickness. The TRISO-coated particle batches were sieved to upgrade the particles by removing over-sized and under-sized material, and the upgraded batches were designated by appending the letter A to the end of the batch number (e.g., 93165A). Secondary upgrading by sieving was performed on the A-designated batches to remove particles with missing or very-thin buffer layers that were identified during previous analysis of the individual batches for defective IPyC, as reported in the acceptance test data report for the AGR-5/6/7 production batches [Hunn et al. 2017]. The additionally-upgraded batches were designated by appending the letter B to the end of the batch number (e.g., 93165B).« less

Remediation System Evaluation, Baird and McGuire Superfund Site

EPA Pesticide Factsheets

The 32.5-acre Baird and McGuire Superfund Site, located in Holbrook, Massachusetts, addresses VOC,SVOC, and arsenic contamination from a chemical mixing and batching plant that operated between 1912and 1983.

Dispersed catalysts for co-processing and coal liquefaction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bockrath, B.; Parfitt, D.; Miller, R.

1995-12-31

The basic goal is to improve dispersed catalysts employed in the production of clean fuels from low value hydrocarbons. The immediate objective is to determine how the properties of the catalysts may be altered to match the demands placed on them by the properties of the feedstock, the qualities of the desired end products, and the economic constraints put upon the process. Several interrelated areas of the application of dispersed catalysts to co-processing and coal conversion are under investigation. The first involves control of the selectivity of MoS{sub 2} catalysts for HDN, HDS, and hydrogenation of aromatics. A second areamore » of research is the development and use of methods to evaluate dispersed catalysts by means of activity and selectivity tests. A micro-flow reactor has been developed for determining intrinsic reactivities using model compounds, and will be used to compare catalysts prepared in different ways. Micro-autoclaves will also be used to develop data in batch experiments at higher partial pressures of hydrogen. The third area under investigation concerns hydrogen spillover reactions between MoS{sub 2} catalysts and carbonaceous supports. Preliminary results obtained by monitoring H{sub 2}/D{sub 2} exchange reactions with a pulse-flow microreactor indicate the presence of spillover between MoS{sub 2} and a graphitic carbon. A more complete study will be made at a later stage of the project. Accomplishments and conclusions are discussed.« less

Magma batches in the Timber Mountain magmatic system, Southwestern Nevada Volcanic Field, Nevada, USA

NASA Astrophysics Data System (ADS)

Mills, James G.; Saltoun, Benjamin W.; Vogel, Thomas A.

1997-09-01

The common occurrence of compositionally and mineralogically zoned ash flow sheets, such as those of the Timber Mountain Group, provides evidence that the source magma bodies were chemically and thermally zoned. The Rainier Mesa and Ammonia Tanks tuffs of the Timber Mountain Group are both large volume (1200 and 900 km 3, respectively) chemically zoned (57-78 wt.% SiO 2) ash flow sheets. Evidence of distinct magma batches in the Timber Mountain system are based on: (1) major- and trace-element variations of whole pumice fragments; (2) major-element variations in phenocrysts; (3) major-element variations in glass matrix; and (4) emplacement temperatures calculated from Fe-Ti oxides and feldspars. There are three distinct groups of pumice fragments in the Rainier Mesa Tuff: a low-silica group and two high-silica groups (a low-Th and a high-Th group). These groups cannot be related by crystal fractionation. The low-silica portion of the Rainier Mesa Tuff is distinct from the low-silica portion of the overlying Ammonia Tanks Tuff, even though the age difference is less than 200,000 years. Three distinct groups occur in the Ammonia Tanks Tuff: a low-silica, intermediate-silica and a high-silica group. Part of the high-silica group may be due to mixing of the two high-silica Rainier Mesa groups. The intermediate-silica group may be due to mixing of the low- and high-silica Ammonia Tanks groups. Three distinct emplacement temperatures occur in the Rainier Mesa Tuff (869, 804, 723 °C) that correspond to the low-silica, high-Th and low-Th magma batches, respectively. These temperature differences could not have been maintained for any length of time in the magma chamber (cf. Turner, J.S., Campbell, I.H., 1986. Convection and mixing in magma chambers. Earth-Sci. Rev. 23, 255-352; Martin, D., Griffiths, R.W., Campbell, I.H., 1987. Compositional and thermal convection in magma chambers. Contrib. Mineral. Petrol. 96, 465-475) and therefore eruption must have occurred soon after emplacement of the magma batches into the chamber. Emplacement temperatures of the pumice fragments from the Ammonia Tanks Tuff show a continuous gradient of temperatures with composition. This continuous temperature gradient is consistent with the model of storage of magma batches in the Ammonia Tanks group that have undergone both thermal and chemical diffusion.

Microreactor and method for preparing a radiolabeled complex or a biomolecule conjugate

DOEpatents

Reichert, David E; Kenis, Paul J. A.; Wheeler, Tobias D; Desai, Amit V; Zeng, Dexing; Onal, Birce C

2015-03-17

A microreactor for preparing a radiolabeled complex or a biomolecule conjugate comprises a microchannel for fluid flow, where the microchannel comprises a mixing portion comprising one or more passive mixing elements, and a reservoir for incubating a mixed fluid. The reservoir is in fluid communication with the microchannel and is disposed downstream of the mixing portion. A method of preparing a radiolabeled complex includes flowing a radiometal solution comprising a metallic radionuclide through a downstream mixing portion of a microchannel, where the downstream mixing portion includes one or more passive mixing elements, and flowing a ligand solution comprising a bifunctional chelator through the downstream mixing portion. The ligand solution and the radiometal solution are passively mixed while in the downstream mixing portion to initiate a chelation reaction between the metallic radionuclide and the bifunctional chelator. The chelation reaction is completed to form a radiolabeled complex.

Chromatographic separation and continuously referenced, on-line monitoring of creatine kinase isoenzymes by use of an immobilized-enzyme microreactor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Denton, M.S.; Bostick, W.D.; Dinsmore, S.R.

1978-08-01

We describe a new concept in continuously referenced monitoring of the isoenzyme activities of creatine kinase (EC 2.7.3.2) after liquid-chromatographic separation. After separation on a diethylaminoethyl-Sephacel column, the three isoenzymes of creatine kinase undergo a series of upled enzyme reactions, ultimately resulting in the formation of ultraviolet-detectable NADPH. A major advantage of this detection system is the immobilized-enzyme microreactor (2 x 17 mm), which may be removed and stored refrigerated when not in use. A split-stream configuration allows self-blanking of endogenous ultraviolet-absorbing constituents in authentic sera samples, which would otherwise make definitive diagnosis and quantitation difficult or impossible. This detectionmore » system is applicable to the automated analysis of creatine kinase isoenzymes in the clinical laboratory. 5 figures; 42 references.« less

Autonomous colloidal crystallization in a galvanic microreactor

NASA Astrophysics Data System (ADS)

Punckt, Christian; Jan, Linda; Jiang, Peng; Frewen, Thomas A.; Saville, Dudley A.; Kevrekidis, Ioannis G.; Aksay, Ilhan A.

2012-10-01

We report on a technique that utilizes an array of galvanic microreactors to guide the assembly of two-dimensional colloidal crystals with spatial and orientational order. Our system is comprised of an array of copper and gold electrodes in a coplanar arrangement, immersed in a dilute hydrochloric acid solution in which colloidal micro-spheres of polystyrene and silica are suspended. Under optimized conditions, two-dimensional colloidal crystals form at the anodic copper with patterns and crystal orientation governed by the electrode geometry. After the aggregation process, the colloidal particles are cemented to the substrate by co-deposition of reaction products. As we vary the electrode geometry, the dissolution rate of the copper electrodes is altered. This way, we control the colloidal motion as well as the degree of reaction product formation. We show that particle motion is governed by a combination of electrokinetic effects acting directly on the colloidal particles and bulk electrolyte flow generated at the copper-gold interface.

Development of photocatalyst coated fluoropolymer based microreactor using ultrasound for water remediation.

PubMed

Colmenares, Juan Carlos; Nair, Vaishakh; Kuna, Ewelina; Łomot, Dariusz

2018-03-01

Formation of thin layers of photocatalyst in photo-microreactor is a challenging work considering the properties of both catalyst and the microchannel material. The deposition of semiconductor materials on fluoropolymer based microcapillary requires the use of economical methods which are also less energy dependent. The current work introduces a new method for depositing nanoparticles of TiO 2 on the inner walls of a hexafluoropropylene tetrafluoroethylene microtube under mild conditions using ultrasound technique. During the ultrasonication process, changes in the polymer surface were observed and characterized using Attenuated Total Reflectance spectroscopy, Scanning Electron Microscopy and Confocal Microscopy. The rough patches form sites for catalyst deposition resulting in the formation of thin layer of TiO 2 nanoparticles in the inner walls of the microtube. The photocatalytic activity of the TiO 2 coated fluoropolymer based microcapillary was evaluated for removal of phenol present in water. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis and characterization of cationic lipid coated magnetic nanoparticles using multiple emulsions as microreactors

NASA Astrophysics Data System (ADS)

Akbaba, Hasan; Karagöz, Uğur; Selamet, Yusuf; Kantarcı, A. Gülten

2017-03-01

The aim of this study was to develop a novel iron oxide nanoparticle synthesis method with in-situ surface coating. For this purpose multiple emulsions were used as microreactors for the first time and magnetic iron oxide particles synthesized in the core of cationic solid lipid nanoparticles. DLS, SEM, TEM, VSM, Raman Spectrometer, XRD, and XPS techniques were performed for characterization of the magnetic nanoparticles. Obtained magnetic nanoparticles are superparamagnetic and no additional process was needed for surface adjustments. They are positively charged as a result of cationic lipid coating and has appropriate particle size (<30 nm) for drug or nucleic acid delivery. Structure analysis showed that magnetic core material is in the form of magnetite. Saturation magnetization value was measured as 15-17 emu g-1 for lipid coated magnetic nanoparticles obtained by multiple emulsion method which is reasonably sufficient for magnetic targeting.

Microwave and continuous flow technologies in drug discovery.

PubMed

Sadler, Sara; Moeller, Alexander R; Jones, Graham B

2012-12-01

Microwave and continuous flow microreactors have become mainstream heating sources in contemporary pharmaceutical company laboratories. Such technologies will continue to benefit from design and engineering improvements, and now play a key role in the drug discovery process. The authors review the applications of flow- and microwave-mediated heating in library, combinatorial, solid-phase, metal-assisted, and protein chemistries. Additionally, the authors provide a description of the combination of microwave and continuous flow platforms, with applications in the preparation of radiopharmaceuticals and in drug candidate development. Literature reviewed is chiefly 2000 - 2012, plus key citations from earlier reports. With the advent of microwave irradiation, reactions that normally took days to complete can now be performed in a matter of minutes. Coupled with the introduction of continuous flow microreactors, pharmaceutical companies have an easy way to improve the greenness and efficiency of many synthetic operations. The combined force of these technologies offers the potential to revolutionize discovery and manufacturing processes.

Chapter 8: Pyrolysis Mechanisms of Lignin Model Compounds Using a Heated Micro-Reactor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Robichaud, David J.; Nimlos, Mark R.; Ellison, G. Barney

2015-10-03

Lignin is an important component of biomass, and the decomposition of its thermal deconstruction products is important in pyrolysis and gasification. In this chapter, we investigate the unimolecular pyrolysis chemistry through the use of singly and doubly substituted benzene molecules that are model compounds representative of lignin and its primary pyrolysis products. These model compounds are decomposed in a heated micro-reactor, and the products, including radicals and unstable intermediates, are measured using photoionization mass spectrometry and matrix isolation infrared spectroscopy. We show that the unimolecular chemistry can yield insight into the initial decomposition of these species. At pyrolysis and gasificationmore » severities, singly substituted benzenes typically undergo bond scission and elimination reactions to form radicals. Some require radical-driven chain reactions. For doubly substituted benzenes, proximity effects of the substituents can change the reaction pathways.« less

A Catalyst-Free Amination of Functional Organolithium Reagents by Flow Chemistry.

PubMed

Kim, Heejin; Yonekura, Yuya; Yoshida, Jun-Ichi

2018-04-03

Reported is the electrophilic amination of functional organolithium intermediates with well-designed aminating reagents under mild reaction conditions using flow microreactors. The aminating reagents were optimized to achieve efficient C-N bond formation without using any catalyst. The electrophilic amination reactions of functionalized aryllithiums were successfully conducted under mild reaction conditions, within 1 minute, by using flow microreactors. The aminating reagent was also prepared by the flow method. Based on stopped-flow NMR analysis, the reaction time for the preparation of the aminating reagent was quickly optimized without the necessity of work-up. Integrated one-flow synthesis consisting of the generation of an aryllithium, the preparation of an aminating reagent, and their combined reaction was successfully achieved to give the desired amine within 5 minutes of total reaction time. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tao Xia; Liu Bing; Hou Qian

A new route for the economic and efficient treatment of azo dye pollutants is reported, in which surface-modified organic-inorganic hybrid mesoporous silica (MS) spheres were chosen as microreactors for the accumulation and subsequent photodegradation of pollutants in defined regions. The surface-modified silica materials were prepared by anchoring the polycationic species such as poly(allylamine hydrochloride) on MS spheres via a simple wet impregnation method. The as-synthesized spheres with well-defined porous structures exhibited 15 times of accumulating capacity for orange II and Congo red compared to that of the pure MS spheres. Diffuse reflectance UV-vis spectroscopy and confocal laser scanning microscopy demonstratedmore » that the accumulated orange II and CR in defined MS spheres were rapidly degraded in the presence of Fenton reagent under visible radiation. Kinetics analysis in recycling degradation showed that the as-synthesized materials might be utilized as environment-friendly preconcentrators/microreactors for the remediation of dye wastewater.« less

The in situ generation and reactive quench of diazonium compounds in the synthesis of azo compounds in microreactors

PubMed Central

Akwi, Faith M

2016-01-01

Summary In this paper, a micro-fluidic optimized process for the continuous flow synthesis of azo compounds is presented. The continuous flow synthesis of Sudan II azo dye was used as a model reaction for the study. At found optimal azo coupling reaction temperature and pH an investigation of the optimum flow rates of the reactants for the diazotization and azo coupling reactions in Little Things Factory-MS microreactors was performed. A conversion of 98% was achieved in approximately 2.4 minutes and a small library of azo compounds was thus generated under these reaction conditions from couplers with aminated or hydroxylated aromatic systems. The scaled up synthesis of these compounds in PTFE tubing (i.d. 1.5 mm) was also investigated, where good reaction conversions ranging between 66–91% were attained. PMID:27829903

Applications of Ni3Al Based Intermetallic Alloys—Current Stage and Potential Perceptivities

PubMed Central

Jozwik, Pawel; Polkowski, Wojciech; Bojar, Zbigniew

2015-01-01

The paper presents an overview of current and prospective applications of Ni3Al based intermetallic alloys—modern engineering materials with special properties that are potentially useful for both structural and functional purposes. The bulk components manufactured from these materials are intended mainly for forging dies, furnace assembly, turbocharger components, valves, and piston head of internal combustion engines. The Ni3Al based alloys produced by a directional solidification are also considered as a material for the fabrication of jet engine turbine blades. Moreover, development of composite materials with Ni3Al based alloys as a matrix hardened by, e.g., TiC, ZrO2, WC, SiC and graphene, is also reported. Due to special physical and chemical properties; it is expected that these materials in the form of thin foils and strips should make a significant contribution to the production of high tech devices, e.g., Micro Electro-Mechanical Systems (MEMS) or Microtechnology-based Energy and Chemical Systems (MECS); as well as heat exchangers; microreactors; micro-actuators; components of combustion chambers and gasket of rocket and jet engines as well components of high specific strength systems. Additionally, their catalytic properties may find an application in catalytic converters, air purification systems from chemical and biological toxic agents or in a hydrogen “production” by a decomposition of hydrocarbons.

Dopamine Polymerization in Liquid Marbles: A General Route to Janus Particle Synthesis.

PubMed

Sheng, Yifeng; Sun, Guanqing; Ngai, To

2016-04-05

Coating a liquid with a particle shell not only renders a droplet superhydrophobic but also isolates a well-confined microenvironment for miniaturized chemical processes. Previously, we have demonstrated that particles at the liquid marble interface provide an ideal platform for the site-selective modification of superhydrophobic particles. However, the need for a special chemical reaction limits their potential use for the fabrication of Janus particles with various properties. Herein, we combine the employment of liquid marbles as microreactors with the remarkable adhesive ability of polydopamine to develop a general route for the synthesis of Janus particles from micrometer-sized superhydrophobic particles. We demonstrate that dopamine polymerization and deposition inside liquid marbles could be used for the selective surface modification of microsized silica particles, resulting in the formation of Janus particles. Moreover, it is possible to manipulate the Janus balance of the particles via the addition of surfactants and/or organic solvents to tune the interfacial energy. More importantly, owing to the many functional groups in polydopamine, we show that versatile strategies could be introduced to use these partially polydopamine-coated silica particles as platforms for further modification, including nanoparticle immobilization, metal ion chelation and reduction, as well as for chemical reactions. Given the flexibility in the choice of cores and the modification strategies, this developed method is distinctive in its high universality, good controllability, and great practicability.

Bioconversion of glycerol to 1,3-propanediol in thin stillage-based media by engineered Lactobacillus panis PM1.

PubMed

Kang, Tae Sun; Korber, Darren R; Tanaka, Takuji

2014-04-01

Thin stillage (TS) is a waste residue that remains after bioethanol production, and its disposal reflects the high costs of bioethanol production. Thus, the development of cost-effective ways to process TS is a pending issue in bioethanol plants. The aim of this study was to evaluate the utilization of TS for the production of the valuable chemical, 1,3-propanediol (1,3-PDO), by Lactobacillus panis PM1. Different fermentation parameters, including temperature, pH and strains [wild-type and a recombinant strain expressing a NADPH-dependent aldehyde reductase (YqhD) gene] were tested in batch and fed-batch cultivations. The highest 1,3-PDO concentration (12.85 g/L) and yield (0.84 g/g) were achieved by batch fermentation at pH-4.5/30 °C by the YqhD recombinant strain. Furthermore, pH-controlled batch fermentation reduced the total fermentation period, resulting in the maximal 1,3-PDO concentration of 16.23 g/L and yield of 0.72 g/g in TS without an expensive nutrient or nitrogen (e.g., yeast extract, beef extract, and peptone) supplementation. The addition of two trace elements, Mg(2+) and Mn(2+), in TS increased 1,3-PDO yield (0.74 g/g) without 3-hydroxypropionaldehyde production, the only intermediate of 1,3-PDO biosynthetic pathway in L. panis PM1. Our results suggest that L. panis PM1 can offer a cost-effective process that utilizes the TS to produce a value-added chemical, 1,3-PDO.

Indigenous microbial capability in solid manure residues to start-up solid-phase anaerobic digesters.

PubMed

Yap, S D; Astals, S; Jensen, P D; Batstone, D J; Tait, S

2017-06-01

Batch solid-phase anaerobic digestion is a technology for sustainable on-farm treatment of solid residues, but is an emerging technology that is yet to be optimised with respect to start-up and inoculation. In the present study, spent bedding from two piggeries (site A and B) were batch digested at total solids (TS) concentration of 5, 10 and 20% at mesophilic (37°C) and thermophilic (55°C) temperatures, without adding an external inoculum. The results showed that the indigenous microbial community present in spent bedding was able to recover the full methane potential of the bedding (140±5 and 227±6L CH 4 kgVS fed -1 for site A and B, respectively), but longer treatment times were required than for digestion with an added external inoculum. Nonetheless, at high solid loadings (i.e. TS level>10%), the digestion performance was affected by chemical inhibition due to ammonia and/or humic acid. Thermophilic temperatures did not influence digestion performance but did increase start-up failure risk. Further, inoculation of residues from the batch digestion to subsequent batch enhanced start-up and achieved full methane potential recovery of the bedding. Inoculation with liquid residue (leachate) was preferred over a solid residue, to preserve treatment capacity for fresh substrate. Overall, the study highlighted that indigenous microbial community in the solid manure residue was capable of recovering full methane potential and that solid-phase digestion was ultimately limited by chemical inhibition rather than lack of suitable microbial community. Copyright © 2017 Elsevier Ltd. All rights reserved.

Catalytic wet-oxidation of a mixed liquid waste: COD and AOX abatement.

PubMed

Goi, D; de Leitenburg, C; Trovarelli, A; Dolcetti, G

2004-12-01

A series of catalytic wet oxidation (CWO) reactions, at temperatures of 430-500 K and in a batch bench-top pressure vessel were carried out utilizing a strong wastewater composed of landfill leachate and heavily organic halogen polluted industrial wastewater. A CeO2-SiO2 mixed oxide catalyst with large surface area to assure optimal oxidation performance was prepared. The catalytic process was examined during batch reactions controlling Chemical Oxygen Demand (COD) and Adsorbable Organic Halogen (AOX) parameters, resulting AOX abatement to achieve better effect. Color and pH were also controlled during batch tests. A simple first order-two stage reaction behavior was supposed and verified with the considered parameters. Finally an OUR test was carried out to evaluate biodegradability changes of wastewater as a result of the catalytic reaction.

Characterization Of The As-Received Sludge Batch 9 Qualification Sample (Htf-51-15-81)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pareizs, J.

Savannah River National Laboratory (SRNL) personnel have been requested to qualify the next sludge batch (Sludge Batch 9 – SB9) for processing at the Defense Waste Processing Facility (DWPF). To accomplish this task, Savannah River Remediation (SRR) has sent SRNL a 3-L slurried sample of Tank 51H (HTF-51-15-81) to be characterized, washed, and then used in a lab-scale demonstration of the DWPF flowsheet (potentially after combining with Tank 40H sludge). This report documents the first steps of the qualification process – characterization of the as-received Tank 51H qualification sample. These results will be used to support a reprojection of SB9more » by SRR from which final Tank 51H washing, frit development, and Chemical Processing Cell (CPC) activities will be based.« less

Engineered Option Treatment of Remediated Nitrate Salts: Surrogate Batch-Blending Testing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anast, Kurt Roy

2016-03-11

This report provides results from batch-blending test work for remediated nitrate salt (RNS) treatment. Batch blending was identified as a preferred option for blending RNS and unremediated nitrate salt (UNS) material with zeolite to effectively safe the salt/Swheat material identified as ignitable (U.S. Environmental Protection Agency code D001). Blending with zeolite was the preferred remediation option identified in the Options Assessment Report and was originally proposed as the best option for remediation by Clark and Funk in their report, Chemical Reactivity and Recommended Remediation Strategy for Los Alamos Remediated Nitrate Salt (RNS) Wastes, and also found to be a preferredmore » option in the Engineering Options Assessment Report: Nitrate Salt Waste Stream Processing. This test work evaluated equipment and recipe alternatives to achieve effective blending of surrogate waste with zeolite.« less

A Partially-Stirred Batch Reactor Model for Under-Ventilated Fire Dynamics

NASA Astrophysics Data System (ADS)

McDermott, Randall; Weinschenk, Craig

2013-11-01

A simple discrete quadrature method is developed for closure of the mean chemical source term in large-eddy simulations (LES) and implemented in the publicly available fire model, Fire Dynamics Simulator (FDS). The method is cast as a partially-stirred batch reactor model for each computational cell. The model has three distinct components: (1) a subgrid mixing environment, (2) a mixing model, and (3) a set of chemical rate laws. The subgrid probability density function (PDF) is described by a linear combination of Dirac delta functions with quadrature weights set to satisfy simple integral constraints for the computational cell. It is shown that under certain limiting assumptions, the present method reduces to the eddy dissipation concept (EDC). The model is used to predict carbon monoxide concentrations in direct numerical simulation (DNS) of a methane slot burner and in LES of an under-ventilated compartment fire.

GICHD mine dog testing project - soil sample results #4.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Barnett, James L.; Phelan, James M.; Archuleta, Luisa M.

2003-08-01

A mine dog evaluation project initiated by the Geneva International Center for Humanitarian Demining is evaluating the capability and reliability of mine detection dogs. The performance of field-operational mine detection dogs will be measured in test minefields in Afghanistan and Bosnia containing actual, but unfused landmines. Repeated performance testing over two years through various seasonal weather conditions will provide data simulating near real world conditions. Soil samples will be obtained adjacent to the buried targets repeatedly over the course of the test. Chemical analysis results from these soil samples will be used to evaluate correlations between mine dog detection performancemore » and seasonal weather conditions. This report documents the analytical chemical methods and results from the fourth batch of soils received. This batch contained samples from Kharga, Afghanistan collected in April 2003 and Sarajevo, Bosnia collected in May 2003.« less

Removal of mercury from an alumina refinery aqueous stream.

PubMed

Mullett, Mark; Tardio, James; Bhargava, Suresh; Dobbs, Charles

2007-06-01

Digestion condensate is formed as a by-product of the alumina refinery digestion process. The solution exhibits a high pH and is chemically reducing, containing many volatile species such as water, volatile organics, ammonia, and mercury. Because digestion condensate is chemically unique, an innovative approach was required to investigate mercury removal. The mercury capacity and adsorption kinetics were investigated using a number of materials including gold, silver and sulphur impregnated silica and a silver impregnated carbon. The results were compared to commercial sorbents, including extruded and powdered virgin activated carbons and a sulphur impregnated mineral. Nano-gold supported on silica (88% removal under batch conditions and 95% removal under flow conditions) and powdered activated carbon (91% under batch conditions and 98% removal under flow conditions) were the most effective materials investigated. The silver and sulphur impregnated materials were unstable in digestion condensate under the test conditions used.

Classification of adulterated honeys by multivariate analysis.

PubMed

Amiry, Saber; Esmaiili, Mohsen; Alizadeh, Mohammad

2017-06-01

In this research, honey samples were adulterated with date syrup (DS) and invert sugar syrup (IS) at three concentrations (7%, 15% and 30%). 102 adulterated samples were prepared in six batches with 17 replications for each batch. For each sample, 32 parameters including color indices, rheological, physical, and chemical parameters were determined. To classify the samples, based on type and concentrations of adulterant, a multivariate analysis was applied using principal component analysis (PCA) followed by a linear discriminant analysis (LDA). Then, 21 principal components (PCs) were selected in five sets. Approximately two-thirds were identified correctly using color indices (62.75%) or rheological properties (67.65%). A power discrimination was obtained using physical properties (97.06%), and the best separations were achieved using two sets of chemical properties (set 1: lactone, diastase activity, sucrose - 100%) (set 2: free acidity, HMF, ash - 95%). Copyright © 2016 Elsevier Ltd. All rights reserved.

Use of autochthonous Pediococcus acidilactici and Staphylococcus vitulus starter cultures in the production of "chorizo" in 2 different traditional industries.

PubMed

Casquete, Rocío; Benito, María J; Martín, Alberto; Ruiz-Moyano, Santiago; Aranda, Emilio; Córdoba, María G

2012-01-01

The present study determined how the different ripening conditions affected the growth and development of 3 autochthonous starter cultures, and the physico-chemical and sensory characteristics of chorizo. Each of 3 strains of Pediococcus acidilactici (MC184, MS198, and MS200) and one of Staphylococcus vitulus (RS34) were associated to prepare the starter cultures, P184S34, P198S34, and P200S34. Then, chorizo was prepared following 2 manufacturing procedures. The autochthonous starter cultures were able to compete and colonize the sausages in both ripening procedures. The use of the starter cultures showed evident differences by the texture analysis, with the control batches being generally tougher than the starter culture batches. Also, the highest biogenic amine (BA) levels were found in control batches and the lowest in P200S34 batches. While the use of these starter cultures does not change the sensory characteristics of these traditional fermented sausages, it improves their homogeneity and safety, except for P184S34 batch in which more BAs are detected in industry 2. The 3 autochthonous starter cultures selected could be used in traditional industries because they are able to compete well and colonize the dry fermented sausages "chorizo." The use of these starter cultures improves the texture and homogeneity of traditional fermented sausages. Biogenic amines decreased in the starter cultures batches improving the safety. © 2011 Institute of Food Technologists®

Characterization of tank 51 sludge samples (HTF-51-17-44/ HTF-51-17-48) in support of sludge batch 10 processing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oji, L. N.

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) Engineering (SRR-E) to provide sample characterization and analyses of Tank 51 sludge samples in support of Sludge Batch (SB) 10. The two Tank 51 sludge samples were sampled and delivered to SRNL in May of 2017. These two tank 51 sludge samples were combined into one composite sample and analyzed for corrosion controls analytes, select radionuclides, chemical elements, density and weight percent total solids and aluminum hydroxides (gibbsite and boehmite) by x-ray diffraction.

Chemical fingerprint of Ganmaoling granule by double-wavelength ultra high performance liquid chromatography and ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry.

PubMed

Lou, Qiong; Ye, Xiaolan; Zhou, Yingyi; Li, Hua; Song, Fenyun

2015-06-01

A method incorporating double-wavelength ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry was developed for the investigation of the chemical fingerprint of Ganmaoling granule. The chromatographic separations were performed on an ACQUITY UPLC HSS C18 column (2.1 × 50 mm, 1.8 μm) at 30°C using gradient elution with water/formic acid (1%) and acetonitrile at a flow rate of 0.4 mL/min. A total of 11 chemical constituents of Ganmaoling granule were identified from their molecular weight, UV spectra, tandem mass spectrometry data, and retention behavior by comparing the results with those of the reference standards or literature. And 25 peaks were selected as the common peaks for fingerprint analysis to evaluate the similarities among 25 batches of Ganmaoling granule. The results of principal component analysis and orthogonal projection to latent structures discriminant analysis showed that the important chemical markers that could distinguish the different batches were revealed as 4,5-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, and 4-O-caffeoylquinic acid. This is the first report of the ultra high performance liquid chromatography chemical fingerprint and component identification of Ganmaoling granule, which could lay a foundation for further studies of Ganmaoling granule. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Bacteriophage PRD1 batch experiments to study attachment, detachment and inactivation processes.

PubMed

Sadeghi, Gholamreza; Schijven, Jack F; Behrends, Thilo; Hassanizadeh, S Majid; van Genuchten, Martinus Th

2013-09-01

Knowledge of virus removal in subsurface environments is pivotal for assessing the risk of viral contamination of water resources and developing appropriate protection measures. Columns packed with sand are frequently used to quantify attachment, detachment and inactivation rates of viruses. Since column transport experiments are very laborious, a common alternative is to perform batch experiments where usually one or two measurements are done assuming equilibrium is reached. It is also possible to perform kinetic batch experiments. In that case, however, it is necessary to monitor changes in the concentration with time. This means that kinetic batch experiments will be almost as laborious as column experiments. Moreover, attachment and detachment rate coefficients derived from batch experiments may differ from those determined using column experiments. The aim of this study was to determine the utility of kinetic batch experiments and investigate the effects of different designs of the batch experiments on estimated attachment, detachment and inactivation rate coefficients. The experiments involved various combinations of container size, sand-water ratio, and mixing method (i.e., rolling or tumbling by pivoting the tubes around their horizontal or vertical axes, respectively). Batch experiments were conducted with clean quartz sand, water at pH 7 and ionic strength of 20 mM, and using the bacteriophage PRD1 as a model virus. Values of attachment, detachment and inactivation rate coefficients were found by fitting an analytical solution of the kinetic model equations to the data. Attachment rate coefficients were found to be systematically higher under tumbling than under rolling conditions because of better mixing and more efficient contact of phages with the surfaces of the sand grains. In both mixing methods, more sand in the container yielded higher attachment rate coefficients. A linear increase in the detachment rate coefficient was observed with increased solid-water ratio using tumbling method. Given the differences in the attachment rate coefficients, and assuming the same sticking efficiencies since chemical conditions of the batch and column experiments were the same, our results show that collision efficiencies of batch experiments are not the same as those of column experiments. Upscaling of the attachment rate from batch to column experiments hence requires proper understanding of the mixing conditions. Because batch experiments, in which the kinetics are monitored, are as laborious as column experiments, there seems to be no major advantage in performing batch instead of column experiments. Copyright © 2013 Elsevier B.V. All rights reserved.

Production of chemicals and fuels from biomass

DOEpatents

Woods, Elizabeth; Qiao, Ming; Myren, Paul; Cortright, Randy D.; Kania, John

2015-12-15

Described are methods, reactor systems, and catalysts for converting biomass to fuels and chemicals in a batch and/or continuous process. The process generally involves the conversion of water insoluble components of biomass, such as hemicellulose, cellulose and lignin, to volatile C.sub.2+O.sub.1-2 oxygenates, such as alcohols, ketones, cyclic ethers, esters, carboxylic acids, aldehydes, and mixtures thereof. In certain applications, the volatile C.sub.2+O.sub.1-2 oxygenates can be collected and used as a final chemical product, or used in downstream processes to produce liquid fuels, chemicals and other products.

Batching alternatives for Phase I retrieval wastes to be processed in WRAP Module 1

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mayancsik, B.A.

1994-10-13

During the next two decades, the transuranic (TRU) waste now stored in the 200 Area burial trenches and storage buildings is to be retrieved, processed in the Waste Receiving and Processing (WRAP) Module 1 facility, and shipped to a final disposal facility. The purpose of this document is to identify the criteria that can be used to batch suspect TRU waste, currently in retrievable storage, for processing through the WRAP Module 1 facility. These criteria are then used to generate a batch plan for Phase 1 Retrieval operations, which will retrieve the waste located in Trench 4C-04 of the 200more » West Area burial ground. The reasons for batching wastes for processing in WRAP Module 1 include reducing the exposure of workers and the environment to hazardous material and ionizing radiation; maximizing the efficiency of the retrieval, processing, and disposal processes by reducing costs, time, and space throughout the process; reducing analytical sampling and analysis; and reducing the amount of cleanup and decontamination between process runs. The criteria selected for batching the drums of retrieved waste entering WRAP Module 1 are based on the available records for the wastes sent to storage as well as knowledge of the processes that generated these wastes. The batching criteria identified in this document include the following: waste generator; type of process used to generate or package the waste; physical waste form; content of hazardous/dangerous chemicals in the waste; radiochemical type and quantity of waste; drum weight; and special waste types. These criteria were applied to the waste drums currently stored in Trench 4C-04. At least one batching scheme is shown for each of the criteria listed above.« less

Modeling Lab-sized Anaerobic Fluidized Bed Reactor (AFBR) for Palm Oil Mill Effluent (POME) treatment: from Batch to Continuous Reactors

NASA Astrophysics Data System (ADS)

Mufti Azis, Muhammad; Sudibyo, Hanifrahmawan; Budhijanto, Wiratni

2018-03-01

Indonesia is aiming to produce 30 million tones/year of crude palm oil (CPO) by 2020. As a result, 90 million tones/year of POME will be produced. POME is highly polluting wastewater which may cause severe environmental problem due to its high chemical oxygen demand (COD) and biochemical oxygen demand (BOD). Due to the limitation of open pond treatment, the use of AFBR has been considered as a potential technology to treat POME. This study aims to develop mathematical models of lab-sized Anaerobic Fluidized Bed Reactor (AFBR) in batch and continuous processes. In addition, the AFBR also utilized natural zeolite as an immobilized media for microbes. To initiate the biomass growth, biodiesel waste has been used as an inoculum. In the first part of this study, a batch AFBR was operated to evaluate the COD, VFA, and CH4 concentrations. By comparing the batch results with and without zeolite, it showed that the addition of 17 g/gSCOD zeolite gave larger COD decrease within 20 days of operation. In order to elucidate the mechanism, parameter estimations of 12 kinetic parameters were proposed to describe the batch reactor performance. The model in general could describe the batch experimental data well. In the second part of this study, the kinetic parameters obtained from batch reactor were used to simulate the performance of double column AFBR where the acidogenic and methanogenic biomass were separated. The simulation showed that a relatively long residence time (Hydraulic Residence Time, HRT) was required to treat POME using the proposed double column AFBR. Sensitivity analyses was conducted and revealed that μm1 appeared to be the most sensitive parameter to reduce the HRT of double column AFBR.

Laboratory-scale integrated ARP filter test

DOE Office of Scientific and Technical Information (OSTI.GOV)

Poirier, M.; Burket, P.

2016-03-01

The Savannah River Site (SRS) is currently treating radioactive liquid waste with the Actinide Removal Process (ARP) and the Modular Caustic Side Solvent Extraction Unit (MCU). Recently, the low filter flux through the ARP of approximately 5 gallons per minute has limited the rate at which radioactive liquid waste can be treated. Salt Batch 6 had a lower processing rate and required frequent filter cleaning. There is a desire to understand the causes of the low filter flux and to increase ARP/MCU throughput. This task attempted to simulate the entire ARP process, including multiple batches (5), washing, chemical cleaning, andmore » blending the feed with heels and recycle streams. The objective of the tests was to determine whether one of these processes is causing excessive fouling of the crossflow or secondary filter. The authors conducted the tests with feed solutions containing 6.6 M sodium Salt Batch 6 simulant supernate with no MST.« less

40 CFR 52.777 - Control strategy: photochemical oxidants (hydrocarbons).

Code of Federal Regulations, 2014 CFR

2014-07-01

... plastics, automotive plastics, and synthetic organic chemical manufacturing industries (SOCMI) batch... wastewater processes, offset lithography operations, business plastics, automotive plastics, and synthetic... order between U.S. Steel (currently USX Corporation) and the IDEM signed by IDEM on March 22, 1996...

40 CFR 52.777 - Control strategy: photochemical oxidants (hydrocarbons).

Code of Federal Regulations, 2010 CFR

2010-07-01

... plastics, automotive plastics, and synthetic organic chemical manufacturing industries (SOCMI) batch... wastewater processes, offset lithography operations, business plastics, automotive plastics, and synthetic... order between U.S. Steel (currently USX Corporation) and the IDEM signed by IDEM on March 22, 1996...

40 CFR 52.777 - Control strategy: photochemical oxidants (hydrocarbons).

Code of Federal Regulations, 2011 CFR

2011-07-01

... plastics, automotive plastics, and synthetic organic chemical manufacturing industries (SOCMI) batch... wastewater processes, offset lithography operations, business plastics, automotive plastics, and synthetic... order between U.S. Steel (currently USX Corporation) and the IDEM signed by IDEM on March 22, 1996...

Integrated continuous bioprocessing: Economic, operational, and environmental feasibility for clinical and commercial antibody manufacture.

PubMed

Pollock, James; Coffman, Jon; Ho, Sa V; Farid, Suzanne S

2017-07-01

This paper presents a systems approach to evaluating the potential of integrated continuous bioprocessing for monoclonal antibody (mAb) manufacture across a product's lifecycle from preclinical to commercial manufacture. The economic, operational, and environmental feasibility of alternative continuous manufacturing strategies were evaluated holistically using a prototype UCL decisional tool that integrated process economics, discrete-event simulation, environmental impact analysis, operational risk analysis, and multiattribute decision-making. The case study focused on comparing whole bioprocesses that used either batch, continuous or a hybrid combination of batch and continuous technologies for cell culture, capture chromatography, and polishing chromatography steps. The cost of goods per gram (COG/g), E-factor, and operational risk scores of each strategy were established across a matrix of scenarios with differing combinations of clinical development phase and company portfolio size. The tool outputs predict that the optimal strategy for early phase production and small/medium-sized companies is the integrated continuous strategy (alternating tangential flow filtration (ATF) perfusion, continuous capture, continuous polishing). However, the top ranking strategy changes for commercial production and companies with large portfolios to the hybrid strategy with fed-batch culture, continuous capture and batch polishing from a COG/g perspective. The multiattribute decision-making analysis highlighted that if the operational feasibility was considered more important than the economic benefits, the hybrid strategy would be preferred for all company scales. Further considerations outside the scope of this work include the process development costs required to adopt continuous processing. © 2017 The Authors Biotechnology Progress published by Wiley Periodicals, Inc. on behalf of American Institute of Chemical Engineers Biotechnol. Prog., 33:854-866, 2017. © 2017 The Authors Biotechnology Progress published by Wiley Periodicals, Inc. on behalf of American Institute of Chemical Engineers.

Validation of reference and identity-defining genes in human mesenchymal stem cells cultured under unrelated fetal bovine serum batches for basic science and clinical application.

PubMed

Banfi, Federica; Colombini, Alessandra; Perucca Orfei, Carlotta; Parazzi, Valentina; Ragni, Enrico

2018-05-26

The molecular profile of human mesenchymal stem cells (MSCs) have emerged as a key factor in defining their identity. Nevertheless, the effect of fetal bovine serum (FBS) batches or origin on MSC molecular signature has been neglected. In this frame, chemical fingerprint of FBS batches from unrelated countries showed strong correlation between chemical composition and country of origin. Thus, the aim of this study was to evaluate in stem cells isolated from bone marrow (BMMSCs) and umbilical cord-blood (CBMSCs) the effects of independently collected FBS batches on both twelve commonly used reference genes (RGs) and a selected panel of thirty-eight genes crucial for MSC definition in both research and clinical settings. Gene expression stability was estimated comparing the outcomes of two applets: geNorm and NormFinder. The bioinformatics analysis emphasized that, in a panorama of general balance, few RG candidates (YWHAZ/UBC for BMMSCs, RPLP0/EF1A for CBMSCs and EF1A/TBP for both MSCs scored together) showed superior stability. In addition, a wider study on genes involved in differentiation/proliferation/stemness processes, often used to define MSC potency, showed that these genes exhibited no major transcriptional modulation after treatment with different FBS, and allowed the identification of genes strongly discriminating between BM- and CBMSC populations. Therefore, in conclusion, FBS origin does not dramatically impact the general molecular profile of MSCs, although we could identify validated candidates able to allow more reliable comparison of data regarding MSC identity and potency and obtained by research laboratories and clinical manufacturers using different sera.

Recommendation of ruthenium source for sludge batch flowsheet studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Woodham, W.

Included herein is a preliminary analysis of previously-generated data from sludge batches 7a, 7b, 8, and 9 sludge simulant and real-waste testing, performed to recommend a form of ruthenium for future sludge batch simulant testing under the nitric-formic flowsheet. Focus is given to reactions present in the Sludge Receipt and Adjustment Tank cycle, given that this cycle historically produces the most changes in chemical composition during Chemical Process Cell processing. Data is presented and analyzed for several runs performed under the nitric-formic flowsheet, with consideration given to effects on the production of hydrogen gas, nitrous oxide gas, consumption of formate,more » conversion of nitrite to nitrate, and the removal and recovery of mercury during processing. Additionally, a brief discussion is given to the effect of ruthenium source selection under the nitric-glycolic flowsheet. An analysis of data generated from scaled demonstration testing, sludge batch 9 qualification testing, and antifoam degradation testing under the nitric-glycolic flowsheet is presented. Experimental parameters of interest under the nitric-glycolic flowsheet include N2O production, glycolate destruction, conversion of glycolate to formate and oxalate, and the conversion of nitrite to nitrate. To date, the number of real-waste experiments that have been performed under the nitric-glycolic flowsheet is insufficient to provide a complete understanding of the effects of ruthenium source selection in simulant experiments with regard to fidelity to real-waste testing. Therefore, a determination of comparability between the two ruthenium sources as employed under the nitric-glycolic flowsheet is made based on available data in order to inform ruthenium source selection for future testing under the nitric-glycolic flowsheet.« less

Study of aniline polymerization reactions through the particle size formation in acidic and neutral medium

NASA Astrophysics Data System (ADS)

Aribowo, Slamet; Hafizah, Mas Ayu Elita; Manaf, Azwar; Andreas

2018-04-01

In the present paper, we reported particle size kinetic studies on the conducting polyaniline (PANI) which synthesized through a chemical oxidative polymerization technique from aniline monomer. PANI was prepared using ammonium persulfate (APS) as oxidizing agent which carried out in acidic and neutral medium at various batch temperatures of respectively 20, 30 and 50 °C. From the studies, it was noticed that the complete polymerization reaction progressed within 480 minutes duration time. The pH of the solution during reaction kinetic reached values 0.8 - to 1.2 in acidic media, while in the neutral media the pH value reached values 3.8 - 4.9. The batch temperature controlled the polymerization reaction in which the reaction progressing, which followed by the temperature rise of solution above the batch temperature before settled down to the initial temperature. An increment in the batch temperature gave highest rise in the solution temperature for the two media which cannot be more than 50 °C. The final product of polymerization reaction was PANI confirmed by Fourier Transform Infra-Red (FTIR) spectrophotometer for molecule structure identification. The averages particle size of PANI which carried out in the two different media is evidently similar in the range 30 - 40 μm and insensitive to the batch temperature. However, the particle size of PANI which obtained from the polymerization reaction at a batch temperature of 50 °C under acidic condition reached ˜53.1 μm at the tip of the propagation stage which started in the first 5 minutes. The size is obviously being the largest among the batch temperatures. Whereas, under neutral condition the particle size is much larger which reached the size 135 μm at the batch temperature of 20 °C. It is concluded that the particle size formation during the polymerization reaction being one of the important parameter to determine particle growing of polymer which indicated the reaction kinetics mechanism of synthesize polyaniline.

A review of the theory, methods and recent applications of high-throughput single-cell droplet microfluidics

NASA Astrophysics Data System (ADS)

Lagus, Todd P.; Edd, Jon F.

2013-03-01

Most cell biology experiments are performed in bulk cell suspensions where cell secretions become diluted and mixed in a contiguous sample. Confinement of single cells to small, picoliter-sized droplets within a continuous phase of oil provides chemical isolation of each cell, creating individual microreactors where rare cell qualities are highlighted and otherwise undetectable signals can be concentrated to measurable levels. Recent work in microfluidics has yielded methods for the encapsulation of cells in aqueous droplets and hydrogels at kilohertz rates, creating the potential for millions of parallel single-cell experiments. However, commercial applications of high-throughput microdroplet generation and downstream sensing and actuation methods are still emerging for cells. Using fluorescence-activated cell sorting (FACS) as a benchmark for commercially available high-throughput screening, this focused review discusses the fluid physics of droplet formation, methods for cell encapsulation in liquids and hydrogels, sensors and actuators and notable biological applications of high-throughput single-cell droplet microfluidics.

Morphological computation and morphological control: steps toward a formal theory and applications.

PubMed

Füchslin, Rudolf M; Dzyakanchuk, Andrej; Flumini, Dandolo; Hauser, Helmut; Hunt, Kenneth J; Luchsinger, Rolf H; Reller, Benedikt; Scheidegger, Stephan; Walker, Richard

2013-01-01

Morphological computation can be loosely defined as the exploitation of the shape, material properties, and physical dynamics of a physical system to improve the efficiency of a computation. Morphological control is the application of morphological computing to a control task. In its theoretical part, this article sharpens and extends these definitions by suggesting new formalized definitions and identifying areas in which the definitions we propose are still inadequate. We go on to describe three ongoing studies, in which we are applying morphological control to problems in medicine and in chemistry. The first involves an inflatable support system for patients with impaired movement, and is based on macroscopic physics and concepts already tested in robotics. The two other case studies (self-assembly of chemical microreactors; models of induced cell repair in radio-oncology) describe processes and devices on the micrometer scale, in which the emergent dynamics of the underlying physical system (e.g., phase transitions) are dominated by stochastic processes such as diffusion.

Pyrogenic transformation of Nannochloropsis oceanica into fatty acid methyl esters without oil extraction for estimating total lipid content.

PubMed

Kim, Jieun; Jung, Jong-Min; Lee, Jechan; Kim, Ki-Hyun; Choi, Tae O; Kim, Jae-Kon; Jeon, Young Jae; Kwon, Eilhann E

2016-07-01

This study fundamentally investigated the pseudo-catalytic transesterification of dried Nannochloropsis oceanica into fatty acid methyl esters (FAMEs) without oil extraction, which was achieved in less than 5min via a thermo-chemical pathway. This study presented that the pseudo-catalytic transesterification reaction was achieved in the presence of silica and that its main driving force was identified as temperature: pores in silica provided the numerous reaction space like a micro-reactor, where the heterogeneous reaction was developed. The introduced FAME derivatization showed an extraordinarily high tolerance of impurities (i.e., pyrolytic products and various extractives). This study also explored the thermal cracking of FAMEs derived from N. oceanica: the thermal cracking of saturated FAMEs was invulnerable at temperatures lower than 400°C. Lastly, this study reported that N. oceanica contained 14.4wt.% of dried N. oceanica and that the introduced methylation technique could be applicable to many research fields sharing the transesterification platform. Copyright © 2016 Elsevier Ltd. All rights reserved.

Ceramic Spheres From Cation Exchange Beads

NASA Technical Reports Server (NTRS)

Dynys, F. W.

2003-01-01

Porous ZrO2 and hollow TiO2 spheres were synthesized from a strong acid cation exchange resin. Spherical cation exchange beads, polystyrene based polymer, were used as a morphological-directing template. Aqueous ion exchange reaction was used to chemically bind (ZrO)(2+) ions to the polystyrene structure. The pyrolysis of the polystyrene at 600 C produces porous ZrO2 spheres with a surface area of 24 sq m/g with a mean sphere size of 42 microns. Hollow TiO2 spheres were synthesized by using the beads as a micro-reactor. A direct surface reaction - between titanium isopropoxide and the resin beads forms a hydrous TiO2 shell around the polystyrene core. The pyrolysis of the polystyrene core at 600 C produces hollow anatase spheres with a surface area of 42 sq m/g with a mean sphere size of 38 microns. The formation of ceramic spheres was studied by XRD, SEM and B.E.T. nitrogen adsorption measurements.

Liquid Marble Coalescence and Triggered Microreaction Driven by Acoustic Levitation.

PubMed

Chen, Zhen; Zang, Duyang; Zhao, Liang; Qu, Mengfei; Li, Xu; Li, Xiaoguang; Li, Lixin; Geng, Xingguo

2017-06-27

Liquid marbles show promising potential for application in the microreactor field. Control of the coalescence between two or among multiple liquid marbles is critical; however, the successful merging of two isolated marbles is difficult because of their mechanically robust particle shells. In this work, the coalescence of multiple liquid marbles was achieved via acoustic levitation. The dynamic behaviors of the liquid marbles were monitored by a high-speed camera. Driven by the sound field, the liquid marbles moved toward each other, collided, and eventually coalesced into a larger single marble. The underlying mechanisms of this process were probed via sound field simulation and acoustic radiation pressure calculation. The results indicated that the pressure gradient on the liquid marble surface favors the formation of a liquid bridge between the liquid marbles, resulting in their coalescence. A preliminary indicator reaction was induced by the coalescence of dual liquid marbles, which suggests that expected chemical reactions can be successfully triggered with multiple reagents contained in isolated liquid marbles via acoustic levitation.

Droplets Formation and Merging in Two-Phase Flow Microfluidics

PubMed Central

Gu, Hao; Duits, Michel H. G.; Mugele, Frieder

2011-01-01

Two-phase flow microfluidics is emerging as a popular technology for a wide range of applications involving high throughput such as encapsulation, chemical synthesis and biochemical assays. Within this platform, the formation and merging of droplets inside an immiscible carrier fluid are two key procedures: (i) the emulsification step should lead to a very well controlled drop size (distribution); and (ii) the use of droplet as micro-reactors requires a reliable merging. A novel trend within this field is the use of additional active means of control besides the commonly used hydrodynamic manipulation. Electric fields are especially suitable for this, due to quantitative control over the amplitude and time dependence of the signals, and the flexibility in designing micro-electrode geometries. With this, the formation and merging of droplets can be achieved on-demand and with high precision. In this review on two-phase flow microfluidics, particular emphasis is given on these aspects. Also recent innovations in microfabrication technologies used for this purpose will be discussed. PMID:21731459

The thermal decomposition of the benzyl radical in a heated micro-reactor. II. Pyrolysis of the tropyl radical

NASA Astrophysics Data System (ADS)

Buckingham, Grant T.; Porterfield, Jessica P.; Kostko, Oleg; Troy, Tyler P.; Ahmed, Musahid; Robichaud, David J.; Nimlos, Mark R.; Daily, John W.; Ellison, G. Barney

2016-07-01

Cycloheptatrienyl (tropyl) radical, C7H7, was cleanly produced in the gas-phase, entrained in He or Ne carrier gas, and subjected to a set of flash-pyrolysis micro-reactors. The pyrolysis products resulting from C7H7 were detected and identified by vacuum ultraviolet photoionization mass spectrometry. Complementary product identification was provided by infrared absorption spectroscopy. Pyrolysis pressures in the micro-reactor were roughly 200 Torr and residence times were approximately 100 μs. Thermal cracking of tropyl radical begins at 1100 K and the products from pyrolysis of C7H7 are only acetylene and cyclopentadienyl radicals. Tropyl radicals do not isomerize to benzyl radicals at reactor temperatures up to 1600 K. Heating samples of either cycloheptatriene or norbornadiene never produced tropyl (C7H7) radicals but rather only benzyl (C6H5CH2). The thermal decomposition of benzyl radicals has been reconsidered without participation of tropyl radicals. There are at least three distinct pathways for pyrolysis of benzyl radical: the Benson fragmentation, the methyl-phenyl radical, and the bridgehead norbornadienyl radical. These three pathways account for the majority of the products detected following pyrolysis of all of the isotopomers: C6H5CH2, C6H5CD2, C6D5CH2, and C6H513CH2. Analysis of the temperature dependence for the pyrolysis of the isotopic species (C6H5CD2, C6D5CH2, and C6H513CH2) suggests the Benson fragmentation and the norbornadienyl pathways open at reactor temperatures of 1300 K while the methyl-phenyl radical channel becomes active at slightly higher temperatures (1500 K).

The thermal decomposition of the benzyl radical in a heated micro-reactor. II. Pyrolysis of the tropyl radical

DOE Office of Scientific and Technical Information (OSTI.GOV)

Buckingham, Grant T.; Porterfield, Jessica P.; Kostko, Oleg

2016-07-05

Cycloheptatrienyl (tropyl) radical, C7H7, was cleanly produced in the gas-phase, entrained in He or Ne carrier gas, and subjected to a set of flash-pyrolysis micro-reactors. The pyrolysis products resulting from C7H7 were detected and identified by vacuum ultraviolet photoionization mass spectrometry. Complementary product identification was provided by infrared absorption spectroscopy. Pyrolysis pressures in the micro-reactor were roughly 200 Torr and residence times were approximately 100 us. Thermal cracking of tropyl radical begins at 1100 K and the products from pyrolysis of C7H7 are only acetylene and cyclopentadienyl radicals. Tropyl radicals do not isomerize to benzyl radicals at reactor temperatures upmore » to 1600 K. Heating samples of either cycloheptatriene or norbornadiene never produced tropyl (C7H7) radicals but rather only benzyl (C6H5CH2). The thermal decomposition of benzyl radicals has been reconsidered without participation of tropyl radicals. There are at least three distinct pathways for pyrolysis of benzyl radical: the Benson fragmentation, the methyl-phenyl radical, and the bridgehead norbornadienyl radical. These three pathways account for the majority of the products detected following pyrolysis of all of the isotopomers: C6H5CH2, C6H5CD2, C6D5CH2, and C6H5 13CH2. Analysis of the temperature dependence for the pyrolysis of the isotopic species (C6H5CD2, C6D5CH2, and C6H5 13CH2) suggests the Benson fragmentation and the norbornadienyl pathways open at reactor temperatures of 1300 K while the methyl-phenyl radical channel becomes active at slightly higher temperatures (1500 K).« less

Bioelectrochemical conversion of CO2 to chemicals: CO2 as a next generation feedstock for electricity-driven bioproduction in batch and continuous modes.

PubMed

Bajracharya, Suman; Vanbroekhoven, Karolien; Buisman, Cees J N; Strik, David P B T B; Pant, Deepak

2017-09-21

The recent concept of microbial electrosynthesis (MES) has evolved as an electricity-driven production technology for chemicals from low-value carbon dioxide (CO 2 ) using micro-organisms as biocatalysts. MES from CO 2 comprises bioelectrochemical reduction of CO 2 to multi-carbon organic compounds using the reducing equivalents produced at the electrically-polarized cathode. The use of CO 2 as a feedstock for chemicals is gaining much attention, since CO 2 is abundantly available and its use is independent of the food supply chain. MES based on CO 2 reduction produces acetate as a primary product. In order to elucidate the performance of the bioelectrochemical CO 2 reduction process using different operation modes (batch vs. continuous), an investigation was carried out using a MES system with a flow-through biocathode supplied with 20 : 80 (v/v) or 80 : 20 (v/v) CO 2  : N 2 gas. The highest acetate production rate of 149 mg L -1 d -1 was observed with a 3.1 V applied cell-voltage under batch mode. While running in continuous mode, high acetate production was achieved with a maximum rate of 100 mg L -1 d -1 . In the continuous mode, the acetate production was not sustained over long-term operation, likely due to insufficient microbial biocatalyst retention within the biocathode compartment (i.e. suspended micro-organisms were washed out of the system). Restarting batch mode operations resulted in a renewed production of acetate. This showed an apparent domination of suspended biocatalysts over the attached (biofilm forming) biocatalysts. Long term CO 2 reduction at the biocathode resulted in the accumulation of acetate, and more reduced compounds like ethanol and butyrate were also formed. Improvements in the production rate and different biomass retention strategies (e.g. selecting for biofilm forming micro-organisms) should be investigated to enable continuous biochemical production from CO 2 using MES. Certainly, other process optimizations will be required to establish MES as an innovative sustainable technology for manufacturing biochemicals from CO 2 as a next generation feedstock.

Modeling of the pyruvate production with Escherichia coli: comparison of mechanistic and neural networks-based models.

PubMed

Zelić, B; Bolf, N; Vasić-Racki, D

2006-06-01

Three different models: the unstructured mechanistic black-box model, the input-output neural network-based model and the externally recurrent neural network model were used to describe the pyruvate production process from glucose and acetate using the genetically modified Escherichia coli YYC202 ldhA::Kan strain. The experimental data were used from the recently described batch and fed-batch experiments [ Zelić B, Study of the process development for Escherichia coli-based pyruvate production. PhD Thesis, University of Zagreb, Faculty of Chemical Engineering and Technology, Zagreb, Croatia, July 2003. (In English); Zelić et al. Bioproc Biosyst Eng 26:249-258 (2004); Zelić et al. Eng Life Sci 3:299-305 (2003); Zelić et al Biotechnol Bioeng 85:638-646 (2004)]. The neural networks were built out of the experimental data obtained in the fed-batch pyruvate production experiments with the constant glucose feed rate. The model validation was performed using the experimental results obtained from the batch and fed-batch pyruvate production experiments with the constant acetate feed rate. Dynamics of the substrate and product concentration changes was estimated using two neural network-based models for biomass and pyruvate. It was shown that neural networks could be used for the modeling of complex microbial fermentation processes, even in conditions in which mechanistic unstructured models cannot be applied.

Acceptance Test Data for BWXT Coated Particle Batch 93164A Defective IPyC Fraction and Pyrocarbon Anisotropy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Helmreich, Grant W.; Hunn, John D.; Skitt, Darren J.

2017-02-01

Coated particle fuel batch J52O-16-93164 was produced by Babcock and Wilcox Technologies (BWXT) for possible selection as fuel for the Advanced Gas Reactor Fuel Development and Qualification (AGR) Program’s AGR-5/6/7 irradiation test in the Idaho National Laboratory (INL) Advanced Test Reactor (ATR), or may be used as demonstration production-scale coated particle fuel for other experiments. The tristructural-isotropic (TRISO) coatings were deposited in a 150-mm-diameter production-scale fluidizedbed chemical vapor deposition (CVD) furnace onto 425-μm-nominal-diameter spherical kernels from BWXT lot J52L-16-69316. Each kernel contained a mixture of 15.5%-enriched uranium carbide and uranium oxide (UCO) and was coated with four consecutive CVD layers:more » a ~50% dense carbon buffer layer with 100-μm-nominal thickness, a dense inner pyrolytic carbon (IPyC) layer with 40-μm-nominal thickness, a silicon carbide (SiC) layer with 35-μm-nominal thickness, and a dense outer pyrolytic carbon (OPyC) layer with 40-μm-nominal thickness. The TRISO-coated particle batch was sieved to upgrade the particles by removing over-sized and under-sized material, and the upgraded batch was designated by appending the letter A to the end of the batch number (i.e., 93164A).« less

Microstructure and Tensile Properties of BN/SiC Coated Hi-Nicalon, and Sylramic SiC Fiber Preforms

NASA Technical Reports Server (NTRS)

Bhatt, Ramakrishna T.; Chen, Yuan L.; Morscher, Gregory N.

2001-01-01

Batch to batch and within batch variations, and the influence of fiber architecture on room temperature physical and tensile properties of BN/SiC coated Hi-Nicalon and Sylramic SiC fiber preform specimens were determined. The three fiber architectures studied were plain weave (PW), 5-harness satin (5HS) and 8-harness satin (8HS) Results indicate that the physical properties vary up to 10 percent within a batch, and up to 20 percent between batches of preforms. Load-reload (Hysteresis) and acoustic emission methods were used to analyze damage accumulation occurring during tensile loading. Early acoustic emission activity, before observable hysteretic behavior, indicates that the damage starts with the formation of nonbridged tunnel cracks. These cracks then propagate and intersect the load bearing "0" fibers giving rise to hysteretic behavior, For the Hi-Nicalon preform specimens, the onset of "0" bundle cracking stress and strain appeared to be independent of the fiber architecture. Also, the "0" fiber bundle cracking strain remained nearly the same for the preform specimens of both fiber types. Transmission Electron Microscope (TEM) analysis indicates that the Chemical Vapor Infiltration (CVI) Boron Nitride (BN) interface coating is mostly amorphous and contains carbon and oxygen impurities, and the CVI SiC coating is crystalline. No reaction exists between the CVI BN and SiC coating.

PROCESS INTENSIFICATION: OXIDATION OF BENZYL ALCOHOL USING A CONTINUOUS ISOTHERMAL REACTOR UNDER MICROWAVE IRRADIATION

EPA Science Inventory

In the past two decades, several investigations have been carried out using microwave radiation for performing chemical transformations. These transformations have been largely performed in conventional batch reactors with limited mixing and heat transfer capabilities. The reacti...

COSOLVENT EFFECTS ON SORPTION AND MOBILITY OF ORGANIC CONTAMINANTS IN SOILS

EPA Science Inventory

Batch equilibrium and column miscible displacement techniques were used to investigate the influence of an organic cosolvent (methanol) on the sorption and transport of three hydrophobic organic chemicals (HOCs) — naphthalene, phenanthrene, and diuron herbicide — in a sandy surfa...

40 CFR 792.3 - Definitions.

Code of Federal Regulations, 2014 CFR

2014-07-01

... Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT (CONTINUED... following terms shall have the meanings specified: Batch means a specific quantity or lot of a test, control... substance is combined for administration to a test system. Control substance means any chemical substance or...

40 CFR 792.3 - Definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT (CONTINUED... following terms shall have the meanings specified: Batch means a specific quantity or lot of a test, control... substance is combined for administration to a test system. Control substance means any chemical substance or...

40 CFR 792.3 - Definitions.

Code of Federal Regulations, 2013 CFR

2013-07-01

... Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT (CONTINUED... following terms shall have the meanings specified: Batch means a specific quantity or lot of a test, control... substance is combined for administration to a test system. Control substance means any chemical substance or...

40 CFR 792.3 - Definitions.

Code of Federal Regulations, 2011 CFR

2011-07-01

... Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT (CONTINUED... following terms shall have the meanings specified: Batch means a specific quantity or lot of a test, control... substance is combined for administration to a test system. Control substance means any chemical substance or...

40 CFR 792.3 - Definitions.

Code of Federal Regulations, 2012 CFR

2012-07-01

... Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT (CONTINUED... following terms shall have the meanings specified: Batch means a specific quantity or lot of a test, control... substance is combined for administration to a test system. Control substance means any chemical substance or...

X-ray Analysis of Defects and Anomalies in AGR-5/6/7 TRISO Particles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Helmreich, Grant W.; Hunn, John D.; Skitt, Darren J.

2017-06-01

Coated particle fuel batches J52O-16-93164, 93165, 93166, 93168, 93169, 93170, and 93172 were produced by Babcock and Wilcox Technologies (BWXT) for possible selection as fuel for the Advanced Gas Reactor Fuel Development and Qualification (AGR) Program’s AGR-5/6/7 irradiation test in the Idaho National Laboratory (INL) Advanced Test Reactor (ATR), or may be used for other tests. Each batch was coated in a 150-mm-diameter production-scale fluidized-bed chemical vapor deposition (CVD) furnace. Tristructural isotropic (TRISO) coatings were deposited on 425-μm-nominal-diameter spherical kernels from BWXT lot J52R-16-69317 containing a mixture of 15.4%-enriched uranium carbide and uranium oxide (UCO), with the exception of Batchmore » 93164, which used similar kernels from BWXT lot J52L-16-69316. The TRISO-coatings consisted of a ~50% dense carbon buffer layer with 100-μmnominal thickness, a dense inner pyrolytic carbon (IPyC) layer with 40-μm-nominal thickness, a silicon carbide (SiC) layer with 35-μm-nominal thickness, and a dense outer pyrolytic carbon (OPyC) layer with 40-μm-nominal thickness. Each coated particle batch was sieved to upgrade the particles by removing over-sized and under-sized material, and the upgraded batch was designated by appending the letter A to the end of the batch number (e.g., 93164A). Secondary upgrading by sieving was performed on the upgraded batches to remove specific anomalies identified during analysis for Defective IPyC, and the upgraded batches were designated by appending the letter B to the end of the batch number (e.g., 93165B). Following this secondary upgrading, coated particle composite J52R-16-98005 was produced by BWXT as fuel for the AGR Program’s AGR-5/6/7 irradiation test in the INL ATR. This composite was comprised of coated particle fuel batches J52O-16-93165B, 93168B, 93169B, and 93170B.« less

Preparation of wafer-level glass cavities by a low-cost chemical foaming process (CFP).

PubMed

Shang, Jintang; Chen, Boyin; Lin, Wei; Wong, Ching-Ping; Zhang, Di; Xu, Chao; Liu, Junwen; Huang, Qing-An

2011-04-21

A novel foaming process-chemical foaming process (CFP)-using foaming agents to fabricate wafer-level micro glass cavities including channels and bubbles was investigated. The process consists of the following steps sequentially: (1) shallow cavities were fabricated by a wet etching on a silicon wafer; (2) powders of a proper foaming agent were placed in a silicon cavity, named 'mother cavity', on the etched silicon surface; (3) the silicon cavities were sealed with a glass wafer by anodic bonding; (4) the bonded wafers were heated to above the softening point of the glass, and baked for several minutes, when the gas released by the decomposition of the foaming agent in the 'mother cavity' went into the other sealed interconnected silicon cavities to foam the softened glass into cylindrical channels named 'daughter channels', or spherical bubbles named 'son bubbles'. Results showed that wafer-level micro glass cavities with smooth wall surfaces were achieved successfully without contamination by the CFP. A model for the CFP was proposed to predict the final shape of the glass cavity. Experimental results corresponded with model predictions. The CFP provides a low-cost avenue to preparation of micro glass cavities of high quality for applications such as micro-reactors, micro total analysis systems (μTAS), analytical and bio-analytical applications, and MEMS packaging.

Selective self-assembly of adenine-silver nanoparticles forms rings resembling the size of cells

PubMed Central

Choi, Sungmoon; Park, Soonyoung; Yang, Seon-Ah; Jeong, Yujin; Yu, Junhua

2015-01-01

Self-assembly has played critical roles in the construction of functional nanomaterials. However, the structure of the macroscale multicomponent materials built by the self-assembly of nanoscale building blocks is hard to predict due to multiple intermolecular interactions of great complexity. Evaporation of solvents is usually an important approach to induce kinetically stable assemblies of building blocks with a large-scale specific arrangement. During such a deweting process, we tried to monitor the possible interactions between silver nanoparticles and nucleobases at a larger scale by epifluorescence microscopy, thanks to the doping of silver nanoparticles with luminescent silver nanodots. ssDNA oligomer-stabilized silver nanoparticles and adenine self-assemble to form ring-like compartments similar to the size of modern cells. However, the silver ions only dismantle the self-assembly of adenine. The rings are thermodynamically stable as the drying process only enrich the nanoparticles-nucleobase mixture to a concentration that activates the self-assembly. The permeable membrane-like edge of the ring is composed of adenine filaments glued together by silver nanoparticles. Interestingly, chemicals are partially confined and accumulated inside the ring, suggesting that this might be used as a microreactor to speed up chemical reactions during a dewetting process. PMID:26643504

Online quench-flow electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry for elucidating kinetic and chemical enzymatic reaction mechanisms.

PubMed

Clarke, David J; Stokes, Adam A; Langridge-Smith, Pat; Mackay, C Logan

2010-03-01

We have developed an automated quench-flow microreactor which interfaces directly to an electrospray ionization (ESI) mass spectrometer. We have used this device in conjunction with ESI Fourier transform ion cyclotron resonance mass spectrometry (FTICR MS) to demonstrate the potential of this approach for studying the mechanistic details of enzyme reactions. For the model system chosen to test this device, namely, the pre-steady-state hydrolysis of p-nitrophenyl acetate by the enzyme chymotrypsin, the kinetic parameters obtained are in good agreement with those in the literature. To our knowledge, this is the first reported use of online quench-flow coupled with FTICR MS. Furthermore, we have exploited the power of FTICR MS to interrogate the quenched covalently bound enzyme intermediate using top-down fragmentation. The accurate mass capabilities of FTICR MS permitted the nature of the intermediate to be assigned with high confidence. Electron capture dissociation (ECD) fragmentation allowed us to locate the intermediate to a five amino acid section of the protein--which includes the known catalytic residue, Ser(195). This experimental approach, which uniquely can provide both kinetic and chemical details of enzyme mechanisms, is a potentially powerful tool for studies of enzyme catalysis.

Physical and chemical microstructural damage in pressed CL-20 explosives

NASA Astrophysics Data System (ADS)

Demol, Gauthier; Sandusky, Harold W.

2000-04-01

The ultimate utility of CL-20 as an ingredient in explosive and propellant formulations will depend upon the ability to understand the factors that are responsible for batch-to-batch variability with respect to sensitivity, and also to control the sensitivity in formulations within acceptable limits. We used light microscopy of cold-mounted, polished samples to characterize CL-20 at various stages in its life cycle. The evolution of damage from the initial neat crystals of CL-20 to the ready-to-use pressed pellets shows that processing seriously damages the crystals. These crystals are very brittle, and several explanations are proposed.

The application of a monolithic triphenylphosphine reagent for conducting Appel reactions in flow microreactors.

PubMed

Roper, Kimberley A; Lange, Heiko; Polyzos, Anastasios; Berry, Malcolm B; Baxendale, Ian R; Ley, Steven V

2011-01-01

Herein we describe the application of a monolithic triphenylphosphine reagent to the Appel reaction in flow-chemistry processing, to generate various brominated products with high purity and in excellent yields, and with no requirement for further off-line purification.

A replaceable microreactor for on-line protein digestion in a two-dimensional capillary electrophoresis system with tandem mass spectrometry detection

PubMed Central

Li, Yihan; Wojcik, Roza; Dovichi, Norman J.

2010-01-01

We describe a two-dimensional capillary electrophoresis system that incorporates a replaceable enzymatic microreactor for on-line protein digestion. In this system, trypsin is immobilized on magnetic beads. At the start of each experiment, old beads are flushed to waste and replaced with a fresh plug of beads, which is captured by a pair of magnets at the distal tip of the first capillary. For analysis, proteins are separated in the first capillary. A fraction is then parked in the reactor to create peptides. Digested peptides are periodically transferred to the second capillary for separation; a fresh protein fraction is simultaneously moved to the reactor for digestion. An electrospray interface is used to introduce peptides into a mass spectrometer for analysis. This procedure is repeated for several dozen fractions under computer control. The system was demonstrated by the separation and digestion of insulin chain b oxidized and β-casein as model proteins. PMID:21030030

Catechol Removal from Aqueous Media Using Laccase Immobilized in Different Macro- and Microreactor Systems.

PubMed

Tušek, Ana Jurinjak; Šalić, Anita; Zelić, Bruno

2017-08-01

Laccase belongs to the group of enzymes that are capable to catalyze the oxidation of phenols. Since the water is only by-product in laccase-catalyzed phenol oxidations, it is ideally "green" enzyme with many possible applications in different industrial processes. To make the oxidation process more sustainable in terms of biocatalyst consumption, immobilization of the enzyme is implemented in to the processes. Additionally, when developing a process, choice of a reactor type plays a significant role in the total outcome.In this study, the use of immobilized laccase from Trametes versicolor for biocatalytic catechol oxidation was explored. Two different methods of immobilization were performed and compared using five different reactor types. In order to compare different systems used for catechol oxidation, biocatalyst turnover number and turnover frequency were calculated. With low consumption of the enzyme and good efficiency, obtained results go in favor of microreactors with enzyme covalently immobilized on the microchannel surface.

Continuous, size and shape-control synthesis of hollow silica nanoparticles enabled by a microreactor-assisted rapid mixing process.

PubMed

He, Yujuan; Kim, Ki-Joong; Chang, Chih-Hung

2017-06-09

Hollow silica nanoparticles (HSNPs) were synthesized using a microreactor-assisted system with a hydrodynamic focusing micromixer. Due to the fast mixing of each precursor in the system, the poly(acrylic acid) (PAA) thermodynamic-locked (TML) conformations were protected from their random aggregations by the immediately initiated growth of silica shells. When altering the mixing time through varying flow rates and flow rate ratios, the different degrees of the aggregation of PAA TML conformations were observed. The globular and necklace-like TML conformations were successfully captured by modifying the PAA concentration at the optimized mixing condition. Uniform HSNPs with an average diameter ∼30 nm were produced from this system. COMSOL numerical models was established to investigate the flow and concentration profiles, and their effects on the formation of PAA templates. Finally, the quality and utility of these uniform HSNPs were demonstrated by the fabrication of antireflective thin films on monocrystalline photovoltaic cells which showed a 3.8% increase in power conversion efficiency.

Stromalized microreactor supports murine hematopoietic progenitor enrichment.

PubMed

Khong, Danika; Li, Matthew; Singleton, Amy; Chin, Ling-Yee; Parekkadan, Biju

2018-01-20

There is an emerging need to process, expand, and even genetically engineer hematopoietic stem and progenitor cells (HSPCs) prior to administration for blood reconstitution therapy. A closed-system and automated solution for ex vivo HSC processing can improve adoption and standardize processing techniques. Here, we report a recirculating flow bioreactor where HSCs are stabilized and enriched for short-term processing by indirect fibroblast feeder coculture. Mouse 3 T3 fibroblasts were seeded on the extraluminal membrane surface of a hollow fiber micro-bioreactor and were found to support HSPC cell number compared to unsupported BMCs. CFSE analysis indicates that 3 T3-support was essential for the enhanced intrinsic cell cycling of HSPCs. This enhanced support was specific to the HSPC population with little to no effect seen with the Lineage positive and Lineage negative cells. Together, these data suggest that stromal-seeded hollow fiber micro-reactors represent a platform to screening various conditions that support the expansion and bioprocessing of HSPCs ex vivo.

Mimicking Insect Communication: Release and Detection of Pheromone, Biosynthesized by an Alcohol Acetyl Transferase Immobilized in a Microreactor

PubMed Central

Muñoz, Lourdes; Dimov, Nikolay; Carot-Sans, Gerard; Bula, Wojciech P.; Guerrero, Angel; Gardeniers, Han J. G. E.

2012-01-01

Infochemical production, release and detection of (Z,E)-9,11-tetradecadienyl acetate, the major component of the pheromone of the moth Spodoptera littoralis, is achieved in a novel microfluidic system designed to mimic the final step of the pheromone biosynthesis by immobilized recombinant alcohol acetyl transferase. The microfluidic system is part of an “artificial gland”, i.e., a chemoemitter that comprises a microreactor connected to a microevaporator and is able to produce and release a pre-defined amount of the major component of the pheromone from the corresponding (Z,E)-9,11-tetradecadienol. Performance of the entire chemoemitter has been assessed in electrophysiological and behavioral experiments. Electroantennographic depolarizations of the pheromone produced by the chemoemitter were ca. 40% relative to that evoked by the synthetic pheromone. In a wind tunnel, the pheromone released from the evaporator elicited on males a similar attraction behavior as 3 virgin females in most of the parameters considered. PMID:23155372

Diamondoid synthesis in atmospheric pressure adamantane-argon-methane-hydrogen mixtures using a continuous flow plasma microreactor

NASA Astrophysics Data System (ADS)

Stauss, Sven; Ishii, Chikako; Pai, David Z.; Urabe, Keiichiro; Terashima, Kazuo

2014-06-01

Due to their small size, low-power consumption and potential for integration with other devices, microplasmas have been used increasingly for the synthesis of nanomaterials. Here, we have investigated the possibility of using dielectric barrier discharges generated in continuous flow glass microreactors for the synthesis of diamondoids, at temperatures of 300 and 320 K, and applied voltages of 3.2-4.3 kVp-p, at a frequency of 10 kHz. The microplasmas were generated in gas mixtures containing argon, methane, hydrogen and adamantane, which was used as a precursor and seed. The plasmas were monitored by optical emission spectroscopy measurements and the synthesized products were characterized by gas chromatography—mass spectrometry (GC-MS). Depending on the gas composition, the optical emission spectra contained CH and C2 bands of varying intensities. The GC-MS measurements revealed that diamantane can be synthesized by microplasmas generated at atmospheric pressure, and that the yields highly depend on the gas composition and the presence of carbon sources.

Continuous, size and shape-control synthesis of hollow silica nanoparticles enabled by a microreactor-assisted rapid mixing process

NASA Astrophysics Data System (ADS)

He, Yujuan; Kim, Ki-Joong; Chang, Chih-Hung

2017-06-01

Hollow silica nanoparticles (HSNPs) were synthesized using a microreactor-assisted system with a hydrodynamic focusing micromixer. Due to the fast mixing of each precursor in the system, the poly(acrylic acid) (PAA) thermodynamic-locked (TML) conformations were protected from their random aggregations by the immediately initiated growth of silica shells. When altering the mixing time through varying flow rates and flow rate ratios, the different degrees of the aggregation of PAA TML conformations were observed. The globular and necklace-like TML conformations were successfully captured by modifying the PAA concentration at the optimized mixing condition. Uniform HSNPs with an average diameter ∼30 nm were produced from this system. COMSOL numerical models was established to investigate the flow and concentration profiles, and their effects on the formation of PAA templates. Finally, the quality and utility of these uniform HSNPs were demonstrated by the fabrication of antireflective thin films on monocrystalline photovoltaic cells which showed a 3.8% increase in power conversion efficiency.

A flow reactor setup for photochemistry of biphasic gas/liquid reactions

PubMed Central

Schachtner, Josef; Bayer, Patrick

2016-01-01

Summary A home-built microreactor system for light-mediated biphasic gas/liquid reactions was assembled from simple commercial components. This paper describes in full detail the nature and function of the required building elements, the assembly of parts, and the tuning and interdependencies of the most important reactor and reaction parameters. Unlike many commercial thin-film and microchannel reactors, the described set-up operates residence times of up to 30 min which cover the typical rates of many organic reactions. The tubular microreactor was successfully applied to the photooxygenation of hydrocarbons (Schenck ene reaction). Major emphasis was laid on the realization of a constant and highly reproducible gas/liquid slug flow and the effective illumination by an appropriate light source. The optimized set of conditions enabled the shortening of reaction times by more than 99% with equal chemoselectivities. The modular home-made flow reactor can serve as a prototype model for the continuous operation of various other reactions at light/liquid/gas interfaces in student, research, and industrial laboratories. PMID:27829887

Structured fluids as microreactors for flavor formation by the Maillard reaction.

PubMed

Vauthey, S; Milo, C; Frossard, P; Garti, N; Leser, M E; Watzke, H J

2000-10-01

Thermal reactions of cysteine/furfural and cysteine/ribose mixtures were studied in model systems to gain more insight into the influence of structured fluids such as L(2) microemulsions and cubic phases on the generation of aroma compounds. Formation of 2-furfurylthiol from cysteine/furfural was particularly efficient in L(2) microemulsions and cubic phases compared to aqueous systems. The reaction led to the formation of two new sulfur compounds, which were identified as 2-(2-furyl)thiazolidine and, tentatively, N-(2-mercaptovinyl)-2-(2-furyl)thiazolidine. Similarly, generation of 2-furfurylthiol and 2-methyl-3-furanthiol from cysteine/ribose mixtures was strongly enhanced in structured fluids. The cubic phase was shown to be even more efficient in flavor generation than the L(2) microemulsion. It was denoted "cubic catalyst" or "cubic selective microreactor". The obtained results are interpreted in terms of a surface and curvature control of the reactions defined by the structural properties of the formed surfactant associates.

Switchable Opening and Closing of a Liquid Marble via Ultrasonic Levitation.

PubMed

Zang, Duyang; Li, Jun; Chen, Zhen; Zhai, Zhicong; Geng, Xingguo; Binks, Bernard P

2015-10-27

Liquid marbles have promising applications in the field of microreactors, where the opening and closing of their surfaces plays a central role. We have levitated liquid water marbles using an acoustic levitator and, thereby, achieved the manipulation of the particle shell in a controlled manner. Upon increasing the sound intensity, the stable levitated liquid marble changes from a quasi-sphere to a flattened ellipsoid. Interestingly, a cavity on the particle shell can be produced on the polar areas, which can be completely healed when decreasing the sound intensity, allowing it to serve as a microreactor. The integral of the acoustic radiation pressure on the part of the particle surface protruding into air is responsible for particle migration from the center of the liquid marble to the edge. Our results demonstrate that the opening and closing of the liquid marble particle shell can be conveniently achieved via acoustic levitation, opening up a new possibility to manipulate liquid marbles coated with non-ferromagnetic particles.

Continuous Microreactor-Assisted Solution Deposition for Scalable Production of CdS Films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ramprasad, Sudhir; Su, Yu-Wei; Chang, Chih-Hung

2013-06-13

Solution deposition offers an attractive, low temperature option in the cost effective production of thin film solar cells. Continuous microreactor-assisted solution deposition (MASD) was used to produce nanocrystalline cadmium sulfide (CdS) films on fluorine doped tin oxide (FTO) coated glass substrates with excellent uniformity. We report a novel liquid coating technique using a ceramic rod to efficiently and uniformly apply reactive solution to large substrates (152 mm × 152 mm). This technique represents an inexpensive approach to utilize the MASD on the substrate for uniform growth of CdS films. Nano-crystalline CdS films have been produced from liquid phase at ~90°C,more » with average thicknesses of 70 nm to 230 nm and with a 5 to 12% thickness variation. The CdS films produced were characterized by UV-Vis spectroscopy, transmission electron microscopy, and X-Ray diffraction to demonstrate their suitability to thin-film solar technology.« less

Testing of the Defense Waste Processing Facility Cold Chemical Dissolution Method in Sludge Batch 9 Qualification

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edwards, T.; Pareizs, J.; Coleman, C.

For each sludge batch that is processed in the Defense Waste Processing Facility (DWPF), the Savannah River National Laboratory (SRNL) tests the applicability of the digestion methods used by the DWPF Laboratory for elemental analysis of Sludge Receipt and Adjustment Tank (SRAT) Receipt samples and SRAT Product process control samples. DWPF SRAT samples are typically dissolved using a method referred to as the DWPF Cold Chemical or Cold Chem Method (CC), (see DWPF Procedure SW4- 15.201). Testing indicates that the CC method produced mixed results. The CC method did not result in complete dissolution of either the SRAT Receipt ormore » SRAT Product with some fine, dark solids remaining. However, elemental analyses did not reveal extreme biases for the major elements in the sludge when compared with analyses obtained following dissolution by hot aqua regia (AR) or sodium peroxide fusion (PF) methods. The CC elemental analyses agreed with the AR and PF methods well enough that it should be adequate for routine process control analyses in the DWPF after much more extensive side-by-side tests of the CC method and the PF method are performed on the first 10 SRAT cycles of the Sludge Batch 9 (SB9) campaign. The DWPF Laboratory should continue with their plans for further tests of the CC method during these 10 SRAT cycles.« less

Multistep continuous-flow synthesis of (R)- and (S)-rolipram using heterogeneous catalysts

NASA Astrophysics Data System (ADS)

Tsubogo, Tetsu; Oyamada, Hidekazu; Kobayashi, Shū

2015-04-01

Chemical manufacturing is conducted using either batch systems or continuous-flow systems. Flow systems have several advantages over batch systems, particularly in terms of productivity, heat and mixing efficiency, safety, and reproducibility. However, for over half a century, pharmaceutical manufacturing has used batch systems because the synthesis of complex molecules such as drugs has been difficult to achieve with continuous-flow systems. Here we describe the continuous-flow synthesis of drugs using only columns packed with heterogeneous catalysts. Commercially available starting materials were successively passed through four columns containing achiral and chiral heterogeneous catalysts to produce (R)-rolipram, an anti-inflammatory drug and one of the family of γ-aminobutyric acid (GABA) derivatives. In addition, simply by replacing a column packed with a chiral heterogeneous catalyst with another column packed with the opposing enantiomer, we obtained antipole (S)-rolipram. Similarly, we also synthesized (R)-phenibut, another drug belonging to the GABA family. These flow systems are simple and stable with no leaching of metal catalysts. Our results demonstrate that multistep (eight steps in this case) chemical transformations for drug synthesis can proceed smoothly under flow conditions using only heterogeneous catalysts, without the isolation of any intermediates and without the separation of any catalysts, co-products, by-products, and excess reagents. We anticipate that such syntheses will be useful in pharmaceutical manufacturing.

Banning of methyl bromide for seed treatment: could Ditylenchus dipsaci again become a major threat to alfalfa production in Europe?

PubMed

Mouttet, Raphaëlle; Escobar-Gutiérrez, Abraham; Esquibet, Magali; Gentzbittel, Laurent; Mugniéry, Didier; Reignault, Philippe; Sarniguet, Corinne; Castagnone-Sereno, Philippe

2014-07-01

In Europe, the stem and bulb nematode Ditylenchus dipsaci has been listed as a quarantine pest by EPPO: without any control, it may cause complete failure of alfalfa crops. Movement of nematodes associated with seeds is considered to be the highest-risk pathway for the spread of this pest. Since the 2010 official withdrawal of methyl bromide in Europe, and in the absence of any alternative chemical, fumigation of contaminated seed batches is no longer possible, which makes the production of nematode-free alfalfa seeds difficult to achieve and leads to unmarketable seed batches. Thermotherapy is being considered as a realistic alternative strategy, but its efficiency still remains to be validated. The combination of the currently available methods (i.e. use of resistant cultivars, seed production according to a certification scheme, mechanical sieving, seed batch inspection) could significantly reduce the likelihood of seed contamination. However, it does not guarantee a total eradication of the nematode. Although it is already widely distributed all over Europe, reclassification of D. dipsaci as a regulated non-quarantine pest to reduce the possibility of further introductions and the rate of spread of this pest appears to be a risky strategy because of the lack of up-to-date documented data to evaluate damage thresholds and determine acceptable tolerance levels. © 2014 Society of Chemical Industry.

Establishment of the Ph. Eur. erythropoietin chemical reference substance batch 1.

PubMed

Burns, C; Bristow, A F; Buchheit, K H; Daas, A; Wierer, M; Costanzo, A

2015-01-01

The Erythropoietin (EPO) European Pharmacopoeia (Ph. Eur.) Biological Reference Preparation (BRP) batch 3 was calibrated in 2006 by in vivo bioassay and was used as a reference preparation for these assays as well as for the physicochemical methods in the Ph. Eur. monograph Erythropoietin concentrated solution (1316). In order to avoid the frequent replacement of this standard and thus reduce the use of animals, a new EPO Chemical Reference Substance (CRS) was established to be used solely for the physicochemical methods. Here we report the outcome of a collaborative study aimed at demonstrating the suitability of the candidate CRS (cCRS) as a reference for the physicochemical methods in the Ph. Eur. monograph. Results from the study demonstrated that for the physicochemical methods currently required in the monograph (capillary zone electrophoresis (CZE), polyacrylamide gel electrophoresis (PAGE)/immunoblotting and peptide mapping), the cCRS is essentially identical to the existing BRP. However, data also indicated that, for the physicochemical methods under consideration for inclusion in a revised monograph (test for oxidised forms and glycan mapping), the suitability of the cCRS as a reference needs to be confirmed with additional work. Further to completion of the study, the Ph. Eur. Commission adopted the cCRS as "Erythropoietin for physicochemical tests CRS batch 1" to be used for CZE, PAGE/immunoblotting and peptide mapping.

Optimisation of enzymatic hydrolysis of apple pomace for production of biofuel and biorefinery chemicals using commercial enzymes.

PubMed

Gama, Repson; Van Dyk, J Susan; Pletschke, Brett I

2015-12-01

Apple pomace, a waste product from the apple juice industry is a potential feedstock for biofuel and biorefinery chemical production. Optimisation of hydrolysis conditions for apple pomace hydrolysis using Viscozyme L and Celluclast 1.5L was investigated using 1 L reaction volumes. The effects of temperature, pH, β-glucosidase supplementation and substrate feeding regimes were determined. Hydrolysis at room temperature using an unbuffered system gave optimal performance. Reactors in batch mode resulted in a better performance (4.2 g/L glucose and 16.8 g/L reducing sugar, 75 % yield for both) than fed-batch (3.2 g/L glucose and 14.6 g/L reducing sugar, 65.5 and 73.1 % yield respectively) in 72 h. The addition of Novozyme 188 to the core mixture of Viscozyme L and Celluclast 1.5L resulted in the doubling of glucose released. The main products (yield %) released from apple pomace hydrolysis were galacturonic acid (78 %), glucose (75 %), arabinose (90 %) and galactose (87 %). These products are potential raw materials for biofuel and biorefinery chemical production.

Application of the International Water Association activated sludge models to describe aerobic sludge digestion.

PubMed

Ghorbani, M; Eskicioglu, C

2011-12-01

Batch and semi-continuous flow aerobic digesters were used to stabilize thickened waste-activated sludge at different initial conditions and mean solids retention times. Under dynamic conditions, total suspended solids, volatile suspended solids (VSS) and total and particulate chemical oxygen demand (COD and PCOD) were monitored in the batch reactors and effluent from the semi-continuous flow reactors. Activated Sludge Model (ASM) no. 1 and ASM no. 3 were applied to measured data (calibration data set) to evaluate the consistency and performances of models at different flow regimes for digester COD and VSS modelling. The results indicated that both ASM1 and ASM3 predicted digester COD, VSS and PCOD concentrations well (R2, Ra2 > or = 0.93). Parameter estimation concluded that compared to ASM1, ASM3 parameters were more consistent across different batch and semi-continuous flow runs with different operating conditions. Model validation on a data set independent from the calibration data successfully predicted digester COD (R2 = 0.88) and VSS (R2 = 0.94) concentrations by ASM3, while ASM1 overestimated both reactor COD (R2 = 0.74) and VSS concentrations (R2 = 0.79) after 15 days of aerobic batch digestion.

Biodegradation kinetics of 1,4-benzoquinone in batch and continuous systems.

PubMed

Kumar, Pardeep; Nemati, Mehdi; Hill, Gordon A

2011-11-01

Combining chemical and biological treatments is a potentially economic approach to remove high concentration of recalcitrant compounds from wastewaters. In the present study, the biodegradation of 1,4-benzoquinone, an intermediate compound formed during phenol oxidation by chlorine dioxide, was investigated using Pseudomonas putida (ATCC 17484) in batch and continuous bioreactors. Batch experiments were conducted to determine the effects of 1,4-benzoquinone concentration and temperature on the microbial activity and biodegradation kinetics. Using the generated data, the maximum specific growth rate and biodegradation rate were determined as 0.94 h(-1) and 6.71 mg of 1,4-benzoquinone l(-1) h(-1). Biodegradation in a continuous bioreactor indicated a linear relationship between substrate loading and biodegradation rates prior to wash out of the cells, with a maximum biodegradation rate of 246 mg l(-1) h(-1) observed at a loading rate of 275 mg l(-1) h(-1) (residence time: 1.82 h). Biokinetic parameters were also determined using the steady state substrate and biomass concentrations at various dilution rates and compared to those obtained in batch cultures.

Building an R&D chemical registration system.

PubMed

Martin, Elyette; Monge, Aurélien; Duret, Jacques-Antoine; Gualandi, Federico; Peitsch, Manuel C; Pospisil, Pavel

2012-05-31

Small molecule chemistry is of central importance to a number of R&D companies in diverse areas such as the pharmaceutical, nutraceutical, food flavoring, and cosmeceutical industries. In order to store and manage thousands of chemical compounds in such an environment, we have built a state-of-the-art master chemical database with unique structure identifiers. Here, we present the concept and methodology we used to build the system that we call the Unique Compound Database (UCD). In the UCD, each molecule is registered only once (uniqueness), structures with alternative representations are entered in a uniform way (normalization), and the chemical structure drawings are recognizable to chemists and to a cartridge. In brief, structural molecules are entered as neutral entities which can be associated with a salt. The salts are listed in a dictionary and bound to the molecule with the appropriate stoichiometric coefficient in an entity called "substance". The substances are associated with batches. Once a molecule is registered, some properties (e.g., ADMET prediction, IUPAC name, chemical properties) are calculated automatically. The UCD has both automated and manual data controls. Moreover, the UCD concept enables the management of user errors in the structure entry by reassigning or archiving the batches. It also allows updating of the records to include newly discovered properties of individual structures. As our research spans a wide variety of scientific fields, the database enables registration of mixtures of compounds, enantiomers, tautomers, and compounds with unknown stereochemistries.

Sorption-desorption of indaziflam in selected agricultural soils

USDA-ARS?s Scientific Manuscript database

Sorption and desorption of indaziflam in 6 soils from Brazil and 3 soils from the USA, with different physical chemical properties, were investigated using the batch equilibration method. Sorption kinetics demonstrated that soil-solution equilibrium was attained in a 24-h period. The Freundlich equa...

In situ hydrogen utilization for high fraction acetate production in mixed culture hollow-fiber membrane biofilm reactor.

PubMed

Zhang, Fang; Ding, Jing; Shen, Nan; Zhang, Yan; Ding, Zhaowei; Dai, Kun; Zeng, Raymond J

2013-12-01

Syngas fermentation is a promising route for resource recovery. Acetate is an important industrial chemical product and also an attractive precursor for liquid biofuels production. This study demonstrated high fraction acetate production from syngas (H₂ and CO₂) in a hollow-fiber membrane biofilm reactor, in which the hydrogen utilizing efficiency reached 100% during the operational period. The maximum concentration of acetate in batch mode was 12.5 g/L, while the acetate concentration in continuous mode with a hydraulic retention time of 9 days was 3.6 ± 0.1 g/L. Since butyrate concentration was rather low and below 0.1 g/L, the acetate fraction was higher than 99% in both batch and continuous modes. Microbial community analysis showed that the biofilm was dominated by Clostridium spp., such as Clostridium ljungdahlii and Clostridium drakei, the percentage of which was 70.5%. This study demonstrates a potential technology for the in situ utilization of syngas and valuable chemical production.

Preparation of plutonium-bearing ceramics via mechanically activated precursor

NASA Astrophysics Data System (ADS)

Chizhevskaya, S. V.; Stefanovsky, S. V.

2000-07-01

The problem of excess weapons plutonium disposition is suggested to be solved by means of its incorporation in stable ceramics with high chemical durability and radiation resistivity. The most promising host phases for plutonium as well as uranium and neutron poisons (gadolinium, hafnium) are zirconolite, pyrochlore, zircon, zirconia [1,2], and murataite [3]. Their production requires high temperatures and a fine-grained homogeneous precursor to reach final waste form with high quality and low leachability. Currently various routes to homogeneous products preparation such as sol-gel technology, wet-milling, and grinding in a ball or planetary mill are used. The best result demonstrates sol-gel technology but this route is very complicated. An alternative technology for preparation of ceramic precursors is the treatment of the oxide batch with high mechanical energy [4]. Such a treatment produces combination of mechanical (fine milling with formation of various defects, homogenization) and chemical (split bonds with formation of active centers—free radicals, ion-radicals, etc.) effects resulting in higher reactivity of the activated batch.

Chemical and pharmacological comparison of modern and traditional dosage forms of Joshanda.

PubMed

Parveen, Sajida; Irfan Bukhari, Nadeem; Shehzadi, Naureen; Qamar, Shaista; Ali, Ejaz; Naheed, Surriya; Latif, Abida; Yuchi, Alamgeer; Hussain, Khalid

2017-12-11

Recently, a traditional remedy (Joshanda) has been replaced largely by modern ready-to-use dosage forms, which have not been compared to the original remedy. Therefore, the present study aimed to compare a number of modern dosage forms with traditional remedy. Seven brands, 3 batches each, were compared with a Lab-made formulation with reference to analytical (proximate analyses, spectroscopic and chromatographic metabolomes) and pharmacological profiles (anti-inflammatory and antibacterial activities). Chemical and pharmacological differences were found between Lab-made Joshanda and modern dosage forms. Such variations were also found within the brands and batches of modern formulations (p < 0.05). The Lab-made Joshanda showed significantly higher pharmacological activities as compared to modern brands (p ). The results of the present study indicate that modern dosage forms are unstandardised and less effective than the traditional remedy. Characteristic profiles obtained from Lab-made Joshanda may be used as reference to produce comparable dosage forms.

Optimal Solutions of Multiproduct Batch Chemical Process Using Multiobjective Genetic Algorithm with Expert Decision System

PubMed Central

Mokeddem, Diab; Khellaf, Abdelhafid

2009-01-01

Optimal design problem are widely known by their multiple performance measures that are often competing with each other. In this paper, an optimal multiproduct batch chemical plant design is presented. The design is firstly formulated as a multiobjective optimization problem, to be solved using the well suited non dominating sorting genetic algorithm (NSGA-II). The NSGA-II have capability to achieve fine tuning of variables in determining a set of non dominating solutions distributed along the Pareto front in a single run of the algorithm. The NSGA-II ability to identify a set of optimal solutions provides the decision-maker DM with a complete picture of the optimal solution space to gain better and appropriate choices. Then an outranking with PROMETHEE II helps the decision-maker to finalize the selection of a best compromise. The effectiveness of NSGA-II method with multiojective optimization problem is illustrated through two carefully referenced examples. PMID:19543537

Ultrasound pretreatment for enhanced biogas production from olive mill wastewater.

PubMed

Oz, Nilgun Ayman; Uzun, Alev Cagla

2015-01-01

This study investigates applicability of low frequency ultrasound technology to olive mill wastewaters (OMWs) as a pretreatment step prior to anaerobic batch reactors to improve biogas production and methane yield. OMWs originating from three phase processes are characterized with high organic content and complex nature. The treatment of the wastewater is problematic and alternative treatment options should be investigated. In the first part of the study, OMW samples were subjected to ultrasound at a frequency of 20kHz with applied powers varying between 50 and 100W under temperature controlled conditions for different time periods in order to determine the most effective sonication conditions. The level of organic matter solubilization at ultrasound experiments was assessed by calculating the ratio of soluble chemical oxygen demand/total chemical oxygen demand (SCOD/TCOD). The results revealed that the optimum ultrasonic condition for diluted OMW is 20kHz, 0.4W/mL for 10min. The application of ultrasound to OMW increased SCOD/TCOD ratio from 0.59 to 0.79. Statistical analysis (Friedman's tests) show that ultrasound was significantly effective on diluted OMW (p<0.05) in terms of SCOD parameter, but not for raw OMW (p>0.05). For raw OMW, this increase has been found to be limited due to high concentration of suspended solids (SS). In the second part of the study, biogas and methane production rates of anaerobic batch reactor fed with the ultrasound pretreated OMW samples were compared with the results of control reactor fed with untreated OMW in order to determine the effect of sonication. A nonparametric statistical procedure, Mann-Whitney U test, was used to compare biogas and methane production from anaerobic batch reactors for control and ultrasound pretreated samples. Results showed that application of low frequency ultrasound to OMW significantly improved both biogas and methane production in anaerobic batch reactor fed with the wastewater (p<0.05). Anaerobic batch reactor fed with ultrasound pretreated diluted OMW produced approximately 20% more biogas and methane compared with the untreated one (control reactor). The overall results indicated that low frequency ultrasound pretreatment increased soluble COD in OMW and subsequently biogas production. Copyright © 2014 Elsevier B.V. All rights reserved.

Microchannel Reactor System Design & Demonstration For On-Site H2O2 Production by Controlled H2/O2 Reaction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Adeniyi Lawal

We successfully demonstrated an innovative hydrogen peroxide (H2O2) production concept which involved the development of flame- and explosion-resistant microchannel reactor system for energy efficient, cost-saving, on-site H2O2 production. We designed, fabricated, evaluated, and optimized a laboratory-scale microchannel reactor system for controlled direct combination of H2 and O2 in all proportions including explosive regime, at a low pressure and a low temperature to produce about 1.5 wt% H2O2 as proposed. In the second phase of the program, as a prelude to full-scale commercialization, we demonstrated our H2O2 production approach by ‘numbering up’ the channels in a multi-channel microreactor-based pilot plant tomore » produce 1 kg/h of H2O2 at 1.5 wt% as demanded by end-users of the developed technology. To our knowledge, we are the first group to accomplish this significant milestone. We identified the reaction pathways that comprise the process, and implemented rigorous mechanistic kinetic studies to obtain the kinetics of the three main dominant reactions. We are not aware of any such comprehensive kinetic studies for the direct combination process, either in a microreactor or any other reactor system. We showed that the mass transfer parameter in our microreactor system is several orders of magnitude higher than what obtains in the macroreactor, attesting to the superior performance of microreactor. A one-dimensional reactor model incorporating the kinetics information enabled us to clarify certain important aspects of the chemistry of the direct combination process as detailed in section 5 of this report. Also, through mathematical modeling and simulation using sophisticated and robust commercial software packages, we were able to elucidate the hydrodynamics of the complex multiphase flows that take place in the microchannel. In conjunction with the kinetics information, we were able to validate the experimental data. If fully implemented across the whole industry as a result of our technology demonstration, our production concept is expected to save >5 trillion Btu/year of steam usage and >3 trillion Btu/year in electric power consumption. Our analysis also indicates >50 % reduction in waste disposal cost and ~10% reduction in feedstock energy. These savings translate to ~30% reduction in overall production and transportation costs for the $1B annual H2O2 market.« less

Isomerization and Fragmentation of Cyclohexanone in a Heated Micro-Reactor.

PubMed

Porterfield, Jessica P; Nguyen, Thanh Lam; Baraban, Joshua H; Buckingham, Grant T; Troy, Tyler P; Kostko, Oleg; Ahmed, Musahid; Stanton, John F; Daily, John W; Ellison, G Barney

2015-12-24

The thermal decomposition of cyclohexanone (C6H10═O) has been studied in a set of flash-pyrolysis microreactors. Decomposition of the ketone was observed when dilute samples of C6H10═O were heated to 1200 K in a continuous flow microreactor. Pyrolysis products were detected and identified by tunable VUV photoionization mass spectroscopy and by photoionization appearance thresholds. Complementary product identification was provided by matrix infrared absorption spectroscopy. Pyrolysis pressures were roughly 100 Torr, and contact times with the microreactors were roughly 100 μs. Thermal cracking of cyclohexanone appeared to result from a variety of competing pathways, all of which open roughly simultaneously. Isomerization of cyclohexanone to the enol, cyclohexen-1-ol (C6H9OH), is followed by retro-Diels-Alder cleavage to CH2═CH2 and CH2═C(OH)-CH═CH2. Further isomerization of CH2═C(OH)-CH═CH2 to methyl vinyl ketone (CH3CO-CH═CH2, MVK) was also observed. Photoionization spectra identified both enols, C6H9OH and CH2═C(OH)-CH═CH2, and the ionization threshold of C6H9OH was measured to be 8.2 ± 0.1 eV. Coupled cluster electronic structure calculations were used to establish the energetics of MVK. The heats of formation of MVK and its enol were calculated to be ΔfH298(cis-CH3CO-CH═CH2) = -26.1 ± 0.5 kcal mol(-1) and ΔfH298(s-cis-1-CH2═C(OH)-CH═CH2) = -13.7 ± 0.5 kcal mol(-1). The reaction enthalpy ΔrxnH298(C6H10═O → CH2═CH2 + s-cis-1-CH2═C(OH)-CH═CH2) is 53 ± 1 kcal mol(-1) and ΔrxnH298(C6H10═O → CH2═CH2 + cis-CH3CO-CH═CH2) is 41 ± 1 kcal mol(-1). At 1200 K, the products of cyclohexanone pyrolysis were found to be C6H9OH, CH2═C(OH)-CH═CH2, MVK, CH2CHCH2, CO, CH2═C═O, CH3, CH2═C═CH2, CH2═CH-CH═CH2, CH2═CHCH2CH3, CH2═CH2, and HC≡CH.

Isomerization and Fragmentation of Cyclohexanone in a Heated Micro-Reactor

DOE PAGES

Porterfield, Jessica P.; Nguyen, Thanh Lam; Baraban, Joshua H.; ...

2015-11-30

Here, the thermal decomposition of cyclohexanone (C 6H 10=O) has been studied in a set of flash-pyrolysis microreactors. Decomposition of the ketone was observed when dilute samples of C 6H 10=O were heated to 1200 K in a continuous flow microreactor. Pyrolysis products were detected and identified by tunable VUV photoionization mass spectroscopy and by photoionization appearance thresholds. Complementary product identification was provided by matrix infrared absorption spectroscopy. Pyrolysis pressures were roughly 100 Torr, and contact times with the microreactors were roughly 100 μs. Thermal cracking of cyclohexanone appeared to result from a variety of competing pathways, all of whichmore » open roughly simultaneously. Isomerization of cyclohexanone to the enol, cyclohexen-1-ol (C 6H 9OH), is followed by retro-Diels–Alder cleavage to CH 2=CH 2 and CH 2=C(OH)–CH=CH 2. Further isomerization of CH 2=C(OH)–CH=CH 2 to methyl vinyl ketone (CH 3CO–CH=CH 2, MVK) was also observed. Photoionization spectra identified both enols, C 6H 9OH and CH 2=C(OH)–CH=CH 2, and the ionization threshold of C 6H 9OH was measured to be 8.2 ± 0.1 eV. Coupled cluster electronic structure calculations were used to establish the energetics of MVK. The heats of formation of MVK and its enol were calculated to be Δ fH 298(cis-CH 3CO–CH=CH 2) = -26.1 ± 0.5 kcal mol –1 and Δ fH 298(s-cis-1-CH 2=C(OH)–CH=CH 2) = -13.7 ± 0.5 kcal mol –1. The reaction enthalpy Δ rxnH 298(C 6H 10=O → CH 2=CH 2 + s-cis-1-CH 2=C(OH)–CH=CH 2) is 53 ± 1 kcal mol –1 and Δ rxnH 298(C 6H 10=O → CH 2=CH 2 + cis-CH 3CO–CH=CH 2) is 41 ± 1 kcal mol –1. At 1200 K, the products of cyclohexanone pyrolysis were found to be C 6H 9OH, CH 2=C(OH)–CH=CH 2, MVK, CH 2CHCH 2, CO, CH 2=C=O, CH 3, CH 2=C=CH 2, CH 2=CH–CH=CH 2, CH 2=CHCH 2CH 3, CH 2=CH 2, and HC≡CH.« less

Coupled solar photo-Fenton and biological treatment for the degradation of diuron and linuron herbicides at pilot scale.

PubMed

Farré, Maria José; Maldonado, Manuel Ignacio; Gernjak, Wolfgang; Oller, Isabel; Malato, Sixto; Domènech, Xavier; Peral, José

2008-06-01

A coupled solar photo-Fenton (chemical) and biological treatment has been used to remove biorecalcitrant diuron (42 mg l(-1)) and linuron (75 mg l(-1)) herbicides from water at pilot plant scale. The chemical process has been carried out in a 82 l solar pilot plant made up by four compound parabolic collector units, and it was followed by a biological treatment performed in a 40 l sequencing batch reactor. Two Fe(II) doses (2 and 5 mg l(-1)) and sequential additions of H2O2 (20 mg l(-1)) have been used to chemically degrade the initially polluted effluent. Next, biodegradability at different oxidation states has been assessed by means of BOD/COD ratio. A reagent dose of Fe=5 mg l(-1) and H2O2=100 mg l(-1) has been required to obtain a biodegradable effluent after 100 min of irradiation time. Finally, the organic content of the photo-treated solution has been completely assimilated by a biomass consortium in the sequencing batch reactor using a total suspended solids concentration of 0.2 g l(-1) and a hydraulic retention time of 24h. Comparison between the data obtained at pilot plant scale (specially the one corresponding to the chemical step) and previously published data from a similar system performing at laboratory scale, has been carried out.

An experimental and modeling study of grain-scale uranium desorption from field-contaminated sediments and the potential influence of microporosity on mass-transfer

NASA Astrophysics Data System (ADS)

Stoliker, D.; Liu, C.; Kent, D. B.; Zachara, J. M.

2012-12-01

The aquifer below the 300-Area of the Hanford site (Richland, WA, USA) is plagued by a persistent plume of dissolved uranium (U(VI)) in excess of the Environmental Protection Agency drinking water maximum contamination level even after the removal of highly contaminated sediments. The aquifer sediments in the seasonally saturated lower vadose zone act as both a source and sink for uranium during stage changes in the nearby Columbia River. Diffusion limitation of uranium mass-transfer within these sediments has been cited as a potential cause of the plume's persistence. Equilibrium U(VI) sorption is a strong function of variable chemical conditions, especially carbonate, hydrogen, and uranyl ion activities. Field-contaminated sediments from the site require up to 1,000 hours to reach equilibrium in static batch reactors. Increases in U(VI) concentrations over longer time-scales result from changes in chemical conditions, which drive reactions with sediments that favor U(VI) desorption. Grain-scale U(VI) sorption/desorption rates are slow, likely owing to diffusion of U(VI) and other solutes through intra-granular pore domains. In order to improve understanding of the impact of intra-granular diffusion and chemical reactions controlling grain-scale U(VI) release, experiments were conducted on individual particle size fractions of a <8 mm composite of field-contaminated, lower vadose zone sediments. For each size fraction, equilibrium U(VI) sorption/desorption in static batch reactors was well-described by surface complexation models over a range of chemical conditions applicable to the field site. Desorption rates from individual size fractions in flow-through batch reactors, examined under a single set of constant chemical conditions with multiple stop-flow events, were similar for all size fractions <2 mm. Kinetic U(VI) desorption in flow-through batch reactors was modeled using a multi-rate surface complexation approach, where sorption/desorption rates were assumed to be proportional to the displacement from equilibrium and multiple diffusion domains were described with a two-parameter lognormal distribution of mass-transfer rate coefficients. Parameters describing mass transfer were the same for all size fractions <2 mm but differed for the largest (2-8 mm) size fraction. The evolution of pH, along with dissolved cation and carbonate concentrations, was modeled using equilibrium cation exchange, rate-limited calcite dissolution, aerobic respiration, and silica dissolution. Desorption and chemical reaction models calibrated with individual size fractions predicted U(VI) and chemical composition as a function of time for the bulk sediment sample. Volumes of pores less than 2.4 nm, quantified using nitrogen adsorption-desorption isotherms, were the same for all size fractions < 2 mm, nearly double that of the 2-8 mm size fraction. Similarity in the observed pore volumes and multi-rate mass-transfer parameters across all size fractions <2 mm suggest the importance of pores in this size class in controlling slow grain-scale U(VI) desorption rates. Models like these provide a means for testing the influence of grain-scale mass-transfer on the persistence of U(VI) plume at the site.

IRIS Update Batch 1, Group 1

EPA Science Inventory

Update the following IRIS chemical dose-response assessments: Barium (cancer, RfC), o-Cresol (RfD, cancer), carbon disulfied (RfD, RfC), 1,1-Dichloroethane (cancer), 2,4-Dimethylphenol (RfD), 1,4-Dibromobenzene (RfD), 1-chloro-1,1-difluroelfane (RfC, Acetyl chloride (cancer),2,4...

40 CFR 63.2520 - What reports must I submit and when?

Code of Federal Regulations, 2012 CFR

2012-07-01

... (CONTINUED) National Emission Standards for Hazardous Air Pollutants: Miscellaneous Organic Chemical... from streams that contain energetics and organic peroxides, and rationale for why meeting the emission... lb/yr, the total uncontrolled organic HAP emissions from the batch process vents in an MCPU will be...

Preozonation of primary-treated municipal wastewater for reuse in biofuel feedstock generation

EPA Science Inventory

The results of a laboratory scale investigation on ozone pretreatment of primary treated municipal wastewater for potential reuse in fermentation processes for the production of biofuels and bio-based feedstock chemicals were presented. Semi-batch preozonation with 3.0 % (w/w) oz...

Removal of Radioactive Materials from Groundwater Using Porous Iron Composite Media

NASA Astrophysics Data System (ADS)

Dorward, E.; Thomas, R.; Cochran, J. P.; Chang, H. S.; Tandukar, M.; Coutelot, F.; Seaman, J. C.

2017-12-01

Uranium (U) is a concern in aqueous environments because of its toxicity. Reducing the mobile U(VI) to the relatively immobile U(IV) can decrease soluble U concentrations. Zero valent iron (ZVI) has been demonstrated as an effective reducing agent for U(VI) as well as other frequently occurring co-contaminants, such as nitrate (NO3-). However, the ability of ZVI to chemically reduce and immobilize U and other associated contaminants in more complex systems containing many alternate electron acceptors and non-ideal chemical conditions remains a concern. Porous iron composite (PIC) materials were evaluated for their ability to address these concerns in both batch and column experiments. We created an artificial groundwater surrogate containing ≈ 100 mg L-1 NO3-, 200 mg L-1 alkalinity, 100 µg L-1 U(VI) as uranyl (UO2+2), 100 µg L-1 rhenium (Re) as perrhenate (ReO4-), and 50 µg L-1 arsenic (As). In batch, we reacted 5 grams of PIC material with 200 mL groundwater surrogate under two different atmospheric conditions to evaluate the impact of O2. At specific time intervals, 5 mL aliquots from each batch treatment were removed for chemical analysis (i.e., U, Re, As, Fe, NO3, etc.) and the pH and ORP of the remaining suspension was measured. The PIC was effective at fully reducing NO3- levels over the extended reaction time despite rapid pH increase (> 8) during equilibration. Soluble levels of U and Re, a chemical surrogate for 99Tc, decreased in a similar fashion to NO3- in both the presence and absence of O2. Soluble As levels decreased more rapidly than other contaminants, but remained at ≈ 1 µg L-1. Very little nitrite (NO2-) was detected in the batch tests, with NH4+ levels consistent with the amount of NO3- reduced. Similar rates of immobilization for U, Re, and As were observed in the presence and absence of NO3-. Subsequent leaching tests corresponding to residence times ranging from 120 to 7.5 minutes demonstrated the ability of the PIC to reduce NO3- to NH4+, with no persistence of NO2-. Uranium and As were readily immobilized regardless of flow velocity. A strong kinetic component was observed for Re leaching behavior in the column tests. These results indicate the strong ability of PIC material to reduce U, NO3-, and other species under conditions that frequently inhibit conventional ZVI effectiveness.

Evaluation of the COSHH Essentials Model with a Mixture of Organic Chemicals at a Medium-Sized Paint Producer

PubMed Central

Lee, Eun Gyung; Slaven, James; Bowen, Russell B.; Harper, Martin

2011-01-01

The Control of Substances Hazardous to Health (COSHH) Essentials model was evaluated using full-shift exposure measurements of five chemical components in a mixture [acetone, ethylbenzene, methyl ethyl ketone, toluene, and xylenes] at a medium-sized plant producing paint materials. Two tasks, batch-making and bucket-washing, were examined. Varying levels of control were already established in both tasks and the average exposures of individual chemicals were considerably lower than the regulatory and advisory 8-h standards. The average exposure fractions using the additive mixture formula were also less than unity (batch-making: 0.25, bucket-washing: 0.56) indicating the mixture of chemicals did not exceed the combined occupational exposure limit (OEL). The paper version of the COSHH Essentials model was used to calculate a predicted exposure range (PER) for each chemical according to different levels of control. The estimated PERs of the tested chemicals for both tasks did not show consistent agreement with exposure measurements when the comparison was made for each control method and this is believed to be because of the considerably different volatilities of the chemicals. Given the combination of health hazard and exposure potential components, the COSHH Essentials model recommended a control approach ‘special advice’ for both tasks, based on the potential reproductive hazard ascribed to toluene. This would not have been the same conclusion if some other chemical had been substituted (for example styrene, which has the same threshold limit value as toluene). Nevertheless, it was special advice, which had led to the combination of hygienic procedures in place at this plant. The probability of the combined exposure fractions exceeding unity was 0.0002 for the batch-making task indicating that the employees performing this task were most likely well protected below the OELs. Although the employees involved in the bucket-washing task had greater potential to exceed the threshold limit value of the mixture (P > 1 = 0.2375), the expected personal exposure after adjusting for the assigned protection factor for the respirators in use would be considerably lower (P > 1 = 0.0161). Thus, our findings suggested that the COSHH essentials model worked reasonably well for the volatile organic chemicals at the plant. However, it was difficult to override the reproductive hazard even though it was meant to be possible in principle. Further, it became apparent that an input of existing controls, which is not possible in the web-based model, may have allowed the model be more widely applicable. The experience of using the web-based COSHH Essentials model generated some suggestions to provide a more user-friendly tool to the model users who do not have expertise in occupational hygiene. PMID:21047985

Evaluation of the COSHH Essentials model with a mixture of organic chemicals at a medium-sized paint producer.

PubMed

Lee, Eun Gyung; Slaven, James; Bowen, Russell B; Harper, Martin

2011-01-01

The Control of Substances Hazardous to Health (COSHH) Essentials model was evaluated using full-shift exposure measurements of five chemical components in a mixture [acetone, ethylbenzene, methyl ethyl ketone, toluene, and xylenes] at a medium-sized plant producing paint materials. Two tasks, batch-making and bucket-washing, were examined. Varying levels of control were already established in both tasks and the average exposures of individual chemicals were considerably lower than the regulatory and advisory 8-h standards. The average exposure fractions using the additive mixture formula were also less than unity (batch-making: 0.25, bucket-washing: 0.56) indicating the mixture of chemicals did not exceed the combined occupational exposure limit (OEL). The paper version of the COSHH Essentials model was used to calculate a predicted exposure range (PER) for each chemical according to different levels of control. The estimated PERs of the tested chemicals for both tasks did not show consistent agreement with exposure measurements when the comparison was made for each control method and this is believed to be because of the considerably different volatilities of the chemicals. Given the combination of health hazard and exposure potential components, the COSHH Essentials model recommended a control approach 'special advice' for both tasks, based on the potential reproductive hazard ascribed to toluene. This would not have been the same conclusion if some other chemical had been substituted (for example styrene, which has the same threshold limit value as toluene). Nevertheless, it was special advice, which had led to the combination of hygienic procedures in place at this plant. The probability of the combined exposure fractions exceeding unity was 0.0002 for the batch-making task indicating that the employees performing this task were most likely well protected below the OELs. Although the employees involved in the bucket-washing task had greater potential to exceed the threshold limit value of the mixture (P > 1 = 0.2375), the expected personal exposure after adjusting for the assigned protection factor for the respirators in use would be considerably lower (P > 1 = 0.0161). Thus, our findings suggested that the COSHH essentials model worked reasonably well for the volatile organic chemicals at the plant. However, it was difficult to override the reproductive hazard even though it was meant to be possible in principle. Further, it became apparent that an input of existing controls, which is not possible in the web-based model, may have allowed the model be more widely applicable. The experience of using the web-based COSHH Essentials model generated some suggestions to provide a more user-friendly tool to the model users who do not have expertise in occupational hygiene.

CATALYTIC HYDRODECHLORINATION OF 1,3-DICHLOROPROPENE. (R826694C626)

EPA Science Inventory

The hydrodechlorination reactions of 1,3-dichloropropene, a component of the waste stream from epichlorohydrin manufacturing, were examined over a variety of catalysts in a packed-bed microreactor. The reactor operated between 7.5–9 Mpa and 325°C and rates of ...

Exploring the Fundamentals of Microreactor Technology with Multidisciplinary Lab Experiments Combining the Synthesis and Characterization of Inorganic Nanoparticles

ERIC Educational Resources Information Center

Emmanuel, Noemie; Emonds-Alt, Gauthier; Lismont, Marjorie; Eppe, Gauthier; Monbaliu, Jean-Christophe M.

2017-01-01

Multidisciplinary lab experiments combining microfluidics, nanoparticle synthesis, and characterization are presented. These experiments rely on the implementation of affordable yet efficient microfluidic setups based on perfluoroalkoxyalkane (PFA) capillary coils and standard HPLC connectors in upper undergraduate chemistry laboratories.…

Development of an Automated Microfluidic Reaction Platform for Multidimensional Screening: Reaction Discovery Employing Bicyclo[3.2.1]octanoid Scaffolds

PubMed Central

Goodell, John R.; McMullen, Jonathan P.; Zaborenko, Nikolay; Maloney, Jason R.; Ho, Chuan-Xing; Jensen, Klavs F.; Porco, John A.

2010-01-01

An automated, silicon-based microreactor system has been developed for rapid, low-volume, multidimensional reaction screening. Use of the microfluidic platform to identify transformations of densely functionalized bicyclo[3.2.1]octanoid scaffolds will be described. PMID:20560568

The application of a monolithic triphenylphosphine reagent for conducting Appel reactions in flow microreactors

PubMed Central

Roper, Kimberley A; Lange, Heiko; Polyzos, Anastasios; Berry, Malcolm B; Baxendale, Ian R

2011-01-01

Summary Herein we describe the application of a monolithic triphenylphosphine reagent to the Appel reaction in flow-chemistry processing, to generate various brominated products with high purity and in excellent yields, and with no requirement for further off-line purification. PMID:22238543

Turbidimetric and photometric determination of total tannins in tea using a micro-flow-batch analyzer.

PubMed

Lima, Marcelo B; Andrade, Stéfani I E; Harding, David P; Pistonesi, Marcelo F; Band, Beatriz S F; Araújo, Mário C U

2012-01-15

Both turbidimetric and photometric determinations of total tannins in samples of green and black tea, using a micro-flow-batch analyzer (μFBA) were studied. The miniaturized system was formed using photocurable urethane-acrylate resin and ultraviolet lithography technique. The turbidimetric method was based on the precipitation reaction of Cu (II) with tannins in acetate medium at a pH of 4.5. The photometric method was based on the complexation reaction of tannins with ferrous tartrate. The turbidimetric μFBA was able to test 200 samples per hour. The photometric μFBA allowed 300 analyses per hour, generating 136μL of residue per analysis. The paired t test, at a 95% confidence level, showed no statistically significant differences between results obtained by both methods and the reference method. The urethane-acrylate μFBA maintained satisfactory physical and chemical properties, and represents an improvement over conventional flow-batch analyzer. Copyright © 2011 Elsevier B.V. All rights reserved.

Effects of anti-foaming agents on biohydrogen production.

PubMed

Sivagurunathan, Periyasamy; Anburajan, Parthiban; Kumar, Gopalakrishnan; Bakonyi, Péter; Nemestóthy, Nándor; Bélafi-Bakó, Katalin; Kim, Sang-Hyoun

2016-08-01

The effects of antifoaming agents on fermentative hydrogen production using galactose in batch and continuous operations were investigated. Batch hydrogen production assays with LS-303 (dimethylpolysiloxane), LG-109 (polyalkylene), LG-126 (polyoxyethylenealkylene), and LG-299 (polyether) showed that the doses and types of antifoaming agents played a significant role in hydrogen production. During batch tests, LS-303 at 100μL/L resulted in the maximum hydrogen production rate (HPR) and hydrogen yield (HY) of 2.5L/L-d and 1.08mol H2/mol galactoseadded, respectively. The following continuously stirred tank reactor operated at 12h HRT with LS-303 at 100μL/L showed a stable HPR and HY of 4.9L/L-d and 1.17mol H2/mol galactoseadded, respectively, which were higher than those found for the control reactor. Microbial community analysis supported the alterations in H2 generation under different operating conditions and the stimulatory impact of certain antifoaming chemicals on H2 production was demonstrated. Copyright © 2016 Elsevier Ltd. All rights reserved.

Laboratory-scale anaerobic sequencing batch reactor for treatment of stillage from fruit distillation.

PubMed

Rada, Elena Cristina; Ragazzi, Marco; Torretta, Vincenzo

2013-01-01

This work describes batch anaerobic digestion tests carried out on stillages, the residue of the distillation process on fruit, in order to contribute to the setting of design parameters for a planned plant. The experimental apparatus was characterized by three reactors, each with a useful volume of 5 L. The different phases of the work carried out were: determining the basic components of the chemical oxygen demand (COD) of the stillages; determining the specific production of biogas; and estimating the rapidly biodegradable COD contained in the stillages. In particular, the main goal of the anaerobic digestion tests on stillages was to measure the parameters of specific gas production (SGP) and gas production rate (GPR) in reactors in which stillages were being digested using ASBR (anaerobic sequencing batch reactor) technology. Runs were developed with increasing concentrations of the feed. The optimal loads for obtaining the maximum SGP and GPR values were 8-9 gCOD L(-1) and 0.9 gCOD g(-1) volatile solids.

Utilization of Stop-flow Micro-tubing Reactors for the Development of Organic Transformations.

PubMed

Toh, Ren Wei; Li, Jie Sheng; Wu, Jie

2018-01-04

A new reaction screening technology for organic synthesis was recently demonstrated by combining elements from both continuous micro-flow and conventional batch reactors, coined stop-flow micro-tubing (SFMT) reactors. In SFMT, chemical reactions that require high pressure can be screened in parallel through a safer and convenient way. Cross-contamination, which is a common problem in reaction screening for continuous flow reactors, is avoided in SFMT. Moreover, the commercially available light-permeable micro-tubing can be incorporated into SFMT, serving as an excellent choice for light-mediated reactions due to a more effective uniform light exposure, compared to batch reactors. Overall, the SFMT reactor system is similar to continuous flow reactors and more superior than batch reactors for reactions that incorporate gas reagents and/or require light-illumination, which enables a simple but highly efficient reaction screening system. Furthermore, any successfully developed reaction in the SFMT reactor system can be conveniently translated to continuous-flow synthesis for large scale production.

Biotic and abiotic dynamics of a high solid-state anaerobic digestion box-type container system.

PubMed

Walter, Andreas; Probst, Maraike; Hinterberger, Stephan; Müller, Horst; Insam, Heribert

2016-03-01

A solid-state anaerobic digestion box-type container system for biomethane production was observed in 12 three-week batch fermentations. Reactor performance was monitored using physico-chemical analysis and the methanogenic community was identified using ANAEROCHIP-microarrays and quantitative PCR. A resilient community was found in all batches, despite variations in inoculum to substrate ratio, feedstock quality, and fluctuating reactor conditions. The consortia were dominated by mixotrophic Methanosarcina that were accompanied by hydrogenotrophic Methanobacterium, Methanoculleus, and Methanocorpusculum. The relationship between biotic and abiotic variables was investigated using bivariate correlation analysis and univariate analysis of variance. High amounts of biogas were produced in batches with high copy numbers of Methanosarcina. High copy numbers of Methanocorpusculum and extensive percolation, however, were found to negatively correlate with biogas production. Supporting these findings, a negative correlation was detected between Methanocorpusculum and Methanosarcina. Based on these results, this study suggests Methanosarcina as an indicator for well-functioning reactor performance. Copyright © 2016 Elsevier Ltd. All rights reserved.

MODELING OF ION-EXCHANGE FOR CESIUM REMOVAL FROM DISSOLVED SALTCAKE IN SRS TANKS 1-3, 37 AND 41

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, F

2007-08-15

This report presents an evaluation of the expected performance of engineered Crystalline Silicotitanate (CST) and spherical Resorcinol-Formaldehyde (RF) ion exchange resin for the removal of cesium from dissolved saltcake in SRS Tanks 1-3, 37 and 41. The application presented in this report reflects the expected behavior of engineered CST IE-911 and spherical RF resin manufactured at the intermediate-scale (approximately 100 gallon batch size; batch 5E-370/641). It is generally believed that scale-up to production-scale in RF resin manufacturing will result in similarly behaving resin batches whose chemical selectivity is unaffected while total capacity per gram of resin may vary. As such,more » the predictions provided within this report should provide reasonable estimates of production-scale column performance. Two versions of the RF cesium isotherm were used. The older version provides a conservative estimate of the resin capacity while the newer version more accurately fits the most recent experimental data.« less

Application of high performance liquid chromatography for the profiling of complex chemical mixtures with the aid of chemometrics.

PubMed

Ni, Yongnian; Zhang, Liangsheng; Churchill, Jane; Kokot, Serge

2007-06-15

In this paper, chemometrics methods were applied to resolve the high performance liquid chromatography (HPLC) fingerprints of complex, many-component substances to compare samples from a batch from a given manufacturer, or from those of different producers. As an example of such complex substances, we used a common Chinese traditional medicine, Huoxiang Zhengqi Tincture (HZT) for this research. Twenty-one samples, each representing a separate HZT production batch from one of three manufacturers were analyzed by HPLC with the aid of a diode array detector (DAD). An Agilent Zorbax Eclipse XDB-C18 column with an Agilent Zorbax high pressure reliance cartridge guard-column were used. The mobile phase consisted of water (A) and methanol (B) with a gradient program of 25-65% (v/v, B) during 0-30min, 65-55% (v/v, B) during 30-35min and 55-100% (v/v, B) during 35-60min (flow rate, 1.0mlmin(-1); injection volume, 20mul; and column temperature-ambient). The detection wavelength was adjusted for maximum sensitivity at different time periods. A peak area matrix with 21objectsx14HPLC variables was obtained by sampling each chromatogram at 14 common retention times. Similarities were then calculated to discriminate the batch-to-batch samples and also, a more informative multi-criteria decision making methodology (MCDM), PROMETHEE and GAIA, was applied to obtain more information from the chromatograms in order to rank and compare the complex HZT profiles. The results showed that with the MCDM analysis, it was possible to match and discriminate correctly the batch samples from the three different manufacturers. Fourier transform infrared (FT-IR) spectra taken from samples from several batches were compared by the common similarity method with the HPLC results. It was found that the FT-IR spectra did not discriminate the samples from the different batches.

Large-scale manufacturing of GMP-compliant anti-EGFR targeted nanocarriers: production of doxorubicin-loaded anti-EGFR-immunoliposomes for a first-in-man clinical trial.

PubMed

Wicki, Andreas; Ritschard, Reto; Loesch, Uli; Deuster, Stefanie; Rochlitz, Christoph; Mamot, Christoph

2015-04-30

We describe the large-scale, GMP-compliant production process of doxorubicin-loaded and anti-EGFR-coated immunoliposomes (anti-EGFR-ILs-dox) used in a first-in-man, dose escalation clinical trial. 10 batches of this nanoparticle have been produced in clean room facilities. Stability data from the pre-GMP and the GMP batch indicate that the anti-EGFR-ILs-dox nanoparticle was stable for at least 18 months after release. Release criteria included visual inspection, sterility testing, as well as measurements of pH (pH 5.0-7.0), doxorubicin HCl concentration (0.45-0.55 mg/ml), endotoxin concentration (<1.21 IU/ml), leakage (<10%), particle size (Z-average of Caelyx ± 20 nm), and particle uptake (uptake absolute: >0.50 ng doxorubicin/μg protein; uptake relatively to PLD: >5 fold). All batches fulfilled the defined release criteria, indicating a high reproducibility as well as batch-to-batch uniformity of the main physico-chemical features of the nanoparticles in the setting of the large-scale GMP process. In the clinical trial, 29 patients were treated with this nanoparticle between 2007 and 2010. Pharmacokinetic data of anti-EGFR-ILs-dox collected during the clinical study revealed stability of the nanocarrier in vivo. Thus, reliable and GMP-compliant production of anti-EGFR-targeted nanoparticles for clinical application is feasible. Copyright © 2015 Elsevier B.V. All rights reserved.

Biodegradation of organic chemicals in soil/water microcosms system: Model development

USGS Publications Warehouse

Liu, L.; Tindall, J.A.; Friedel, M.J.; Zhang, W.

2007-01-01

The chemical interactions of hydrophobic organic contaminants with soils and sediments may result in strong binding and slow subsequent release rates that significantly affect remediation rates and endpoints. In order to illustrate the recalcitrance of chemical to degradation on sites, a sorption mechanism of intraparticle sequestration was postulated to operate on chemical remediation sites. Pseudo-first order sequestration kinetics is used in the study with the hypothesis that sequestration is an irreversibly surface-mediated process. A mathematical model based on mass balance equations was developed to describe the fate of chemical degradation in soil/water microcosm systems. In the model, diffusion was represented by Fick's second law, local sorption-desorption by a linear isotherm, irreversible sequestration by a pseudo-first order kinetics and biodegradation by Monod kinetics. Solutions were obtained to provide estimates of chemical concentrations. The mathematical model was applied to a benzene biodegradation batch test and simulated model responses correlated well compared to measurements of biodegradation of benzene in the batch soil/water microcosm system. A sensitivity analysis was performed to assess the effects of several parameters on model behavior. Overall chemical removal rate decreased and sequestration increased quickly with an increase in the sorption partition coefficient. When soil particle radius, a, was greater than 1 mm, an increase in radius produced a significant decrease in overall chemical removal rate as well as an increase in sequestration. However, when soil particle radius was less than 0.1 mm, an increase in radius resulted in small changes in the removal rate and sequestration. As pseudo-first order sequestration rate increased, both chemical removal rate and sequestration increased slightly. Model simulation results showed that desorption resistance played an important role in the bioavailability of organic chemicals in porous media. Complete biostabilization of chemicals on remediation sites can be achieved when the concentration of the reversibly sorbed chemical reduces to zero (i.e., undetectable), with a certain amount of irreversibly sequestrated chemical left inside the soil particle solid phase. ?? 2006 Springer Science + Business Media B.V.

Bullet identification: a case of a fatal hunting accident resolved by comparison of lead shot using instrumental neutron activation analysis.

PubMed

Capannesi, G; Sedda, A F

1992-03-01

Bullet identification by chemical analysis often provides a powerful clue in forensic science. A case is reported in which a hunting accident was resolved by using instrumental neutron activation analysis (INAA) for direct comparison of the trace element content in lead shot. Different preparation batches of lead shot appear to have a high within-group composition homogeneity, and good differentiation is achieved between different batches. Determination of the nickel and antimony content on a bush branch demonstrated that the branch had been perforated by one of the shot pellets, and this helped the detectives in reconstruction of the crime scene.